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Volume 35, Issue 3
Displaying 1-48 of 48 articles from this issue
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Yutaka ASAHI, Masami TANAKA, Kazuko MIMA1986 Volume 35 Issue 3 Pages 147-150
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTen base halides in Japanese Pharmacopoeia were determined by nonaqueous titration after treating with mercuric acetate. Aim of this study was to omit the poisonous reagent. Bethanechol chloride (I), pilocarpine hydrochloride (II), scopolamine hydrobromide (III) and homatropine hydrobromide (IV) could be determined by potentiometric titration with 1 eq. perchloric acid in acetic anhydride-acetic acid (9:17:3). Quinine hydrochloride (V) and dibucaine hydrochloride (VI) were similarly titrated with 2 eq. perchloric acid. Procainamide hydrochloride (VII) and tetracaine hydrochloride (VIII) were also titrated with 1 eq. perchloric acid after acetylation of the aromatic amine. A silver-silver chloride electrode with ceramic junction containing acetic acid saturated with lithium chloride and a regular glass electrode were preferred as the electrodes. Standard deviation of this method was 0.3 %. The potentiometry was more exact than indicator method using methylrosanilinium chloride. It was estimated from the potential of glass electrode at the half equivalent point that the order of acid strength was perchloric acid, hydrobromic acid and hydrochloric acid and that of base strength was quaternary amine (I), tertiary amines (III, VIII), quinolines (V, VI), aromatic amines (VII, VIII) and aromatic amides (VII, VIII).View full abstractDownload PDF (746K) -
Spectrophotometric determination of drugs containing carboxylic group using dicyclohexylcarbodiimideRieko MATSUDA, Yasushi TAKEDA, Mumio ISHIBASHI, Mitsuru UCHIYAMA, Masa ...1986 Volume 35 Issue 3 Pages 151-156
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe coloration method with one step formation of hydroxamate from carboxylic acid was applied to the spectrophotometric determination of drug formulations. Carboxylic acid was reacted with hydroxylamine perchlorate (HAP) to form hydroxamic acid by the aid of dicyclohexylcarbodiimide (DCC). The iron hydroxamate was formed with iron(III) perchlorate in ethanolic solution of perchloric acid. The optimum condition was studied for ibuprofen (IB), sodium valproate (VA) and mefenamic acid (MF). The established procedure is as follows. The drug was extracted with ethanol from the formulation and diluted to about 5 mM with ethanol. To 1 ml of the solution were added 1 ml of 0.3 M HAP ethanolic solution and 1 ml of 0.3 M DCC ethanolic solution. The mixture was reacted at 50°C for 20 min. After cooling 1 ml of 0.02 M iron (III) perchlorate ethanolic solution containing 0.2 M perchloric acid was added, and ethanol was added to adjust the total volume to 10 ml. The absorbance was measured at 538 nm for IB and VA, and at 608 nm for MF. The calibration curves were linear in the range of 2 mM to 10 mM, and relative standard deviation was less than 1% for the standard solutions and 14.5% for the preparations (n = 5). The applicability of this method was studied on 14 drugs.View full abstractDownload PDF (886K) -
Drugs in fallen and floating dust in a dispensaryMisuzu ICHIBA, Hashime KANAZAWA, Nobuyuki SHIMIZU, Mieko KOBO, Keitaro ...1986 Volume 35 Issue 3 Pages 157-160
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe fallen dust was collected on a membrane filter at the height of 120 cm from the floor, while the floating dust was sucked on a membrane filter under 550 mmHg at the 150 cm height. Collection of these dust was conducted at one place near the dispensing corner of powders during the period of 9 : 00 am to 5 : 00 pm on Feb. 5, 1985. The respective resulting dust (fallen dust 0.36 mg, floating dust 1.34 mg) was successively examined with optical, fluorescence, and polarizing microscopes. By microscopic comparison of dust with standard drugs, eleven kinds of drugs (three agents affecting central nervous system, three agents affecting digestive organs, two vitamins, and three excipients) were identified from the dust. The existence of all drugs except excipients was also confirmed by the chemical ionization mass spectrometry.View full abstractDownload PDF (807K) -
Kiyoko TAKAMURA, Satoshi INOUE, Kunio ITO, Fumiyo Kusu1986 Volume 35 Issue 3 Pages 161-166
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn anodically pretreated glassy carbon (GC) electrode was applied to the voltammetric determination of phenothiazine drugs. Pretreatment of GG electrode was made by anodic oxidation in 0.5 mol dm-3 phosphate at 1.6 V vs. SCE for 2 min. Using this electrode, voltammograms were measured for nine drugs by conventional technique of potential scanning in 0.5 mol dm-3 phosphate buffer (pH 6.8). All the drugs investigated gave some oxidation peaks on the voltammograms. Their first peak currents were proportional to the drug concentration, and the linear relations were obtained ranging in concentration from 5 × 10-8 to 10-6 mol dm-3. The method was applied further to the determination of such drugs in some commercial injections with good results.View full abstractDownload PDF (901K) -
Shinji HIRANO, Tsutomu MASUJIMA, Hisanobu YOSHIDA, Hideo IMAI1986 Volume 35 Issue 3 Pages 167-172
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSHighly sensitive determination of adriamycin (an anticancer chemotherapy agent) using preconcentration by adsorption on glassy carbon electrode was investigated by an electrochemical method. A glassy carbon electrode was pre-treated by electrolytic oxidation at 1.4 V vs. Ag/AgCl for 25 min in 0.1 M McIlvaine buffer (pH 6.0) containing 0.5 M sodium sulfate. The electrode rotating at 1000 r.p.m. was dipped in 0.5 ml adriamycin solution for 10 min. Then, the quantity of adriamycin adsorbed was estimated by the oxidative peak current (or by the reductive peak current) recorded by scanning 00.9 V span at 200 mV/s in pH 2.0 solution. The determination range was pmol with 0.5 ml sample solution, and the within-day relative standard deviation was 2.7% (n=10). Plasma sample was pre-treated by two-stages solvent extraction, the first at pH 3.0 to remove interfering plasma component and the second at pH 8.0 to extractadriamycin. The recovery of adriamycin was 95%.View full abstractDownload PDF (756K) -
Ryoko CHIBA, Yoko ISHII1986 Volume 35 Issue 3 Pages 173-176
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid and sensitive high performance liquid chromatographic method was established for simultaneous determination of the five main alkaloids (morphine, codeine, narceine, noscapine, papaverine) in opium alkaloid hydrochloride (JPX). A sample was separated on a column (150 mm × 4.6 mm i. d.) packed with reversed phase (Hitachi Gel # 3056), and eluted with a mixture of acetonitrile, 0.005 M phosphate buffer (pH 3) and 0.2 M heptanesulfonate (50 : 50 : 1.5) as the mobile phase. The effluent was monitored with a ultraviolet detector at a wavelength of 254 nm. Determination was carrid out successfully by using ethylmorphine hydrochloride as an internal standard. Recoveries of these alkaloids for known standard sample were satisfactory. The relative standard deviation for the determination of these alkaloids was less than 1.5%. This chromatographic method is simple, accurate and selective with an analysis time of less than 15 min.View full abstractDownload PDF (481K) -
Tadao SAKAI, Satoshi OJIMA, Eiji SAEKI, Masaya TANAKA1986 Volume 35 Issue 3 Pages 177-183
