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Volume 49 (2008)
- Issue 6 Pages 381-
- Issue 5 Pages 333-
- Issue 4 Pages 261-
- Issue 3 Pages 125-
- Issue 2 Pages 63-
- Issue 1 Pages 1-
Volume 49, Issue 3
Displaying 1-16 of 16 articles from this issue
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Originals
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Hisaya TERADA, Shoichiro NOGUCHI, Yoshimasa MARUYAMA, Haruyasu KATO, Y ...2008 Volume 49 Issue 3 Pages 125-135
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA rapid analytical method for the simultaneous determination of carbamate pesticides in processed foods was established by liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS). The pesticides were extracted from samples with acetonitrile using accelerated solvent extract equipment, except for the fine powder type spices, which were extracted in an ultrasonic bath. The crude extract was cleaned up with a multi-solvent GPC column (Shodex Asahipak GF-310 HQ) using acetonitrile as a mobile phase. The eluent from the column at the retention time between 13 to 18 min was concentrated under nitrogen gas and dissolved in a mixture of acetonitrile-water-0.2 mol/L ammonium formate buffer pH 6.0 (10 : 9 : 1). An aliquot was injected into the LC/MS/MS using electrospray ionization (ESI) with acquisition in the positive mode.
The recoveries of 29 kinds of pesticide from dried fruits (raisin, prune and mango) and spices (turmeric, masala, sage, thyme and red pepper) fortified at levels of 0.1 and 0.01 μg/g were mostly in the range of 50 to 150% and those from soybean paste and soy sauce fortified at 0.01 μg/g were 46.9 to 122.6% (C.V. 3.8 to 37.6%), except for 4 kinds of pesticide. The determination limits (S/N≥10) corresponded to 0.001 to 0.05 μg/g of the pesticides in red pepper.View full abstractDownload PDF (848K) -
Hiroyuki TADA, Hiroyuki NAGAI, Koichi SHIRAKI, Yoshihiro DEYASHIKI2008 Volume 49 Issue 3 Pages 136-140
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simplified method for the determination of benzylaminopurine in agricultural products by LC/MS was investigated. Benzylaminopurine in agricultural products was extracted with acetone and the extract was concentrated to below 30 mL. Buffer solution of pH 9.0 and ethyl acetate were added to the residue, and the solution was shaken. The ethyl acetate layer was evaporated to dryness, and the residue was dissolved in acetone-n-hexane (1 : 1). The solution was applied to a SAX/PSA mini-column, which was then rinsed with acetone-n-hexane (1 : 1). Benzylaminopurine was eluted with acetone-n-hexane (1 : 1) containing 1% water. The eluates were evaporated to dryness, and the residue was dissolved in 10 mmol/L ammonium acetate-methanol (1 : 1). Benzylaminopurine was analyzed by LC/MS. The MS detection was performed in the selected ion monitoring (SIM) mode, with detection of the M+H+ ion of benzylaminopurine (m/z 226) generated by electrospray ionization (ESI). Recoveries of benzylaminopurine from 15 agricultural products were in the range of 83.1-97.2%. The limits of detection (S/N=3) of benzylaminopurine in all samples except green tea and in green tea were 0.0003 and 0.0012 μg/g, respectively.View full abstractDownload PDF (581K) -
Machiko SAKA, Kazuaki IIJIMA, Mayumi NISHIDA, Yukiko KOMA, Naomi HASEG ...2008 Volume 49 Issue 3 Pages 141-149
