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Multiresidue Determination of Pesticides in Fruits and Vegetables by Gas Chromatography/Mass Spectrometry/Selected Ion Monitoring

以氣相層析/質譜分析法建立蔬果中農藥之多重殘留量檢驗方法

摘要


本研究評估了以稍加修飾之Luke多重殘留農藥萃取法自蘋果、葡萄、胡瓜、甘藍及小白菜五種作物中萃取captan,chlorothalonil,cyanofenphos,dichlorvos,dimethoate,EPN,fonofos,mevinphos,phenthoate,phorate,pirimiphos-methyl及prothiophos十二種殘留農藥,再以gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM)進行偵測之多重殘留檢驗方法。十二種農藥在2~50 ng/μl濃度範圍內之標準曲線均呈線性,其迴歸係數(r)界於captan的0.939與phenthoate的0.999之間。添加0.5 ppm各種農藥於五種蔬果之回收情形,除captan在五種作物中之最低偵測極限均大於0.5 ppm外,其餘十一種農藥在五種作物中之回收率在46.3到108.3%之間,變異係數界於0.7到19.0%,平均為7.5%。本方法最低偵測極限除captan外,其餘十一種農藥在五種作物中可達0.1~0.05 ppm。由於質譜儀比一般傳統的GC檢測器具有較高的分子專一性(molecular specificity),且可設定同時追蹤數百種標的離子(target ions),因此GC/MS方法實為一值得政府機關大力開發,用以監測日常食品中殘留農藥之檢驗方法。

關鍵字

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並列摘要


A multiresidue method using gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) for the determination of captan, chlorothalonil, cyanofenphos, dichlorvos, dimethoate, EPN, fonofos, mevinphos, phenthoate, phorate, pirimiphos-methyl, and prothiophos residues in fruits and vegetables was evaluated. The pesticides were extracted with a slightly modified Luke multiresidue procedure, separated by capillary column gas chromatography, and detected by mass chromatography with a quadrupole mass spectrometer in the electron impact mode. Recovery studies were performed at the 0.5 ppm fortification level of each pesticide in apples, cabbages, cucumbers, grapes and pak-choi. Recoveries were between 46 and 108%. Coefficients of variation were between 0.7 and 19.0%, with an average of 7.5%. The estimated limits of detection of the pesticides in the crops were 0.1-0.05 ppm, except that captan had limits of detection in the crops higher than 0.5 ppm. Because the mass spectrometer is capable of achieving higher levels of molecular specificity as compared to the traditional GC detectors and can be programmed to search for several hundred target inos, GC/MS would be a promising method for regulatory agencies to explore for monitoring pesticide residues in daily food supply.

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