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe sensitive and selective method described here is based on the reaction of monovalent cation of quinine (HQ+) and quaternary ammonium ion (R4N+) with divalent anion (A2-) of diprotic acid dye, such as Bromochlorophenol Blue (BCPB) or Bromocresol Purple(BCP), to form a 1 : 1 : 1 ternary ion association complex (R4N+·HQ+·A2-) extractable into 1, 2-dichloroethane at nearly pH 7. Berberine and cetylpyridinium ion could be extracted in large amounts into 1, 2-dichloroethane with the above dyes only in the presence of quinine. Other amines and some kinds of quaternary ammonium ions were not extracted. Accordingly, the formation of R4N+·HQ+·A2-might enhance extractability and selectivity of berberine and cetylpyridinium ion. Molar absorptivities were 4.99 × 104 mol-1 cm-1 1 for berberine-quinine-BCPB associate, 1.24 × 104for berberine-quinine-BCP and 4.68 × 104 for cetylpyridinium ion-quinine-BCPB, respectively. These blue associates with BCPB and BCP showed maximum absorbances at 605 and 593 nm, respectively and could be applied in spectrophotometric determination of berberine and cetylpyridinium ion used as cationic disinfectants in drugs.View full abstractDownload PDF (1007K) -
Koji KAWANABE, Eiko YAMAGUCHI1986 Volume 35 Issue 3 Pages 184-188
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new and simple technique for thin-layer chromatography was devised by use of glass sticks in place of glass plates. The glass sticks used were slim glass tubes of 2.3 mm in diammter and 13 cm in length. The adsorvent was uniformly spread over the surface of the glass sticks by vertically passing through a funnel con taining aqueous suspension of the silica gel with microcrystalline cellulose and 3% of hydroxyethyl cellose. After the heat-activation of the adsorvent at 90°C for 30 min, the thin-layer stick was shaved to two surfaec for the dual wavelength linear-scannig method and standard solution were spotted 2 cm from the lower end of the stick. The developing distnace was set at 5 cm for all the tests. The thin-layer stick after development was set on a Shimadzu Chromatoscanner CS-910 and was exposed with dual wavelength(λS, λP). Compared with the conventional detection methods with spray reagents, the present method is much easier in operation and furthermore, detection sensitivity is higer. This technique was applied to the identification of drugs such as caffeine, phenacetine, phenol, acrinol and salicylic acid contained in preparations in Pharmacopoeia of Japan(X).View full abstractDownload PDF (578K) -
Syoji KANEKO, Yuki TSUSHIMA, Yutaka YOSHIDA, Masanori KAYANO1986 Volume 35 Issue 3 Pages 189-192
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and accurate gas chromatographic method for the determination of dimethylpolysiloxane(DMPS) in gastrointestinal drugs was established. This method is based on the formation of dimethyldiethoxysilane (DMES) by the reaction between DMPS and ethyl silicate under alkaline condition. The procedure is as follows : Take appropriate amount of powdered drug containing about 10 mg of DMPS, add 8 ml of ethyl silicate and 0.4 g of potassium hydroxide, and reflux for 30 min at 160180°C. After cooling, distill the reaction mixture, and collect about 7 ml of distillate. Make the volume of the distillate up to 10 ml with ethyl silicate. Inject 10μl of this solution into gas chromatograph, and calculate the content of DMPS in the drug from calibration curve based on peak area of DMES. Gas chromatographic conditions are as follows: Column; Diasolid ZF (3 mm i.d. × 2 m), column temp.; 50°C, injection temp. ; 100°C, detector; flame ionization detector. The calibration curve was linear in the range of 0.41.2 mg/ml of DMPS. Re coveries of DMPS from drugs tested were quantitative. Ten replicate determination of a drug containing 20.0 mg/1.2 g of DMPS gave average value of 19.62 mg/1.2 g(98.1%) and relative standard deviation of 2.98%.View full abstractDownload PDF (683K) -
I. Determination of salicylic acid and phenol in pharmaceutical preparations in the Japanese Pharmacopoeia XMuneo MORISHITA, Hideaki IIZUKA, Masa KATAYANAGI, Takehiko YAJIMA1986 Volume 35 Issue 3 Pages 193-197
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination method of phenol and salicylic acid in pharmaceutical preparations was investigated by using adsorption chromatography with steam as a carrier, the temperature of which was more than 100°C. Chromosorb P AW (6080 meshes) modified with 4% phosphoric acid was employed as a stationary phase. With benzoic acid as an internal standard, both phenol and salicylic acid were able to be determined quantitatively without interference by moisture in samples or solvent alcohol under the following conditions: for phenol, column temperature, 140°C and water feeding rate, 18.7 μl/min; for salicylic acid, column temperature, 200°C and water feeding rate, 40 μl/min. Simultaneous determination of phenol and salicylic acid was performed by raising the column temperature at a rate of 10°C/min from 130°C to 240 °C and at the water feeding rate of 10μl/min. Benzoic acid was also used as an internal standard for the simultaneous determination. Following results were obtained by the regression analysis of the weight ratio (X1, X2) and the peak height ratio (Y1, Y2) between phenol or salicylic acid and benzoic acid: regression equations, Y1=736X1-0.006 and Y2=0.529X2+0.027; correlation coefficients, r1=0.996 and r2=0.998; relative standard deviations after five runs, 0.16% for Y1 and 0.39% for Y2. These data indicate that the present method is good enough for quantitative analysis. Under the conditions mentioned above, six pharmaceuticals specified in JPX were successfully analyzed quantitatively.View full abstractDownload PDF (806K) -
II. Determination of methyl salicylate, menthol and camphor in medicated spirits in the Japanese Pharmacopoeia XHideaki IIZUKA, Muneo MORISHITA, Masa KATAYANAGI, Takehiko YAJIMA1986 Volume 35 Issue 3 Pages 198-201
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination method of dl-camphor, l-menthol and methyl salicylate in medicated spirits was established by the use of steam carrier gas chromatography with an Ohkura gas chromatograph SSC-1/Model 701 equipped with a hydrogen flame ionization detector. A glass column, 2.2 mm i.d. and 1 m in length, packed. with 6080 mesh Neopack 1B coated with 10% polyethylene glycol 20 M (PEG20 M) was used. The column was used at a constant temperature of 135°C and an injector temperature was kept at 200°C. The carrier flow rate was that obtained by feeding water at a rate of 10μl/min. Isopropyl carbamate was chosen as an internal standard for the simultaneous determination of the three components. Under the conditions employed, dl-camphor, l-menthol, isopropyl carbamate and methyl salicylate were eluted in this order within 15 min as sharp peaks with satisfactory resolution and reproducibility. Following results were obtained by the regression analyses of the weight ratio (X1, X2, X3) and the peak height ratio (Y1, Y2, Y3) between dl-camphor (X1, Y1), l-menthol (X2, Y2) or methyl salicylate (X3, Y3) and the internal standard: regression equations, Y1=4.136X1+0.0155, Y2=2.814X2+0.099 and Y3=1.150X3+0.155; correlation coefficients, r1=0.998, r2=0.999 and r3=0.991; relative standard deviations after five runs were 0.67, 0.72 and 0.84% for Y1, Y2 and Y3, respectively. Under the chromatographic conditions mentioned above, two medicated spirits prepared as described in JPX and three commercial medicated spirits were successfully analysed. quantitatively only with dilution without further pretreatment of samples.View full abstractDownload PDF (479K) -
Nobuyuki HITOMI, Kesamitsu SHIMIZU, Keiichi YAMAMOTO, Osamu MIURA, Eiz ...1986 Volume 35 Issue 3 Pages 202-206
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA quantitative quality control method of traditional chinese drugs (TCD) by HPLC is described, by choosing Mao-to formulation as an example of TCD. Six compounds, namely l- and d-ψ-ephedrine, amygdalin, cinnamaldehyde, glycyrrhizin and liquiritin specific to each of four constituent crude drugs of the formulation (Ephedrae Herba, Armeniacae Semen, Cinnamomi Cortex, Glycyrrhizae Radix) were used as reference substances. These compounds present in crude drugs as well as in processed preparations could be precisely assayed on an ODS column using four different mobile phases. In addition, it was stated that HPLC is similarly applicable to determination of some compounds specific to other several crude drugs than the above-mentioned ones.View full abstractDownload PDF (757K) -
