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卢克等人测定水果和蔬菜中多种农药残留的方法:协同研究。

The Luke et al. method for determining multipesticide residues in fruits and vegetables: collaborative study.

作者信息

Sawyer L D

出版信息

J Assoc Off Anal Chem. 1985 Jan-Feb;68(1):64-71.

PMID:3980415
Abstract

Ten laboratories analyzed unfortified and fortified samples of lettuce, tomatoes, and strawberries for organochlorine and organophosphorus pesticides by applicable portions of the comprehensive multipesticide method of Luke et al. The 3 crops were fortified with 6 pesticides, alpha-BHC, dieldrin, chlorpyrifos, acephate, omethoate, and monocrotophos, each at 3 levels per crop. Included in the 54 fortifications were 16 pairs of blind duplicates: same pesticide, crop, and level. Recoveries were calculated by area comparisons with known reference materials, using the responses obtained from 2 separate element-specific gas chromatographic (GC) systems. The organochlorine pesticides were chromatographed on a methyl silicone column and detected with a Hall 700A electrolytic conductivity detector, and the organophosphorus pesticides were determined with a flame photometric detector after being chromatographed on a specified DEGS column material. Chlorpyrifos was quantitated on both GC systems. Mean recoveries ranged from 82.6% for acephate fortified at 0.5000 ppm in strawberries to 118.1% for 0.0636 ppm fortification of chlorpyrifos in lettuce. Interlaboratory coefficients of variation ranged from 4.0% for 0.6360 ppm fortification of chlorpyrifos in tomatoes to 17.8% for the 0.0636 ppm chlorpyrifos level in lettuce. The procedure features essentially no cleanup before GC and proved comparable to existing multiresidue methods for pesticides of the class types studied, as evidenced by the intra- and interlaboratory measurements of precision and recoveries obtained. The method with the 2 GC systems has been adopted official first action.

摘要

十个实验室采用Luke等人的综合多农药方法的适用部分,对生菜、番茄和草莓的未强化和强化样本进行有机氯和有机磷农药分析。这三种作物分别用六种农药进行强化,即α-六六六、狄氏剂、毒死蜱、乙酰甲胺磷、氧乐果和久效磷,每种作物每种农药设三个强化水平。在54次强化分析中包括16对盲样重复:相同的农药、作物和水平。回收率通过与已知参考物质的面积比较来计算,使用从两个单独的元素特异性气相色谱(GC)系统获得的响应。有机氯农药在甲基硅氧烷柱上进行色谱分离,并用Hall 700A电解电导检测器检测,有机磷农药在特定的DEGS柱材料上进行色谱分离后,用火焰光度检测器测定。毒死蜱在两个GC系统上都进行了定量分析。平均回收率范围为:草莓中乙酰甲胺磷强化水平为0.5000 ppm时为82.6%,生菜中毒死蜱强化水平为0.0636 ppm时为118.1%。实验室间变异系数范围为:番茄中毒死蜱强化水平为0.6360 ppm时为4.0%,生菜中毒死蜱水平为0.0636 ppm时为17.8%。该方法的特点是在气相色谱分析前基本无需净化,并且通过实验室内和实验室间的精密度和回收率测量证明,与所研究的这类农药的现有多残留方法相当。采用两个GC系统的该方法已被正式首次采用。

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