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Volume 22 (1981)
- Issue 6 Pages 455-
- Issue 5 Pages 339-
- Issue 4 Pages 263-
- Issue 3 Pages 183-
- Issue 2 Pages 113-
- Issue 1 Pages 1-
Volume 22, Issue 6
Displaying 1-18 of 18 articles from this issue
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Yoshiaki ANDO1981 Volume 22 Issue 6 Pages 455-461
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
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Kimihito OTSUKA, Kyoko HORIBE, Akira SUGITANI, Fujizo YAMADA1981 Volume 22 Issue 6 Pages 462-466_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSA method is described for the quantitative determination of clopidol in chicken tissues and eggs by high performance liquid chromatography. Samples were extracted with methanol and the extract was passed through an alumina column and then purified by anion exchange column chromatography with 1% acetic acid in methanol as an eluent. In the case of chicken tissues, the eluate was further purified by alumina column chromatography. The solvent was evaporated off and the residue was dissolved in methanol containing caffeine as an internal standard. Clopidol was separated on a column packed with LiChrosorb RP-18 (5μm) by using acetonitrile-water (10:90, v/v%) as a mobile phase, with detection at 265nm. The recoveries of clopidol added to chicken tissues and eggs at levels of 0.1 to 0.5ppm were 95.1% and 96.8%, respectively. This method was applied to commercial chicken tissues and eggs.View full abstractDownload PDF (564K) -
Studies on Residues of Synthetic Antibacterials in Livestock Products. VNorihide NOSE, Youji HOSHINO, Yoshinori KIKUCHI, Fumiko YAMADA, Akinob ...1981 Volume 22 Issue 6 Pages 467-471_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSThe residual caprylohydroxamic acid (CAP) in chicken and eggs was determined by gas liquid chromatography (GC) with an electron capture detector (ECD) of the derivative formed by reaction with pentafluorobenzoyl chloride (PFB-Cl).
The methanol extract of the sample was cleaned up by ion exchange column chromatography on Amberlite CG-400 (OH form) with 10% sodium chloride-methanol (1→10) mixture as an eluent.
CAP reacted quantitatively with PFB-Cl (20μl) in saturated sodium bicarbonate: methanol (1.5:0.5) solution in a boiling water bath for 2 minutes. The reaction product was subjected to GC after extraction with n-hexane.
GC was performed on a 2m glass column packed with 5% Thermon 1000 and 5% SP-2100 on Gaschrom Q (0.25+1.75). The column temperature was 190°C and the carrier gas (N2) flow rate was 20ml/min. Under these conditions, the retention time of the reaction product is about 12 minutes.
A linear calibration curve was obtained from 0.02ppm to 0.1ppm of CAP. The minimum detectable amount was 20pg of CAP and 0.01ppm in samples. The recoveries of CAP added to chicken and eggs were in the range of 90.7%-90.0%.View full abstractDownload PDF (638K) -
Masaaki IMANAKA, Kazuyoshi MATSUNAGA, Tatsuo ISHIDA1981 Volume 22 Issue 6 Pages 472-478_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSA gas-liquid chromatographic procedure using FPD, which makes use of Trichlorfon (Dipterex, DEP) itself as the indicator peak on the FPD gaschromatogram, has been developed for the determination of DEP in livestock products.
A column of Thermon 3000 on Shimalite TPA with a length shorter than 0.5m was used; DEP gave a very symmetrical peak with a retention time different from those of well-known degradation products such as dimethylphosphite (DMP) and dichlorvos (DDVP). The shape of this peak did not change even when the injection quantity ranged from 0.5 to 4000ng. The peak height were not lowered by co-existing substances in the sample solution. Furthermore, the peak was confirmed to be that of DEP itself by gas chromatography-mass spectrometry. These results enabled us to use the peak as an index for residue analysis.
The recoveries of DEP added to various kinds of livestock products at the level of 0.4ppm ranged from 90.4% (chicken egg) to 102% (cow milk). The detection limit was 2ppb (whole basis).View full abstractDownload PDF (761K) -
Yoji KASUGA, Kimihito OTSUKA, Akira SUGITANI, Fujizo YAMADA1981 Volume 22 Issue 6 Pages 479-483_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSA high-performance liquid chromatographic method for quantitative analysis of nalidixic acid (NA) in fishes has been established.