Kou HAYAKAWA, Tomio FUJITA1986 Volume 35 Issue 3 Pages 207-210
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn analytical method for chondroitin sulfate (an acidic sulfated-mucopolysaccharide) was developed. Using a silica-based glycerylpropyl column (Shimpack DIOL-300; dp=5 μm, pore size 300 Å, 500 × 7.9 mm i. d.) with a methanol-potassium chloride-water mixture as eluting solvent, chondroitin sulfate was determined in 30 min at a flow rate of 1 ml/min. The characteristic of the elution order was determined with two chondroitin sulfate standards. The molecular weights of them were previously determined as to be 25000 and 5000 by viscometry. The two standards were eluted in the order of their unique molecular weights. The standard with molecular weight of 25000 was eluted on a narrower pore-size column (Shimpack DIOL-150) as a sharp peak, which indicated a phenomenon of exclusion. By using polyethylene glycol as standards for calibration, the molecular weights of the two chondroitin standards were determined as expectedly by viscometry. The application of this method to some commercial preparations were performed. Commercial injection and eye-drops were analysed and found not to be disturbed by other components in the preparations. In the analysis of eye drops for chondroitin sulfate, the peak areas were correlated to the amounts (0.89% R.S.D., n=3). Molecular weight characteristics of chondroitin were also determined within 1.6% R. S. D. for eye-drops and 1.2% R. S. D. for injections, respectively. Thus, this method was shown to be applicable to simultaneous determination and molecular size characterization of chondroitin sulfate in some commercial preparations.View full abstractDownload PDF (599K) -
Teruhiko HAGIWARA, Shinichi UEHARA, Kunihiro KAMTA, Misako TAKAHASHI, ...1986 Volume 35 Issue 3 Pages 211-214
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for determination of trace amounts of gitoxin in digoxin tablet was developed by using reversed phase high performance liquid chromatography. A solution of chloroform and methanol(2 : 1) was added to the powdered digoxin tablet and refluxed for 30 min in a water bath. After filtration, the extracted solution was evaporated and 2.5 ml of 70% methanol solution was added. The residue was dissolved by ultrasonication for 10 min. A 25μl of the ultrasonicated solution was injected onto the HPLC system and peak area was measured. The condition of HPLC was as follows: Column, Hiber RP-18, 7 μm, 4 mm φ × 25 cm (Merck); mobile phase, 65% methanol in water; flow rate, 1 ml/min; detection, UV 225 nm; sensitivity, 0.02 AUFS; integrator sensitivity, ATT × 2; column temp., ambient. The calibration curve between peak area and amount of gitoxin was linear up to 700μg of gitoxin. The within-day relative standard deviations of the proposed method for the analyses of spiked digoxin tablet (1 g) at 5, 250 and 700μg were 2.69, 1.11 and 1.58%, respectively, mean recoveries being more than 96%. The lower determination limit was 0.5μg of gitoxin in 1 g of powdered tablet. Gitoxin was found in digoxin tablet ranging from 0.13 to 0.34%, but not found in digitoxin tablet and lanatoside C tablet.View full abstractDownload PDF (560K) -
Yoshinobu AKADA, Youichi KANEMATSU1986 Volume 35 Issue 3 Pages 215-218
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of geniposide, geniposidic acid and gardenoside in gardenia fruit (Shan-shi-shi in Japanese) by high performance liquid chromatography (HPLC) was established. These iridoid glucosides in aqueous extract of gardenia fruit were separated on a Microsorb C8 column (4.6 mm i.d. × 150 mm) with an eluent of 10 mM phosphate buffer (pH 3.0)-methanol (5 : 1) and detected at 242 nm. Aqeous extracts of gardenia fruit was injected directly into the column without any pretreatments, and sufficient separation could be achieved within 30 min. Contents of iridoid glucosides were calculated from calibration curves based on their peak heights in HPLC chromatogram. Recovery of these glucosides by this method was found to be quantitative. This HPLC method was considered to be useful for the evaluation of gardenia fruit. Correlations between these iridoid glucosides contents and crocin content was also examined.View full abstractDownload PDF (573K) -
Masakazu HORSE, Youji HOSHINO, Norihide NOSE, Hisao IWASAKI, Yasuo SHI ...1986 Volume 35 Issue 3 Pages 219-224
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid method for the determination of spiramycin in swine, cattle and chicken muscles has been developed by means of high performance liquid chromatography (HPLC). The three components of spiramycin were isolated by the HPLC on a Nucleosil 5C18 column (25 cm × 10.0 mm i.d.). The three components were identified as expected spiramycin I, spiramycin II and spiramycin III by mass spectrometry.The drug was extracted from muscle with 0.5% metaphosphoric acid-methanol(7 : 3). The filtered extract was adjusted to pH 8.5, and extracted with dichloromethane. After evaporation of dichloromethane, the residue was dissolved in distilled water-acetonitrile (7 : 3). Spiramycin was separated on the Nucleosil 5C18 column by using 0.05 M phosphate buffer pH 2.5-acetonitrile (72 : 28), and detected at 232 nm with 0.02 AUFS. The calibration curve for spiramycin was linear from 20 ng to 200 ng. Recoveries of spiramycin add to swine, cattle and chicken muscles at the level of 1.0 ppm were 91.4, 88.4 and 91.7%, respectively. The detection limit for spiramycin was 0.05 ppm in this procedure.View full abstractDownload PDF (928K) -
Development of automatic sample cleanup procedureYutaka HASHIMOTO, Yumi NAKAI, Masataka ISHIBASHI, Hiroshi MIYAZAKI, Ha ...1986 Volume 35 Issue 3 Pages 225-229
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn automatic sample clean-up procedure for high performance liquid chromatographic (HPLC) analysis of Etoposide in biological materials was developed by the use of a liquid chromatographic module (LC Module). This technique was based on the automation of selective extraction of Etoposide from a cartridge packed with chemically bonded silica sorbent with a solvent system for HPLC mobile phase and transference of the eluate into a HPLC column using this LC Module. Phenylsilica was the most suitable packing materials for the adsorption of Etoposide from biological samples. After the charge of sample onto the cartridge a number of these cartridge were placed onto the LC Module for the extraction, clean-up, on-stream elution and injection into a HPLC column. Etoposide was selectively eluted from this cartridge within 36 s and the substances in biological sample were still retained in this disposable cartridge. Thus, all operation for this analysis was achieved within 15 min. The recovery of Etoposide in biological samples was practically quantitative and excellent reproducibility was obtained.View full abstractDownload PDF (712K) -
Tomonori HAYASHI, Atsushi TAMURA, Hisanobu YOSHIDA1986 Volume 35 Issue 3 Pages 230-235