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSThe effects of processing and cooking on the levels of pesticide residues in rice samples were investigated for 11 pesticides in pre-harvest (9 pesticides) and post-harvest (4 pesticides) samples. In the polishing process, the transfer ratio (%, total pesticide residue amount in product/that in brown rice) of rice bran ranged from 40% to 106%, and the transfer ratio of polished rice ranged from 9% to 65% in pre-harvest samples. These values varied from pesticide to pesticide. The processing factor (the concentration (mg/kg) of pesticide in product/that in the brown rice) of polished rice ranged from 0.11 to 0.73. The loss of pesticides during processing and/or cooking did not correlate to any single physical or chemical property. Investigation of changes of pesticide residues during processing and/or cooking is useful not only to establish MRLs, but also to recognize actual levels of pesticide residues in food.View full abstractDownload PDF (1504K) -
Machiko SAKA, Kazuaki IIJIMA, Mayumi NISHIDA, Yukiko KOMA, Naomi HASEG ...2008 Volume 49 Issue 3 Pages 150-159
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSThe effects of processing and cooking on the levels of pesticide residues in wheat samples were investigated for 13 pesticides in pre-harvest (Pre, 9 pesticides) and post-harvest (Post, 6 pesticides) samples. In the milling process, the transfer ratios (%, total pesticide residue amount in product/that in wheat grain) of wheat bran were greater than 70% and 80% for pre-harvest and post-harvest samples, respectively. The transfer ratios of flour ranged from 1.7% to 23% (Pre) and 4.0% to 11% (Post). There was no significant difference in transfer ratio among the pesticides investigated. The processing factors (Pf, the concentration (mg/kg) of pesticide in product/that in the wheat grain) of flour ranged from 0.030 to 0.40 (Pre) and 0.069 to 0.18 (Post). The values in pre-harvest samples were higher than those in post-harvest samples. Investigation of changes of pesticide residues during processing and/or cooking is useful not only to establish MRLs, but also to recognize actual levels of pesticide residues in food.View full abstractDownload PDF (2157K) -
Machiko SAKA, Kazuaki IIJIMA, Mayumi NISHIDA, Yukiko KOMA, Naomi HASEG ...2008 Volume 49 Issue 3 Pages 160-167
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSThe effects of processing and cooking on the levels of pesticide residues in soybean samples were investigated for 14 pesticides in pre-harvest samples. On soaking, the transfer ratios (%, total pesticide residue amount in product/that in soybean) of soaked soybean were greater than 60% for most of the pesticides investigated. The transfer ratio of soymilk ranged from 37% to 92%, and that of tofu ranged from 7% to 63%. The processing factor (Pf, the concentration (mg/kg) of pesticide in product/that in soybean) of tofu ranged from 0.026 to 0.28. These values varied among pesticides. There was a high correlation between the log Pow and the transfer ratio of tofu. The test described here should be useful to obtain the transfer ratios of pesticide residues in processing and/or cooking steps.View full abstractDownload PDF (1187K) -
Masakazu HORIE, Harumi KOBAYASHI, Rie ISHII, Akihiro IBE, Kazuhiro FUJ ...2008 Volume 49 Issue 3 Pages 168-176
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simple and rapid screening method using bioassay for the simultaneous analysis of antibacterials (penicillins, cephalosporins, macrolides, tetracyclines, quinolones, etc.) in meat has been developed. A 5 g sample was homogenized with 5 mL of methanol, and the homogenate was centrifuged for 10 min with 3,000 rpm. The pulp disk method with Bacillus subtilis BGA (Antibiotic Medium 5 (pH 8) and 8 (pH 6)), Micrococcus luteus ATCC 9341 and Geobacillus stearothermophilus as test organisms was employed for the assay of the antibacterials. Typical antibacterials (penicillin G, ampicillin, cefapirin, cefalexin, erythromycin, spiramycin, oxytetracycline, chlortetracycline, streptomycin, dihydrostreptomycin, enrofloxacin and oxolinic acid) were detected at levels of ca. 0.005-2.5 μg/g in meat. Therefore, we recommend this proposed screening method for routine analysis of residual antibacterials in livestock products.View full abstractDownload PDF (607K) -