NA was extracted from fish homogenate in 0.2M phosphate buffer (pH 6.0) with ethyl acetate. The extract was concentrated under a vacuum on a rotary evaporator and the residue was transferred to a separating funnel containing 2% sodium chloride soln. After removal of fat with n-hexane, NA was extracted with chloroform. The extract was concentrated and the residue was transferred to a glass-stoppered centrifuge tube containing 0.1M borate buffer (pH 10.0). The tube was shaken, then centrifuged, and the upper phase was injected into a liquid chromatograph. NA was separated in approximately 5min by using a Zipax SAX column (2.6×500mm) with 0.01M tetraborate soln. (pH 9.1) containing 0.006M sodium sulfate as the mobile phase. The UV detector was set at 258nm. The quantity of NA was calculated from the peak height ratio of NA to piromidic acid used as an internal standard.
The calibration curve was linear over the range from 1 to 100μg/ml.
The recoveries of NA added to the fishes were 96.6 to 100.4% and the detection limit was 0.05μg/ml.View full abstractDownload PDF (492K) -
Yoshihiro IWATA, Akira SUGITANI, Fujizo YAMADA1981 Volume 22 Issue 6 Pages 484-489_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSOrganosulfides in aromatic vegetables such as onion, welsh-onion, leek, garlic and shallot strongly interfere with the analysis of residual organophosphorus pesticides by flame photometric detector-gas liquid chromatography (FPD-GLC).
To overcome this problem, the removal of the interfering substances in onion was investigated by the use of column chromatography.
The method consists of the following procedures: extraction with acetonitrile, concentration of the extract and cleanup on an Amberlite XAD-8 column, and FPD-GLC.
By these procedures, sulfides were efficiently removed to allow good recovery of organophosphorus pesticides added to onion samples, as follows: Diadinon 76%, Malathion 81%, Dichlorvos 82%, Phenthoate 82%, Dimethoate 83%, EPN 85%, Parathion 85%, Phosalon 90%, Chlorpyriphos 92%, Fenitrothion 99%, Fenthion 105%.
The proposed method can also be successfully applied for the analysis of residual organophosphorus pesticides in welsh-onion and leek.View full abstractDownload PDF (620K) -
Studies on nitrite formation in the oral cavity. IIITsuguo SASAKI, Fumie KAMEOKA, Tsutomu ICHIKAWA, Kagenori MATANO1981 Volume 22 Issue 6 Pages 490-495_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSWe measured the intraoral nitrite-producing activity in 100 healthy adults by the “NO3--solution method” and the “NO3--filter paper method” in order to investigate the variations of nitrite-producing activity with age and sex. A fairly high positive correlation (r=0.636, P<0.01) was found between the values obtained by the two methods.
The geometric mean values (95% confidence limits) of nitrite-producing activity in males and females obtained by the “NO3--solution method” were 46.20 (40.33-52.88) and 29.72 (23.61-37.41)μg/min, respectively. The difference between the sexes was significant at the 5% level as determined by the “NO3--solution method”, but there were no statistically significant differences among various age groups in either sex.View full abstractDownload PDF (589K) -
Studies on Residues of Synthetic Antibacterials in Livestock Products. VINorihide NOSE, Youji HOSHINO, Yoshinori KIKUCHI, Fumiko YAMADA, Saju K ...1981 Volume 22 Issue 6 Pages 496-500_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSNicarbazin (NCZ) is an equimolar complex of 4, 4-dinitrocarbanilide (DNC) and 2-hydroxy-4, 6-dimethylpyrimidine.
Gas chromatographic determination with an electron capture detector (ECD) was carried out for p-nitroaniline (NA) obtained by acid hydrolysis of NCZ in a liquid paraffin bath at 150°C for 15 minutes. NA, a reaction product, was extracted with ethyl acetate in the presence of supersaturated sodium chloride in alkaline solution and the NA was determined by gas liquid chromatography.
Gas chromatography: A Shimadzu GC 4CMPFE gas chromatograph with an ECD was used for NA. The column consisted of a glass tube (1mm×3mm ID) packed with 5% Thermon 3000 on Chromosorb W (AW DMCS, 80-100 mesh) and conditioned at 190°C. The temperature of the bath detector and injector was 230°C and the flow rate of nitrogen carrier gas was 20ml/min.
A sample was extracted with methanol in an electric blender. The extract was cleaned up by ion exchange column chromatography on Amberlite CG-400 (OH form). The eluent was a mixture of hydrochloric acid and methanol (2:98).
The recoveries of NCZ added to chicken tissues and eggs were in the range of 85-97%. The minimum detectable concentration was 0.02ppm as NCZ.View full abstractDownload PDF (521K) -
Shinjiro HORI, Takashi KASHIMOTO, Nobuharu KUNITA1981 Volume 22 Issue 6 Pages 501-507_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSPolychlorinated biphenyl (PCB), polychlorinated terphenyl (PCT) and polychlorinated quaterphenyl (PCQ) were administered orally at a dose of 0.2mg per mouse (or 2mg per rat) per day from the 10th day (or 17th day) of pregnancy to parturition.