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDirect injection of plasma sample onto the precolumn of an automated sample clean-up system for the RP-HPLC determination of adriamycins is proposed. After injection of plasma sample onto the precolumn of protein-coated ODS, the intial aqueous solution eluted out plasma proteins and hydrophilic components during the trapping of adriamycins on the precolumn. Then, the precolumn was connected, in a back flush mode, to the analytical ODS column to allow adriamycins to be separated through the analytical column. The elution system was changed depending on the detection method. With fluorometry (Ex. 475 nm/ Em. 580 nm), it was possible to determine the adriamycins in plasma with simple two steps elution system. However, with UV-spectrophotometry (UV 290 nm), two points were important, the first point was to wash out the interfering compounds from the precolumn using three steps washing solvents, the second was to elute adriamycinol from the analytical column after the buffer change artifacts. The latter condition might offer some concept for applying the present method for setting up a method for the determination of non-fluorecent drugs with UV adsorbing characteristics. In view of simplicity and accuracy for the determination of total (free + bound to plasma proteins) adriamycins in plasma, the present method was superior to the conventional HPLC method which involved deproteinization step with 5% TCA or 50% acetonitrile. The recovery of adriamycin, adriamycinol and adriamycinone spiked in rabbit plasma (5 × 10-6 M each) was almost quantitative (100±2%) with good reproducibility(R.S.D. less than 2%, n= 5), when 1 00 p.1 of the plasma was analyzed, indicating that the method did not always need an internal standard. Adriamycins in a pure aqueous solution (below ca. 10-6 M) have trends to be adsorbed to the glass wall, however, the present method was almost free from this trouble. Levels of adriamycins in rabbit plasma after intravenous administration of adriamycin (3.8 mg/kg) could be followed by the present method.View full abstractDownload PDF (881K) -
Hiroyuki MURAKITA, Morimasa HAYASHI, Hirohisa MIKAMI, Yasuo ISHIDA1986 Volume 35 Issue 3 Pages 236-240
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn analysis of drugs in human serum by high performance liquid chromatography (HPLC), preparation of sample is essential due to complexity of sample composition. Manual preparation of sample is time-consuming work. Automated sample preparation using pre-column extraction and column switching was examined. The system consists of two flow lines which are connected each other by a flow changeover valve. The system is controlled by microprocessors. Drugs of interest are trapped by hydrophobic interaction on pre-column (4 mm i. d. × 30 mm L.: tetramethylolmethanetriacrylate resin packing) which is then introduced to the analytical column by column switching. Hydrophilic interaction is suppressed in this column. Weak hydrophilic interaction prevents proteins from irreversible adsorption. Proteins in serum can be shunted by base such as triethylamine. When elution of the drugs from the pre-column is completed, the flow changeover valve is switched back to its initial position and then the pre-column is regenerated for the subsequent sample. Preparation mobile phases which can extract anticonvulsants, theophylline and lidocaine selectively were chosen. Baseline stability was examined using blank serum. This system made direct injection of serum and stable automated analysis possible. The analysis by this system was free of interference from serum. Good recovery and reproducibility were obtained for all components analyzed.View full abstractDownload PDF (821K) -
Jun HAGINAKA, Terumichi NAKAGAWA1986 Volume 35 Issue 3 Pages 241-244
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCephradine (CED) and cephalexin (CEX) which is an impurity in CED products, were separated from regular components of plasma and urine on a reversed phase C18 column using sodium heptylsulfonate as an ion-pairing agent, and detected at 260 nm. The limits of accurate determination of CED and CEX in plasma were 100 ng/ml. The precision (relative standard deviation) was of the order of 2.03% (n=5) at a CED concentration of 1.0μg/ml in plasma. CEX content in commercial CED capsules was determined by the proposed method. It was found that a CED capsule contained 2.88% of CEX. The pharmacokinetic behavior of CED and CEX after an oral administration was discussed using the moment analysis method. The results revealed that CED had almost the same bioavailability as CEX, and the coexistence of CEX in commercial CED capsules had no influence on the pharmacokinetic feature of CED.View full abstractDownload PDF (532K) -
Kiyokatsu HIBI, Akio WADA, Mikio TAKEUCHI, Makoto HATTA1986 Volume 35 Issue 3 Pages 245-249
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method was developed for the determination of thiamylal in blood by means of reversed phase high performance liquid chromatography. Two hundred microliters of serum or plasma containing thiamylal was spiked with 60 μl ofn-propyl p-hydroxybenzoate methanol solution (25 mg/100 ml) as an internal standard. Deproteinization of this sample was performed by adding acetonitrile and centrifuging at 4500 r.p.m. for 10 min. The supernatant was filtered with 0.45 μm membrane filter and 20 μ 1 of the filtrate was subjected to reversed phase high performance liquid chromatography. The recovery for thiamylal by this method was 104407%. The sufficient resolution was obtained by using a silica-ODS column, Finepak SIL C18T (250 mm × 4.6 mm i. d.) at 40°C and 10 mM phosphate buffer (pH 3.0)-acetonitrile(50 : 50) as mobile phase with the flow rate of 1.0 ml/min. UV absorption of the effluent was monitored at 288 urn. Thiamylal concentration in serum or plasma was determined by internal standard method, using the peak height ratio of thiamylal peak to n-propyl-phydroxybenzoate peak (I.S.). The detection limit of thiamylal was about 0.6 μg (S/N=3). The precision of the determination by this method was 0.14% as relative standard deviation. This method was successfully applied to the measurement of concentrationtime curve of thiamylal in patient blood. The obtained curve was very useful for optimization of dosage regimen.View full abstractDownload PDF (600K) -
Ryoichi KIZU, Shin-ichi HIGASHI, Kazuichi HAYAKAWA, Motoichi MIYAZAKI1986 Volume 35 Issue 3 Pages 250-255
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for determination of (trans-l-1, 2-diaminocyclohexane) oxalatoplatinum (II) (l-OHP), introduced by Kidani et al. as one of the promising antineoplastic platinum complexes, in plasma and urine by high performance liquid chromatography (HPLC) was investigated in order to contribute for metabolic study of l-OHP. The recommended pretreatment procedures and HPLC conditions are as follows. Pretreatment of plasma and urine ; pretreatment column is composed of Dowex 1-X8 (5 mm i.d. × 6 cm), Dowex 50 W-X4 (5 mm i.d. x 3 cm) and Sep-Pak C18 cartridge. Blood samples are centrifuged at 1000 g for 3 min to obtain plasma. One ml of plasma or urine is immediately placed on the pretreatment column and is eluted with water at the flow rate of 1.2 ml/min. The initial 6 ml portion of effluent is discarded and subsequent 10 ml portion is collected. An aliquot (100 μl) of the effluent collected is subjected to HPLC. All of these pretreatment procedures are carried out at 5±2°C. HPLC conditions ; column : Finepak SIL C18 (4.6 mm i.d. × 25 cm), eluent : H2O-MeOH (95 : 5), column temperature : 40°C, flow rate : 1 ml/min, detection wavelength : 210 nm, injection volume : 100μl. Under the conditions described above, a linear relationship was obtained between peak height and l-OHP concentration in plasma and urine. Determination limit was 0.5 μM l-OHP in sample solutions. Recovery of l-OHP in pretreatment was 86±3% in plasma and 83±2% in urine. A sensitive and precise determination of l-OHP in plasma and urine will be possible by this method.View full abstractDownload PDF (729K) -
Hiroaki KUBO, Yoshie KOBAYASHI, Toshio KINOSHITA1986 Volume 35 Issue 3 Pages 256-258
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and accurate method for the determination of disopyramide in serum by high performance liquid chromatography is described. Only 100μl of serum was required. Disopyramide in serum was purified by solid-liquid extraction method using Chem Elut and then liquid-liquid extraction method using dilute phosphoric acid. An aliquot of the acidic aqueous solution was injected directly into the chromatograph. Chromatographic conditions were as follows: column, Waters Radial-Pak CN cartridge (10 cm × 8 mm i.d.) ; detector, UV-210 nm; mobile phase, 25% acetonitrile solution containing 0.01 M dibutylamine (pH 3.0 with phosphoric acid) ; flow rate, 2.0 ml/min; internal standard, p-chlorodisopyramide. The retention times for disopyramide and p-chlorodisopyramide were 7 min and 11.5 min, respectively. A calibration curve was linear in the range from 0.5 μg/ml to 8 μg/ml. Within-run and day-to-day reproducibilities for 3.0 μg/ml are ± 3.4 % (n = 10) and ±3.8% (n = 8), respectively. This method and fluorescence polarization immunoassay have shown a good correlation (r=0.996).View full abstractDownload PDF (406K) -