Shoichiro NOGUCHI, Hisaya TERADA, Yukio TAMURA2008 Volume 49 Issue 3 Pages 177-188
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simultaneous determination of veterinary drugs in livestock food and seafood using liquid chromatography with tandem mass spectrometry (LC/MS/MS) was developed. Veterinary drugs were extracted with 95% acetonitrile. The solution was passed through a Florisil column, and the solvent was replaced with phosphate buffer. The extract was charged on a Sep-Pak Plus C18 mini-column and divided into 40% methanol eluate fraction and 70% acetonitrile eluate fraction. Test solutions were analyzed by LC/MS/MS with gradient elution. By using this method, 37 kinds of veterinary drugs were obtained with over 60% recovery, and quantitation was possible in cattle muscle, egg and fish. This method was inapplicable to 28 kinds of veterinary drugs. Although quantitation was not achieved, 42 other kinds of veterinary drugs can be screened. Since the limit of quantitation for this method is less than the provisional limit in general, it is useful as a screening method in residual analysis of veterinary drugs.View full abstractDownload PDF (727K) -
Hiroko KAJITA, Chizuko AKUTSU, Eriko HATAKEYAMA, Takashi KOMUKAI2008 Volume 49 Issue 3 Pages 189-195
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA multiresidue method was developed for determination of nine aminoglycoside antibiotics (streptomycin, dihydrostreptomycin, spectinomycin, neomycin, kanamycin, gentamicin, destomycin A, apramycin, and tobramycin) in milk by LC/MS/MS. The drugs were extracted with 0.01 mol/L potassium dihydrogen phosphate containing 2% trichloroacetic acid, and the extracted solution was cleaned on cation-exchange cartridge columns (Oasis WCX and Oasis MCX). LC separation was performed on a TSK-gel VMpak25 column (50 mm×2.0 mm i.d.) using gradient elution with 0.1% formic acid and acetonitrile containing 0.1% formic acid as the mobile phase. Recoveries of the drugs spiked at 0.01 or 0.1 μg/g in milk ranged from 66.1 to 110.8%, with a coefficient of variation of less than 17.1%. Limits of quantification of the drugs in milk were 0.001∼0.01 μg/g. This method was used for analysis of milk from a lactating cow treated for clinical mastitis with two intramammary infusions of kanamycin (KM). Milk samples were analyzed during the withdrawal times at 12-hour intervals. KM concentrations were lower than the Japanese provisional MRLs (0.4 μg/g) at 60 hours after infusion, and subsequently fell to 0.01 μg/g.View full abstractDownload PDF (689K) -
Kazuhiro FUJITA, Hironobu ITO, Michiyo ISHIHARA, Sachi INUKAI, Hiroyuk ...2008 Volume 49 Issue 3 Pages 196-203
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSAn efficient clean-up procedure was developed for the trace residue determination of tetracyclines (TCs) in dark-colored honeys. TCs were extracted from samples with McIlvaine buffer (pH 4.0) containing 0.01 mol/L Na2EDTA. The extracts were treated with both a polymeric cartridge (GL-Pak PLS-2) and a metal chelate affinity column (MCAC) preloaded with copper(II). TCs were eluted and analyzed by high-performance liquid chromatography (HPLC) using fluorescence detection. The method was evaluated for the determination of oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) in buckwheat honey, because its color is the darkest. The mean recoveries of OTC, TC and CTC from spiked samples, at three fortification levels, were >70%, and the relative standard deviations (RSDs) were <10%. Limits of quantitation (LOQs) of OTC, TC, and CTC were estimated to be 0.015 mg/kg, 0.019 mg/kg, and 0.024 mg/kg, respectively.View full abstractDownload PDF (290K) -
