Gas chromatographic simultaneous determination of organophosphorus pesticides in feed after clean-up by gel-permeation chromatography and solid-phase extraction
An analytical method for organophosphorus pesticides in feed was established by capillary column gas chromatography. After water was added to a sample, the pesticides were simultaneously extracted with acetonitrile. The extract was purified with a gelpermeation chromatograph on a stainless-steel col...
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| Published in | BUNSEKI KAGAKU Vol. 46; no. 2; pp. 121 - 130 |
|---|---|
| Main Authors | , , , |
| Format | Journal Article |
| Language | English Japanese |
| Published |
Tokyo
The Japan Society for Analytical Chemistry
01.01.1997
Japan Science and Technology Agency |
| Subjects | |
| Online Access | Get full text |
| ISSN | 0525-1931 |
| DOI | 10.2116/bunsekikagaku.46.121 |
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| Abstract | An analytical method for organophosphorus pesticides in feed was established by capillary column gas chromatography. After water was added to a sample, the pesticides were simultaneously extracted with acetonitrile. The extract was purified with a gelpermeation chromatograph on a stainless-steel column (20 mm i.d. X 300 mm), followed with a Florisil cartridge or a charcoal activate cartridge. The pesticides were simultaneously determined by a gas chromatograph equipped with a FPD on a fussed silica capillary column bonded 5% diphenyl 95% dimethyl polysiloxane or trifluoropropylmethyl polysiloxane (0.25 mm i.d. × 300 mm, 0.25 μm film tiness). The recovery test was conducted with mixed feed and hay (alfalfa) spiked with pesticides at levels of 0.022.0 ppm. Except for metamidophos and tiometon, the mean recoveries at levels of more than 0.02 ppm were in the range of 73119%, and the relative standard deviation of repeatability (RSDr) was within 14%. A cross check test was carried out at 3 laboratories with mixed feed spiked with the pesticides at levels of 1.0 ppm. The mean recoveries were in the range of 80129%, and the relative standard deviation of reproducibility (RSDR) was within 20%. |
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| AbstractList | An analytical method for organophosphorus pesticides in feed was established by capillary column gas chromatography. After water was added to a sample, the pesticides were simultaneously extracted with acetonitrile. The extract was purified with a gelpermeation chromatograph on a stainless-steel column (20 mm i.d. X 300 mm), followed with a Florisil cartridge or a charcoal activate cartridge. The pesticides were simultaneously determined by a gas chromatograph equipped with a FPD on a fussed silica capillary column bonded 5% diphenyl 95% dimethyl polysiloxane or trifluoropropylmethyl polysiloxane (0.25 mm i.d. × 300 mm, 0.25 μm film tiness). The recovery test was conducted with mixed feed and hay (alfalfa) spiked with pesticides at levels of 0.022.0 ppm. Except for metamidophos and tiometon, the mean recoveries at levels of more than 0.02 ppm were in the range of 73119%, and the relative standard deviation of repeatability (RSDr) was within 14%. A cross check test was carried out at 3 laboratories with mixed feed spiked with the pesticides at levels of 1.0 ppm. The mean recoveries were in the range of 80129%, and the relative standard deviation of reproducibility (RSDR) was within 20%. |