Hiroaki KUBO, Haozhi LI, Yoshie KOBAYASHI, Toshio KINOSHITA1986 Volume 35 Issue 3 Pages 259-262
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple, rapid and reproducible method for the determination of furosemide in serum and urine by high performance liquid chromatography has been developed. Only 1000 μl of serum is required. Serum proteins are precipitated with 100μl of acetonitrile. After the centrifugation, 100μl of the supernatant and the same volume of the counter ion solution (0.01 M hexanesulfonic acid sodium salt, pH 2.8) is drawn into a microsyringe, successively. Urine is diluted with water to 50 times. Fifty microliters of the diluted urine and then the same volume of the counter ion solution are drawn into the microsyringe. Afer mixing the two solutions in the microsyringe, the whole mixture is directly injected into the chromatograph. The chromatograph used is that from Waters Associates consisted of a model 6000 A pump and a U6K injector. A Radial Pak μ Bondapak C18 (10 μm 10 cm × 8 mm i. d.) cartridge was used as the analytical column. The flow rate of mobile phase, 30% acetonitrile solution containing 5 mM hexanesulfonic acid sodium salt (pH 3.5) was 2.5 ml/min. The eluate was monitored with a Hitachi F-1000 fluorescence detector. The wavelength of excitation was 333 nm and that of emission was 415 nm. The retention time for furosemide was 11 min. A calibration curve was linear in the range from 25 ng/ml to 10μg/ml for the serum and from 1.25 μg/ml to 25 μg/ml for the urine. The limit of detection was 2.5 ng/ml of serum and 5.8 ng/ml of urine. The recoveries of added furosemide were above 93.5% for the serum and 90.8% for the urine. For the analyses of serum samples at 116.5, 233 and 466 ng/ml, the within-run reproducibilities were 3.48, 3.40 and 2.66% (n=10) respectively, and those of the day-to-day were 2.07, 1.44 and 0.40% (n=6) respectively. For the diluted urine, the within-run reproducibility for 500 ng/ml was 2.58% (n=11).View full abstractDownload PDF (430K) -
Takashi ARAI, Hiroaki KUBO, Toshio KINOSHITA, Hiroyuki NAKAZAWA, Masah ...1986 Volume 35 Issue 3 Pages 263-267
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of theophylline (TP) in human serum was developed using high performance liquid chromatography (HPLC) with electrochemical detection. Cyclic voltammetry was used to investigate the electrochemical behavior of TP for its amperometric determination. As a result, the electrochemical activity of TP showed a significant dependence on pH. In preparation of sample for HPLC, the deproteinization method with methanol was adopted and sulfamonomethoxine was chosen as internal standard. Only 20μl or less amount of serum was required. Serum proteins were precipitated with 500μl methanol containing the internal standard. After the centrifugation, 10μl or less of supernatant was injected into the chromatograph with an amperometric detector set at 1000 mV (16 nA). To avoid contamination peaks, the flow rate of the mobile phase, 6% acetonitrile solution cotaining 0.1 M phosphate buffer (pH 7.3), was set at 0.9 ml/min. The amount of TP was determined by measuring peak height ratios. The within-run and day-to-day reproducibilities for 10 μg/ml were ± 4.3% and ± 5.1% (n=10), and those for 20 μg/ml were ±3.1 % and ±2.8% (n=10) respectively. The proposed method can be carried out with less than 20μl of serum and compared with fluorescence polarization immunoassay: FPIA (r=0.973). This method is simple, rapid and sensitive and will be applicable to routine works in clinical laboratories.View full abstractDownload PDF (674K) -
Yoshikazu YAMAMURA, Katsuyoshi UCHINO, Akemi AKIBA, Yukiya SAITOH, Fuj ...1986 Volume 35 Issue 3 Pages 268-271
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTwo detection methods for abused anthraquinone derivativc-containing laxatives (ADL) in urine based on the coloration by 1, 8-dihydroxyanthraquinone derivatives (1, 8-OHAD)-aluminum chelation and high performance liquid chromatography (HPLC) have been developed. Since ADL were generally excreted in urine as 1, 8-OHAD after oral administration, rhein (RH), danthron (DT) and emodin (EM) were detected in the present paper. In case of the coloring method, after adsorption of the urine extracts in organic phase to Bondapak C18/Corasil, 1, 8-OHAD on the resin were separated from urinary componets by using 3 different concentrations of acetonitrile-2% acetic acid solution. The fraction containing 1, 8-OHAD was poured into an alumina column and 1, 8-OHAD were detected as a pinkish coloring due to chelated compound. HPLC was performed on a reversed-phase C18 column using a mobile phase of acetonitrile-2% acetic acid solution (7 : 3, v/v%) with ultraviolet detection (250 nm). The detection limits of RH, DT and EM were 0.1μg in both methods. These methods were applied to 24 h urine samples after oral administration of 5 kinds of ADL to a normal subject. RH, DT and/or EM were detected in each sample. By applying these methods to urine sample of a female patient with hypokalemia, RH was detected in her urine.View full abstractDownload PDF (3429K) -
Bromvalerylurea, amobarbital and gultethimideKazuyo NISHIHARA, Yukinao KOHDA, Hajime KOTAKI, Yukiya SAITOH, Hiroshi ...1986 Volume 35 Issue 3 Pages 272-277
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA screening technique using high performance liquid chromatography (HPLC) and an identification technique based on gas chromatography/mass spectrometry are presented for serum hypnotics of an acute drug intoxicated patient with coma. In addition, an HPLC method for the simultaneous determination of serum bromvalerylurea (BVU), amobarbital (AMB) and gultethimide (GTM) was developed. These drugs were extracted from serum with chloroform containing allobarbital as an internal standard, and chromatographed on a reversed phase column (Nucleosil® 7C18) with a mobile phase of acetonitorile-0.01 M acetate buffer (pH 4.0)=3:7 (v/v). The recoveries of BVU, AMB and GTM from serum sample were 99.3, 100.3 and 99.9%, respectively. The detection limits were0.1, 0.2 and 0.1μg/ml, respectively. This HPLC method was successfully applied to the measurement of serum BVU, AMB and GTM concentrations during treatment of three acute hypnotic intoxicated patients.View full abstractDownload PDF (924K) -
Tatsumi SHINOHARA, Osamu ISHIDAKA, Tsuneo TANAKA, Atsushi MOMOSE1986 Volume 35 Issue 3 Pages 278-282
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and reproducible method for the determination of phenylbutazone(PBZ) and its metabolites, oxyphenbutazone (OPBZ) and γ-hydroxyphenylbutazone (HPBZ), in horse plasma and urine by high performance liquid chromatography (HPLC) was developed. Plasma (0.5 ml) was diluted with 0.5 ml of 2 M acetate buffer (pH 5.0) and extracted with 7 ml of dichlormethane. After centrifugation at 3000 r.p.m. (1600 g) for 10 min, the organic phase was evaporated to dryness under nitrogen stream at 40°C. The residue was dissolved in 200 μl of acetonitrile-water-triethylamine (55 : 42 : 0.5) with sonication and flash mixing. After re-centrifugation at 3500 r.p.m. (2200 g) for 10 min, supernatant was transferred to a micro test-tube and 20μl portion of the solution was applied to HPLC (column : Cosmosil 5C18, 15 cm × 4.6 mm i. d.; column temperature: 40°C; mobile phase: acetonitrile-wateracetic acid, 55 : 42 : 3; flow rate: 1.0 ml/min; detector : UV at 254 nm). It was undesirable for the quantitative analysis that HPBZ was split into two peaks on a chromatogram, because of equilibration of HPBZ with δ-caprolactone-α-carbonic acid-N, N'-diphenylhydrazide in the mobile phase. However, this isomerization could be prevented by dissolving the sample in a solution containing trace amount of triethylamine. The retention times of HPBZ, OPBZ, methenolone (internal standard) and PBZ were 4.1, 5.3, 8.1 and 12.8 min, respectively. Urine (0.25 ml) was treated by the same procedure, except that extraction with 7 ml of benzene and mobile phase, acetonitrile-water-acetic acid (49 : 48 : 3), were used. The detection limits of each metabolite from plasma and urine were 0.25 μg/ml and 0.5 μg/ml, respectively. The proposed method is reproducible for the assay of PBZ and its metabolites in plasma and urine, and applicable to the pharmacokinetic studies of the drug in horses.View full abstractDownload PDF (947K) -