Masakazu HORIE, Yayoi TABARA, Rie ISHII, Kazuaki HASHIMOTO, Youko YAMA ...2008 Volume 49 Issue 3 Pages 204-210
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA sensitive and selective method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of nitrofurazone (NFZ) in swine muscle, swine liver, chicken muscle, chicken liver, egg, eel, yellowtail and shrimp has been developed. The drug was extracted with 0.2% metaphosphoric acid-methanol (6 : 4), and the extracts were cleaned up on an Oasis HLB cartridge (200 mg). The extracts were analyzed by LC-MS/MS using electrospray ionizationin the negative ion mode. The LC separation was performed on a Hypersil Gold C18 column (15 cm×2.1 mm i.d.) with a gradient system of 0.01% formic acid-acetonitrile as the mobile phase at a flow rate of 0.2 mL/min. The quantitative and confirmatory determination of NFZ was performed by selected reaction monitoring (SRM). The calibration graph for NFZ was rectilinear from 0.2 to 100 ng/mL with SRM. The recoveries of NFZ from samples fortified at 1 and 10 ng/g were 79.6-106.8%, and quantification limit was 0.2 ng/g for the drug. This is well below the detection limit (1 ng/g) set by the Japanese Food Sanitation Law.View full abstractDownload PDF (1208K)
Notes
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Naeo MATSUMOTO, Mayumi YOSHIKAWA, Kuniaki EDA, Ayumi KOBAYASHI, Masumi ...2008 Volume 49 Issue 3 Pages 211-222
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simple preprocessing method was developed for multiresidue determination of pesticides in processed agricultural products. Residues were extracted from homogenized samples with acetonitrile in a glass centrifuge tube, followed by salting-out and partitioning with n-hexane. Co-extractives were removed by means of mini-column clean up. Analysis was performed by GC/MS and LC/MS/MS. The prepared sample solutions were examined for matrix effects. Matrix effects had both positive and negative effects on quantitative value. Calibration was achieved by preparing matrix-matched calibration standards to counteract the matrix effects. Of the 235 pesticides spiked at 0.05 or 0.10 μg/g (Method GC), 0.025 or 0.05 μg/g (Method LC) into 8 foods (garlic paste, diced green sweet pepper, green peas paste, celery paste, sweet potato paste, dried adzuki beans, boiled bamboo shoots, tomato paste), recoveries of 214 pesticides were between 50 and 100% and the coefficient of variation was below 20%. This method is useful as a multi-residue analysis method for screening of pesticides in foods.View full abstractDownload PDF (686K) -
Yasuhiro TAMURA, Ichiro TAKANO, Maki KOBAYASHI, Sanae TOMIZAWA, Yukina ...2008 Volume 49 Issue 3 Pages 223-227
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA method for the determination of hymexazol in agricultural produdcts by gas chromatography with a highly sensitive nitrogen-phosphorus detector (GC-NPD) was investigated. Hymexazol was extracted with acetonitrile, and the acetonitrile layer was separated by salting-out. The water layer was loaded onto a Chem-ElutTM column. Hymexazol in the water layer was adsorbed on the column, and eluted with ethyl acetate. The acetonitrile layer and the eluate were mixed and evaporated. The residue was dissolved in ethyl acetate, and the sample solution was cleaned up on a C18 column. Hymexazol in the eluate was analyzed by GC-NPD with a high-polarity capillary column (DB-FFAP) and highly deactivated inlet liner.