| Author | SHIRAI, Yuji HAYAKAWA, Toshiaki SUZUKI, Shigetaka HIBINO, Hiroshi |
| Author_xml | – sequence: 1 fullname: HIBINO, Hiroshi organization: Tokyo Fertilizer and Feed Inspection Station, Ministry of Agriculture, Forestry and Fisheries – sequence: 1 fullname: SUZUKI, Shigetaka organization: Tokyo Fertilizer and Feed Inspection Station, Ministry of Agriculture, Forestry and Fisheries – sequence: 1 fullname: HAYAKAWA, Toshiaki organization: Tokyo Fertilizer and Feed Inspection Station, Ministry of Agriculture, Forestry and Fisheries – sequence: 1 fullname: SHIRAI, Yuji organization: Fukuoka Fertilizer and Feed Inspection Station, Ministry of Agriculture, Forestry and Fisheries |
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| References_xml | – reference: 16) 田中文隆, 川幡 寛, 宗 千幸, 井出あかね, 園田正則, 石川なおみ, 会田重道 : 第16回農薬残留分析研究会講演資料集, p.38(1992). – reference: 2) 金澤 純 : "農薬の環境科学", P.86(1992), (合同出版). – reference: 21) L. P. Hart, W. E. Braselter, Jr. : J. Agric. Food Chem., 31,657 (1983). – reference: 17) 田中文隆, 園田正則, 小倉理恵子, 宗 千幸, 川幡 寛, 深谷晴美, 井出あかね : 第15回農薬残留分析研究会講演資料集, p.31(1991). – reference: 24) 政令第405号, 1997年12月27日. – reference: 3) 木津憲治, 大川秀郎 : "農業と環境から農薬を考える-その視点と選択-", p.63(1994), (ソフトサイエンス社). – reference: 23) 厚生省告示第161号, 1995年8月14日. – reference: 26) 農薬残留分析法研究班 : "最新農薬の残留分析法", p.627(1995), (中央法規出版). – reference: 9) 高橋邦彦, 石井里枝, 飯島正雄, 星野庸二 : 食品衛生学雑誌, 36,607(1995). – reference: 22) 農林水産省畜産局長 : 7畜B第1660号, 1995年11月15日. – reference: 12) 残留分析簡易分析法開発検討委員会 : 食品衛生研究, 45, 7, 12,635(1995). – reference: 18) 石井康雄, 谷内純一, 坂本 剛 : 日本農薬学会誌, 15,231(1990). – reference: 8) 糸山智子, 関口幸弘, 鯉口 智, 平原嘉親, 太田光恵, 木村実如, 三好智子, 成田美加子, 長谷川眞住, 宮田昌弘, 鎌倉和政, 前田憲二, 山名孝善, 外海泰秀 : 食品衛生学雑誌, 36,516(1995). – reference: 27) 富澤長次郎, 上路雅子, 腰岡政二編 : "最新農薬データブック", (1989), (ソフトサイエンス社). – reference: 13) D. L. Stalling, J. L. Tindle : J. Assoc. Off Anal. Chem., 55, 32 (1972). – reference: 15) 田中文隆, 川幡 寛, 鈴木久美子, 宗 千幸, 鈴木あかね, 石川なおみ, 会田重道 : 第17回農薬残留分析研究会講演資料集, p.20(1993). – reference: 1) 咲花茂樹 : 農業及び園芸, 67,154(1992). – reference: 14) L. D. Johnson, R. H. Waltz, J. P. Ussary, F. E. Kaiser : J. Assoc. Off Anal. Chem., 59,174 (1976). – reference: 5) 西島 修 : ぶんせき(Bunseki), 1989,989. – reference: 11) 永山敏廣 : 食品衛生学雑誌, 36,635(1995). – reference: 10) 平井佐紀子, 陰地義樹, 佐々木美智子 : 食品衛生学雑誌, 36,635(1995). – reference: 20) M. E. Stack, S. Nesheim, N. L. Brown, A. E. Pohrand : J. Assoc. Off Anal. Chem., 59,966 (1976). – reference: 4) 小田中芳次 : ぶんせき(Bunseki), 1992,989. – reference: 7) 農林水産省農産園芸局植物防疫課監修 : "農薬要覧", p.473(1991), (日本食物防疫協会). – reference: 6) 児玉 徹 : ぶんせき(Bunseki), 1993,642. – reference: 25) 尾花裕孝, 起橋雅浩, 堀伸二郎, 菊池康介 : 第71回日本食品衛生学会学術講演会要旨集, p.44(1996). – reference: 19) D. M. Holstege, D. L. Scharberg, E. R. Richardson, G. Moller : J. Assoc. Off Anal. Chem., 74,394 (1991). |
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| SubjectTerms | capillary gas chromatography (GC) charcoal activate cartridge Florisil cartridge gel permeation chromatography (GPC) organophosphorus pesticide |
| Title | Gas chromatographic simultaneous determination of organophosphorus pesticides in feed after clean-up by gel-permeation chromatography and solid-phase extraction |
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