Hirofumi SUZUKI, Shigeru FUJIWARA, Kouichi AKIMOTO, Isao SUGIMOTO1986 Volume 35 Issue 3 Pages 283-287
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and sensitive high performance liquid chromatographic assay was developed for the determination of phenylpropanolamine (PPA) in plasma using a single-step solvent extraction and pre-column fluorescence derivatization with NBD-F (4-fluoro-7-nitrobenzo-2-oxa-1, 3-diazole). To 0.5 ml of plasma were added an internal standard {(1S, 2S)-(+)-2-amino1, 3-propanedio} and 0.5 ml of 0.1 M NaOH, and the sample was extracted with 6 ml of ethyl acetate. After centrifugation, 5 ml of the ethyl acetate layer was evaporated to dryness under a stream of nitrogen and the residue was mixed with 150 μl of 67 mM phosphate buffer (pH 7.0). A 50μl aliquot of the solution was mixed with 50μl of a 10 mM NBD-F solution in ethanol. The mixture was allowed to react at 80°C for 5 min in the dark, and the reaction was stopped by acidification with 15 μl of 0.1 M HCl. A 10 μl aliquot of the solution was analyzed by HPLC on a Lichrosorb RP-18 column (5μm, 125 mm × 4 mm i. d.) equipped with a guard column (Corasil-C18) with 50% methanol containing 0.1% phosphoric acid as mobile phase (1 ml/min). Fluorometric detection was done at excitation and emission wavelengths of 470 nm and 533 nm, respectively. The retention times for PPA and the internal standard were 8 min and 4 min, respectively. The detection limit was 2 ng/ml and the assay gave a linear response in the range of 5400 ng/ml. The within-day relative standard deviation from 10 to 200 ng/ml were 1.23.9%, the day-to-day relative standard deviation were 3.3% at 50 ng/ml and 2.0% at 150 ng/ml. This method was successfully used for monitoring of PPA in dog plasmas after oral administration.View full abstractDownload PDF (689K) -
Hitoshi NOHTA, Etsuko YAMAGUCHI, Akane MITSUI, Kenji OHTSUBO, Yosuke O ...1986 Volume 35 Issue 3 Pages 288-292
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIsoproterenol has been employed as a bronchodilator and a cardiac stimulant. A simple and highly sensitive method for the determination of free isoproterenol and total isoproterenol (the sum of free isoproterenol and its major metabolite, isoproterenol sulfate) in human plasma and urine by high performance liquid chromatography with fluorescence detection has been established. After strong cation-exchange chromatography on a Toyopak SP cartridge, free isoproterenol and N-methyldopamine (internal standard) in plasma or urine are converted into the corresponding fluorescent compounds by reaction with 1, 2-diphenylethylenediamine in aqueous acetonitrile in the presence of potassium hexacyanoferrate (III). These compounds are separated within 8 min on a reversed phase column, TSK-gel ODS 120T with isocratic elution using a mixture of methanol and 50 mM tris-hydrochloric acid buffer (pH 7.0) (4 : 1, v/v). Isoproterenol sulfate is hydrolyzed by heating with perchloric acid at 100°C for 20 min to isoproterenol. The detection limit for isoproterenol is 15 fmol in a 50-μl injection volume. This method can be applied to monitoring isoproterenol in plasma and urine.View full abstractDownload PDF (794K) -
Tomiharu ITO, Masahiro ABE, Fumihiko IMAMURA, Yasuhiko MATSUKI, Toshio ...1986 Volume 35 Issue 3 Pages 293-297
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSGas chromatography/mass spectrometric method for determination of ifenprodil in plasma and urine is described. The clean-up of ifenprodil in plasma and urine was efficiently attained by extraction with ethyl acetate under acidic and basic conditions, and that of conjugated ifenprodil was carried out by the use of Clin Elut cartridge after hydrolysis with hydrochloric acid. Ifenprodil was converted into the trimethylsilyl derivative and subjected to GC/MS. The quantitation limit of ifenprodil was 150 pg/ml plasma and the recovery rates of ifenprodil added to plasma and urine were 96.9% and 88.1%, respectively. The plasma and urine levels of ifenprodil after oral administration of the drug to human volunteers and dogs were determined by the proposed method.View full abstractDownload PDF (676K) -
Akihiko NAKAGAWA, Yukimi TANISHIMA, Takashi HIROTA, Hidekuni TAKAHAGI, ...1986 Volume 35 Issue 3 Pages 298-302
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of CS-570, a chemically stable prostacyclin analogue, was developed by using immobilized antibody column followed by GC/ MS. The CS-570 antibody, obtained from rabbit serum after giving CS-570-BSA for three months, was coupled to Sepharose 4B and the immobilized antibody was used as extraction phase for clean-up of the drug. A plasma sample, spiked with d6-CS-570 as internal standard, was applied to the immobilized antibody column. After washing the column, CS-570 was eluted with 90% acetonitrile solution. Negativeion chemical-ionization mass spectrum of the pentafluorobenzyl-trimethylsilyl derivative showed the intense ion at m/z (M-181) when ammonia was used as reagent gas. This ion was used for selective ion monitoring. Reproducibility (R.S.D.) was 2.4% (n=3) at the 12 ng/ml level and the limit of determination was 0.1 ng/ml when 1 ml sample was available. The clean-up method based on immobilized antibody column was superior to the conventional procedure due to its higher selectivity and efficiency.View full abstractDownload PDF (760K) -
Kusuo NARITA, Hisayo KITAMURA1986 Volume 35 Issue 3 Pages 303-305
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn this study, melting curve which shows the relationship between temperature and light transmittance of the sample, was obtained by use of a Mettler FP-1 automatic melting point instrument. Temperature was elevated at a rate of 0.02 K/min near the beginning of melting. In the presence of reference material, the purity of a sample could be evaluated from the comparison of melting point lowering rates of the sample and the reference material. On the other hand, in the absence of the reference, the purity of a sample could be evaluated by a modified comparative method. This method is based on the result that the melting point of a pure substance coincides with the temperature of intersecting point of two lines, which are obtained by plotting melting points and half changed points of melting curves of samples containing known ratios of contaminant.View full abstractDownload PDF (581K) -
Nobuharu GOTO, Masahiro HOSOYA, Shinroh SETOGUCHI1986 Volume 35 Issue 3 Pages 306-308
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSStability of new antitumor agent, S-(N-rnethylcarbamoyl)-L-cysteine ethyl ester hydrochloride (Y-6430) was studied. Y-6430 and its analogues were incubated in 20 mM phosphate buffer (pH 7.5) at 37°C and residual contents were determined by high performance liquid chromatography (HPLC) with a photodiode array detector {column: Cosmosil 5C18; mobile phase: linear gradient from 20 mM KH2PO4 to 20 mM KH2-PO4-Methanol(1 : 1) in 20 min; flow rate: 1.0 ml/min} Half-lives of Y-6430 and its analogues in the buffer were 200 min and 5010 min, respectively. Decomposition of Y-6430 was remarkably accelerated by the addition of L-cysteine or L-glutamine. Decomposition products from Y-6430 solution incubated with or without L-cysteine were isolated by HPLC and their chemical structures were proposed on the basis of their ultraviolet absorption, nuclear magnetic resonance and mass spectra. The products isolated from Y-6430 solution incubated with L-cysteine were formed as the result of elimination of its ethyl moiety. On the other hand, elimination of N-methylamine, N-methylcarbamoyl and N-methylisothiocyanate moieties predominated in the solution incubated without L-cysteine.View full abstractDownload PDF (509K) -