Recoveries of hymexazol spiked in agricultural products (tomato, lemon, soybean and other samples) at the level of 0.1 μg/g ranged from 65.0 to 84.7%. The limit of detection was 0.02μg/g.View full abstractDownload PDF (579K) -
Mizue SAITO, Daisuke KOZUTSUMI, Michiko KAWASAKI, Miho KANBASHI, Ruka ...2008 Volume 49 Issue 3 Pages 228-238
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simple, sensitive and selective method with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS) has been developed to detect 342 pesticides and veterinary drugs contaminating bovine milk at the maximum residue limits (MRLs) defined in the “positive list system”. Sample preparation was performed by extracting the analytes with acetonitrile, followed by salting-out with sodium chloride. For some pesticides, the extract was further cleaned up by n-hexane partitioning and PSA cartridge column chromatography. GC/MS-EI or -NCI was used to determine pesticide residues, while LC/MS/MS-ESI was applicable to the determination of pesticide and veterinary drug residues. The variation of the recoveries of these drugs at MRL was relatively wide; however the relative standard deviations of the recovery of each drug were within 28%, suggesting that the present method is good enough for use as a screening test for contaminants at the MRLs. These results show that this method is useful for multiresidue analysis of numerous pesticides and veterinary drugs in bovine milk.View full abstractDownload PDF (554K) -
Yoh-ichi YATSUKAWA, Kazuhiro FUJITA, Munetomo NAKAMURA, Masatoshi WATA ...2008 Volume 49 Issue 3 Pages 239-243
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simple and rapid LC/MS method for simultaneous determination of sedecamyin (SCM) and terdecamycin (TDM) in livestock products has been developed. SCM and TDM were extracted with acetonitrile. The extract was washed with n-hexane and then evaporated to dryness. The residue was dissolved in methanol, and injected into the LC/MS. The mass spectrometer was operated in the positive electrospray ionization (ESI) mode. LC separation was performed on a high-pH-resistant C18 column with 10 mmol/L carbonic acid-ammonia buffer (pH 10.0)-acetonitrile as a mobile pahse. The recoveries from swine muscle and liver fortified at the levels of 0.01 and 0.05 μg/g were 77-88%, and those from poultry muscle and liver fortified at the levels of 0.01 and 0.3 μg/g were 51-93%. The quantitation limits of SCM and TDM were 0.008 μg/g and 0.005 μg/g, respectively.View full abstractDownload PDF (441K) -
Takao CHONAN, Toru FUJIMOTO, Maki INOUE, Teijiro TAZAWA, Hiroshi OGAWA2008 Volume 49 Issue 3 Pages 244-248
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA simple and rapid multiresidue method was developed for the determination of twelve quinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, nalidixic acid, norfloxacin, ofloxacin, orbifloxacin, oxolinic acid and sarafloxacin) in muscle, liver, chicken eggs, milk, prawn and rainbow trout.
The quinolones were extracted from a sample with acetonitrile-water (95 : 5). A fifth part of the filtered extract was diluted with water to keep the acetonitrile ratio at ca. 60%, and passed through a C18 mini-column. The eluate was evaporated to dryness, and the residues were dissolved in methanol-water (30 : 70) for HPLC analysis.
The quinolones were separated on a Inertsil ODS-3V column (4.6 mm i.d.×250 mm) with a gradient system of 0.1% phosphoric acid-acetonitrile as the mobile phase, with fluorescence detection.
No interfering peak was found on the chromatograms of animal and fishery products, except for milk. The recoveries of the quinolones were over 60% from the animal and fishery products fortified at 0.1 μg/g, and the quantification limits of the quinolones were 0.005 μg/g. This proposed method was found to be effective and suitable for the screening of the quinolones in animal and fishery products.View full abstractDownload PDF (592K)
Report
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Maki KOBAYASH, Ichiro TAKANO, Yasuhiro TAMURA, Sanae TOMIZAWA, Yukinar ...2008 Volume 49 Issue 3 Pages 249-260
Published: June 30, 2008
Released on J-STAGE: July 17, 2008
JOURNAL FREE ACCESSA survey of pesticide residues in 490 imported cereal products on the Tokyo market from April 1994 to March 2006 was carried out. Eight kinds of organophosphorus pesticides (chlorpyrifos, chlorpyrifos-methyl, DDVP, diazinon, etrimfos, malathion, MEP and pirimiphos-methyl) were detected at levels between Tr (below 0.01 ppm) and 0.82 ppm from 91 samples.
In our investigations, chlorpyrifos-methyl and malathion tended to be detected in samples from America, pirimiphos-methyl in those from Europe, and MEP in those from Oceania. Thus, pesticide residues seemed to be different in produce from different areas.
Residue levels of these pesticides were calculated as between 0.08 and 13.2% of their ADI values according to the daily intake of cereal products. Therefore, these cereal products should be safe for normal usage.View full abstractDownload PDF (621K)
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