The accumulation of PCB, PCT and PCQ in the mother and the transfer to fetuses or suckling babies were measured at weekly intervals. The dstribution of the compounds among the internal organs was also investigated.
The amount of PCB or PCT transferred from a mother mouse to suckling babies increased markedly during 14 days after birth, and that of PCQ increased gradually during 21 days after parturition. The accumulation ratio (percent of administered dose transferred from a dam to sucklings aged 14 days) was 16.3% for PCB, 7.3% for PCT and 2.2% for PCQ.
On the other hand, the ratio of transfer from a mother mouse to fetuses was 1/10-1/80 of that from a mother mouse to the sucklings. The transferability was in the order: PCB>PCT>PCQ.
The distribution of the compounds among the internal organs was found to be changed by lactation. The measured accumulation ratios of the compounds in liver and adipose tissue suggest that PCB moves easily from the fat of a dam to the babies, and that much PCT or PCQ is transferred from the liver of a dam to the sucklings.View full abstractDownload PDF (849K) -
Studies on Residues of Synthetic Antibacterials in Livestock Products. VIINorihide NOSE, Youji HOSHINO, Fumiko YAMADA, Yoshinori KIKUCHI, Saju K ...1981 Volume 22 Issue 6 Pages 508-512_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSA procedure for the gas chromatographic determination of Ethopabate (ETP) in chicken tissues and eggs was established as follows. A mixture of 0.5ml of benzene solution of ETP, 70μl of heptafluorobutyric acid (HFB) and 200μl of heptafluorobutyric anhydride (HFBA) was allowed to stand for 15min in a paraffin bath at 220°C. The reaction product was extracted with benzene in alkaline sodium carbonate. The ETP was determined by gas liquid chromatography.
Gas chromatography: A Shimadzu GC 4CMPFE gas chromatograph with an ECD was used for determination of ETP. The column consisted of a glass tube (1m×3mm ID) packed with 5% Thermon 1000 on Chromosorb W (AW, DMCS 80-100 mesh) and conditioned at 190°C. The detector and injector temperatures were 230°C and the flow rate of nitrogen carrier gas was 40ml/min.
The recoveries of ETP added to chicken tissues and eggs were in the range from 90.8 to 96.3 with an average of 94.3% at levels from 0.1ppm to 0.5ppm. The minimum detectable amount was 10pg as ETP and 0.02ppm in a sample. The calibration curve was linear from 0.02ppm to 0.2ppm.View full abstractDownload PDF (518K) -
Shozo FUKUI, Teruhisa HIRAYAMA, Motoshi NOHARA, Yoshihiko SAKAGAMI1981 Volume 22 Issue 6 Pages 513-519_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSAnalysis of total As and some As components (As (III), As (V), monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) in sea foods [Hijiki (Hizikia fusiforme), Konbu (Laminaria japonica), dried shrimp and flat fish (Kareius bicoloratus)] and in urine after ingestion of these foods were carried out by the following methods: the BAL chelate method (As (III), As (V) and MMAA), the ECD-GC method (DMAA) and the wet digestion with Ni2+ and graphite furnace atomic absorption method (total As).
Most of As (more than 90%) in aqueous extracts of Konbu, shrimp and flat fish exists in unidentified bound forms with organic compounds, i. e., not as inorganic or methylated arsenic. A large portion of As (more than 80%) in Hijiki is present as inorganic arsenate and arsenite (60% and 20%, respectively) or as substances releasing inorganic arsenicals in acid media.
Excretion patterns of As in urine after ingestion of these sea foods were as follows: in the case of Hijiki, a large part of As (more than 40% of total excreted As) is excreted as DMAA, while in the case of Konbu, DMAA accounted for most of the excreted arsenic.
On the other hand, in the case of shrimp and flat fish, over 50% of As is excreted as unidentified bound forms with organic compound (s). The As in these foods, except for Hijiki, is rapidly excreted in urine (within 40hr after eating), but prolonged excretion is observed in the case of Hijiki. This may be due to the high inorganic As content in Hijiki.
The As excretion ratios of Hijiki, shrimp and flat fish in urine are 51%, 47.4% and 24.2%. These values suggest that other As components may be incorporated in the body and/or excreted by other routes (in the feces and by expiration).