Masaaki ISHIKAWA, Masatoshi YAMAMOTO, Toshio MASUI, Kazuichi HAYAKAWA, ...1986 Volume 35 Issue 3 Pages 309-311
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of inorganic ions in aqueous infusions was studied by photometric ion chromatography(PIC) using a conventional HPLC system equipped with a UV monitor. Inorganic cations(Na+, K+, Mg2+ and Ca2+) could be separated on a strong cation exchange column, Oyobunko ASC-4000 column (4.6 mm i.d.×250 mm), with 1×10-4 M CuSO4 for Na+, K+ and 2×10-3 M CuSO4 for Mg2+, Ca2+ as eluents, and detected at 220 nm. Inorganic anions (Cl- PO43- and SO42-) could be separated on a strong anion exchange column, Oyobunko ASA-4000 column (4.6 mm i.d.×250 mm), with 1×10-3 M disodium phthalate (pH 10) as an eluent, and detected at 260 nm. A sample solution was simply diluted with distilled water, and could be analyzed by PIC. Relative standard deviations (n=5) for above ions in a commercial infusion were below 2.0%.View full abstractDownload PDF (546K) -
Naobumi Ôr, Yonezo MATSUMOTO, Hajimu KITAHARA, Hisako MIYAZAKI1986 Volume 35 Issue 3 Pages 312-313
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDirect enantiomeric separation of α-methylarylacetic acid anti-inflammatory agents has been studied by high performance liquid chromatography with a chiral stationary phase, N-3, 5-dinitorobenzoyl-(R)-phenylglycine chemically bonded to aminopropyl silica gel. Enantiomers of fenoprofen, ketoprofen and pranoprofen were separated with good separation factors (α=1.06, 1.05 and 1.04). It is very noticed that these α-methyl-arylacetic acid enantiomers can be separated without any pre-derivatization such as amidation or esterification. These results suggest that enantiomers of another aromatic carboxylic acid may be also resolved directly with this chiral stationary phase.View full abstractDownload PDF (299K) -
Yukio ASO, Sumie YOSHIOKA, Toshio SHIBAZAKI, Mitsuru UCHIYAMA1986 Volume 35 Issue 3 Pages 314-316
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe high performance liquid chromatography using chiral mobile phase containing L-phenylalanine-copper (II) complex was evaluated for purity test and stability test of L-Dopa preparations. The influences of the complex concentration and methanol content in the mobile phase on the separation of D- and L-Dopas were studied. The complex concentration had little influence on the separation, while the decrease in methanol content increased the retention time and the resolution. The detection limits obtained with UV detector and electrochemical detector were compared, and it was found that electrochemical detector could detect much less D-Dopa in the presence of L-Dopa than UV detector. D- and L-Dopas in tablets were determined simultaneously by connecting a UV detector and an electrochemical detector in series.View full abstractDownload PDF (433K) -
Toshinobu HONDO, Muneo SAITO, Masaaki SENDA1986 Volume 35 Issue 3 Pages 316-319
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWe have already reported the new double-stage separation method which combines supercritical fluid. extraction (SFE) directly with supercritical fluid chromatography (SFC). The new SFE/SFC method incorporates SFE as the first separation step and SFC as the second separation step. This arrangement allows the analyst to apply raw and solid samples directly to the system. In addition, the use of SFE/SFC enables true SFC which is not affected by the solvent, that often plays a role of modifier only for early eluting peaks, used for dissolving samples. Here, application of this method to the analysis of vitamin Ks is described. A solution of vitamins K1, K2 and K3 were dried on a piece of filter paper, then applied to the SFE/SFC system. Stopped-flow extraction was performed at 40 °C with 200 bar pressure for 2.5 min, then the extract was directly introduced into the SFC system. All the three vitamins were completely separated on a silica gel column within 4.5 min using supercritical carbon dioxide (2.0 1 /min) with acetonitrile (0.1 ml/ min) as a modifier. The relative standard deviation of the retention times was less than 2.0% for ten consecutive runs.View full abstractDownload PDF (568K) -
Yoshinobu AKADA1986 Volume 35 Issue 3 Pages 320-322
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and rapid method was developed for the determination of calcium pantothenate(Pa-Ca) or panthenol(Pol) in pharmaceutical preparations by high performance liquid chromatography(HPLC). They could successfully be separated on a column of Nucleosil 5C18 with a mixture of 10 mM phosphate buffer (pH 3.0)-acetonitrile (97 : 3) as a mobile phase and detected at 208 nm. Aqueous extract from a preparation was applied to a Chemco-Sep ODS-A pretreatment column, and Pa-Ca and Pol were eluted with the above mobile phase. The eluate was made up to a constant volume and injected to HPLC system. The contents of Pa-Ca and Pol in the preparation were calculated by using calibration curves based on their peak heights on HPLC chromatogram. Several vitamin preparations were analyzed by the proposed method.View full abstractDownload PDF (352K) -
Ryoko CHIBA, Yoko ISMI1986 Volume 35 Issue 3 Pages 323-326
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the simultaneous determination of yohimbine hydrochloride and methyltestosterone in a tablet by high performance liquid chromatography (HPLC) was established. Yohimbine hydrochloride and methyltestosterone in the tablet were extracted with methanol. Chromatographic separation was achieved on a reversed phase column packed with Hitachi Gel #3056 using a mobile phase of methanol-water0.2 M ammonium phosphate(pH 3) (70 : 30 : 2 in v/v). The eluate was monitored with an ultraviolet detector at a wavelength of 270 nm. Determination was carried out successfully by using homosulfamine as an internal standard. Recoveries of yohimbine hydrochloride and methyltestosterone from mixture of standards were quantitative. The relative standard deviation for them were less than 2.0%. By this chromatographic method, these components in commercial tablets could be si multaneously determined without any interference. The method is rapid with a total analysis time of within 10 min.View full abstractDownload PDF (692K) -
Kazuhiko SAGARA, Yuji ITO, Mitsuharu OJIMA, Toshiyuki OSHIMA, Tsuguchi ...1986 Volume 35 Issue 3 Pages 326-329
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBerberine, palmatine and coptisine in Coptidis Rhizoma, Phellodendri Cortex and their oriental pharmaceutical preparations were determined by ion pair high performance liquid chromatography. Coptidis Rhizoma obtained in China had two unknown peaks which were not detected in that of Japan, and the ratios of palmatine to berberine in Chinese sample were ranged from 9.1 to 41.5%, meanwhile those in Japanese sample were from 1.4 to 4.8%. Discrimination between Chinese sample and Japanese one is possible from the ratio of these alkaloids. On the other hand, regarding Phellodendri Cortex constitutive difference between Chinese sample and Japanese one was not obtained. The recoveries of the alkaloids in the decoction of oriental pharmaceutical preparation were lower by 5093% than that of the powders, and those in even shichimotsukoka-to which did not contain Glycyrrhizae Radix and Rhei Rhizoma were decreased in its decoction was lower by about 50% than the powder. It was suggested that there were any components in Paeoniae Radix, Cnidii Rhizoma and Uncariae Ramulus which interacted with berberine-type alkaloids.View full abstractDownload PDF (623K) -