Furthermore, As components in shrimp were fractionated. An As-containing fraction from dried shrimp appears to be an arseno-oligopeptide, since the fraction gave a positive ninhydrin reaction and yielded arsenobetaine upon acid hydrolysis.View full abstractDownload PDF (814K) -
Metabolic Fate of the Precursors of N-Nitroso Compounds. IVHajimu ISHIWATA, Hiroko MIZUSHIRO, Ayako SAKAI, Akio TANIMURA1981 Volume 22 Issue 6 Pages 520-525_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSThe metabolic fate of nitrate in the lower digestive tract was investigated using Wistar male rats. Little or no nitrate or nitrite was detected in the contents of the digestive tract except that 1232±208ppm of nitrate was found in the stomach contents when rats were fed on a diet containing 5000ppm of nitrate for a week. The secretion of blood nitrate into the lower digestive tract was clearly observed by replacement of the contents with saline in ligated sections of the tract; no nitrate was detected in any ligated sections with contents, but the lower small intestine, cecum and large intestine filled with saline contained 23±13, 35±6 and 46±12ppm of nitrate, respectively, at 15min after the injection of 5mg of nitrate into the abdominal vein.
Nitrate injected into the lower digestive tract was rapidly reduced to nitrite by the contents. Upon simultaneous injection of 250μg each of nitrate and dimethylamine into ligated sections with contents, the formation of N-nitrosodimethylamine was observed at the level of 10-51ppb. Rapid absorption of N-nitrosodimethylamine from the sections was also observed.View full abstractDownload PDF (715K) -
Youko NANASE, Kumiyo TAKATA, Satoshi SHIMAOKA, Shizuyuki DOHI1981 Volume 22 Issue 6 Pages 526-530_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSAn analytical method was investigated for the determination of saccharin by thin layer chromatography-densitometry. Saccharin was separated well from other food additives on a thin layer plate (Kiesel Gel 60 F254) with a hexane-ethyl acetate-formic acid developing solvent system. Fumaric acid, having an Rf value similar to that of saccharin, could be separated from it by the use of hexane-ethyl acetate-formic acid=10:20:0.15.
Calibration plots of concentration vs. the integrated value were found to be linear within the concentration range of 0.5-10μg and the plot could be extrapolated through zero. The limit of detection was 0.2μg as saccharin.
Recoveries of saccharin added to soft drinks, kamaboko, cooked soybeans, tsukudani and tsukemono were 93.3, 91.3, 90.3, 87.1 and 85.1%, respectively, and the accuracy of determination for commercial foods was as good as that of gas chromatographic determination.
The assay of saccharin by thin layer chromatography-densitometry was faster than that by gas chromatography. This thin layer chromatography-densitometry procedure seems to be suitable for the routine analysis of saccharin.View full abstractDownload PDF (575K) -
Hiroshi MOMOKAWA, Waka YAMADA, Fumiko SATO, Keiichi SAKAI1981 Volume 22 Issue 6 Pages 531-535_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSA simple method for the determination of total bromide in foods was investigated.
A 10g sample was ashed with magnesium oxide and dissolved in water. After centrifugation, the solution was oxidized with potassium dichromate sulfuric acid mixture in a bromine generator. The liberated bromine was reacted with fluorescein and quantitated by measurement of the absorbance at 515nm. Chlorine ion did not interfere at up to 1200-fold excess. Iodine ion could be eliminated before the assay by bubbling nitrogen through the solution under mild oxidizing conditions. This method can determine as little as 2.5ppm of bromine in a sample. The recoveries of bromine added to bread and fish jelly products were 98-104%.View full abstractDownload PDF (492K) -
Kimio HIDAKA1981 Volume 22 Issue 6 Pages 536-538_1
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSStyrene polymers and acrylonitrile-styrene copolymers in dimethylformamide solution were precipitated by adding methyl alcohol. Toluene, styrene, ethylbenzene, iso-propylbenzene, and n-propylbenzene in the filtered methyl alcohol solution were determined by high performance liquid chromatography (HPLC) on a Zorbax-ODS column with a mobile phase of methyl alcohol-water (70+30) and with detection at 260nm.
Detection limits by HPLC were 10ppm and 500ppm in the samples analyzed for styrene and other chemicals, respectively. Recoveries of the five compounds added to the resin solution were 93-105%. Styrene in twenty-five samples was determined by the proposed HPLC method. The results are in excellent agreement with those obtained by the accepted GC method.View full abstractDownload PDF (374K) -
Studies on Bromide Residues in Agricultural Products and Processed Foods. IIHisashi KAMIMURA, Motohiro NISHIJIMA, Toshihiro NAGAYAMA, Kazuo YASUDA ...1981 Volume 22 Issue 6 Pages 539-546
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSDownload PDF (781K) -
Hydrocarbon Constituents in Foods. IITakeji CHIKAMOTO, Takeshi MAITANI1981 Volume 22 Issue 6 Pages 547-550
Published: December 05, 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSDownload PDF (492K) -
1981 Volume 22 Issue 6 Pages 562
Published: 1981
Released on J-STAGE: December 11, 2009
JOURNAL FREE ACCESSDownload PDF (55K)
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