Masaaki KAI, Yasuhiro SAKAMOTO, Tetsuro MIURA, Yosuke OHKURA1986 Volume 35 Issue 3 Pages 329-332
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA high performance liquid chromatographic method is described for the determination of antipain which is a protease inhibitor and also a possible therapeutic drug for muscular destrophy. Antipain was converted to the fluorescent derivative by reaction with benzoin, a fluorogenic reagent for guanidino group. The derivative was then determined on a reversed phase column with isocratic elution within 15 min by using fluorescence detector. The detection limit of antipain in mouse serum was 0.42μg/ml, which corresponds to the amount of 240 pg (400 fmol) in an injection volume of 100μ1 at a signal to noise ratio of 2. The calibration graph for the compound was linear up to at least a concentration of 30 μg/ml in the serum. The proposed method was simple, rapid and sensitive enough to permit the quantification of antipain in as little as 40 μl of mouse serum dosed with the compound.View full abstractDownload PDF (704K) -
Osamu ISHIDAKA, Tatsumi SHINOHARA, Tsuneo TANAKA, Atsushi MOMOSE1986 Volume 35 Issue 3 Pages 332-334
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA high performance liquid chromatographic procedure was developed for the quantitative analysis of mefenamic acid in horse plasma. To a 0.25 ml plasma sample, 25 μg of internal standard was added, and was extracted with methylene chloride under acidic conditions. Portions of the organic layer were evaporated to dryness under nitrogen gas. 'The residues were reconstituted in methanol and injected onto a column packed with Cosmosil 5C18. The elution was performed with a mixed solvent of methanol and 2% acetic acid (70 : 30, v/v) at 40°C. The flow rate was 2 ml/min, and the effluent was monitored at 352 nm. Mefenamic acid and the internal standard eluted at 8.8 and 11.2 min, respectively. The peak area ratio (mefenamic acid/internal standard) versus plasma concentration was linear in the range of 0.150μg/ml of mefenamic acid in plasma, and the detection limit of mefenamic acid was 0.05μg/ml. This method was successfully applied to the determination of mefenamic acid in the horse plasma after drug administration.View full abstractDownload PDF (398K) -
Gen TAMAI, Hisanobu YOSHIDA, Hideo IMAI1986 Volume 35 Issue 3 Pages 335-337
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSButyl Toyopearl (BT) 650-M (Toyo Soda Co.), a polyvinyl resin with butyl and hydroxyl surface groups, of which the former exhibits hydrophobic interaction with proteins, was used to deproteinize the serum samples for the direct injection HPLC analysis of drugs. It was found that 0.050.75% trichloroacetic acid, 0.054.0% of trifluoroacetic acid or 0.0250.5% perchloric acid (PCA) was effective for the adsorption of BSA on BT 650-M as well as conventional 2050% ammonium sulfate solution. In 0.5% PCA solution the quantity of BSA adsorbed was about 40 mg/ml wet gel. For eluting BSA by the reversible desorption, the salting-in (optimum at about 0.2 M phosphate solution, pH 7.0), solubility increase in methanol (tested up to 30%) and hydrogen bond breaking by 5 M urea increased the peak height by 15, 4 and 2.5 times, respectively, than the case of elution by water. It seemed that the hydrogen bonding also functioned for the adsorption. The method was applied to the HPLC determination of 6-mercaptopurine (6-MP), theophylline(TP) and chlorpromazine (CPZ) spiked in rabbit serum at the therapeutic concentration. An excellent reproducibility (R.S.D. : 1.8% for 6-MP, 0.78% for TP and 2.1% for CPZ) and good recovery (99.7% for 6-MP, 100.0% for TP and 99.2% for CPZ), regardless of their binding ratio to serum proteins, were ascertained. The use of column switching for troika column system, a BT 650-M precolumn, a minicolumn which trapped analytes and an analytical column, was recommended in order to protect BT 650-M which was fragile at high pressure.View full abstractDownload PDF (315K) -
Hideyuki NISHIZAWA, Yoshihiro ABE1986 Volume 35 Issue 3 Pages T7-T11
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA very handy and economical system, possible to perform zone electrophoresis, SDS electrophoresis, isoelectric focusing and two-dimensional electrophoresis, was described. The premanufactured and stored gel (0.5 mm in thickness) had advantages in short time for practice and treatment before and after use. Combined with a simple apparatus, the system was found to be useful for the routine work of electrophoretic investigations.View full abstractDownload PDF (1170K) -
Formulation of retinyl palmitate soft capsule and evaluation of its quality and stabilityTakao INOUE, Yukio SHOJI, Yasuji TAKASHIMA, Reijiro KOHNO, Hitoshi EZA ...1986 Volume 35 Issue 3 Pages T12-T15
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSVitamin A contents are often determined by high. performance liquid chromatographic method in laboratories, but the reference standard is available only for thin-layer chromatography. Vitamin A palmitate reference standard was prepared by diluting retinyl palmitate ( JP grade, about 1700000 IU/g) to 200000 IU/g with middle chain triglyceride (MCT) and was packed in gelatin soft capsule. This reference standard was evaluated in 12 laboratories by TLC, UV and HPLC methods. Stability testing was carried out with this sample stored in 50°C, 40°C, 25°C and room temperature for 6 months. The stability result of this reference standard was better than expected.View full abstractDownload PDF (635K) -
Minoru SAWADA, Ichiro MOTOYAMA, Sachiko YAMADA, Yoshikiyo KANAYA1986 Volume 35 Issue 3 Pages T16-T21
Published: March 05, 1986
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn automated assay for many kinds of phenothiazine drugs using a palladium chloride solution was established. by application of a continuous flow analysis. The procedure was as follows: Dissolve a sample in a mixture of 0.625 M sulfuric acid and dimethylformamide(DMF) (2 : 3) to make about 3 × 10-3 M solution. A standard solution was prepared in the same way. A 4.2 × 10-3 M palladium chloride stock solution was prepared by dissolving palladium chloride in 0.625 M sulfuric acid and diluted with DMF(4 : 1) before use. Using automatic analyzer, the sample solution was diluted with a mixture of 0.625 M sulfuric acid and DMF(4 : 1) to one seventh concentration, and the diluted sample solution was added to the six fold volume of the palladium chloride solution. Determine the absorbance of this mixture at 490 nm. The accuracy was 99, .100% except pharmaceutical preparations containing excess of chloride and the reproducibility was 0.10.3% (n=5). It was possible to assay up to 30 samples per day which are 2 to 3 times as many as those handled manually. The continuous variation methods showed that the palladium complex was composed of Pd and phenothiazine by 1 to 1. The absorption at about 490 nm resulting from the palladium complex was affected by substituents at 2- and 10-positions of a phenothiazine ring.View full abstractDownload PDF (717K) -
Hiroaki TAKAHASHI, Hiroyuki MORIYAMA, Kenichi MATSUBARA, Makoto FUKAMA ...1986 Volume 35 Issue 3 Pages T22-T27
Published: March 05, 1986
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe protein-coated ODS column (TSKprecolumn BSA-ODS) or chemically treated silica column (TSKprecolumn SW) was used for the enrichment of the drugs and the removal of proteins in plasma or serum. The enriched drugs in the precolumn are introduced automatically to the analytical column using the column switching device. Drugs such as theophylline or ethosuximide were analysed successively within 15 min including sample preparation. The drugs in plasma can be analysed with good recovery and good precision.View full abstractDownload PDF (967K)
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