Anastassiades Michelangelo, Lehotay Steven J, Stajnbaher Darinka, Schenck Frank J
U.S. Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 E. Mermaid Ln, Wyndmoor, PA 19038, USA.
J AOAC Int. 2003 Mar-Apr;86(2):412-31.
A simple, fast, and inexpensive method for the determination of pesticide residues in fruits and vegetables is introduced. The procedure involves initial single-phase extraction of 10 g sample with 10 mL acetonitrile, followed by liquid-liquid partitioning formed by addition of 4 g anhydrous MgSO4 plus 1 g NaCl. Removal of residual water and cleanup are performed simultaneously by using a rapid procedure called dispersive solid-phase extraction (dispersive-SPE), in which 150 mg anhydrous MgSO4 and 25 mg primary secondary amine (PSA) sorbent are simply mixed with 1 mL acetonitrile extract. The dispersive-SPE with PSA effectively removes many polar matrix components, such as organic acids, certain polar pigments, and sugars, to some extent from the food extracts. Gas chromatography/mass spectrometry (GC/MS) is then used for quantitative and confirmatory analysis of GC-amenable pesticides. Recoveries between 85 and 101% (mostly > 95%) and repeatabilities typically < 5% have been achieved for a wide range of fortified pesticides, including very polar and basic compounds such as methamidophos, acephate, omethoate, imazalil, and thiabendazole. Using this method, a single chemist can prepare a batch of 6 previously chopped samples in < 30 min with approximately 1 dollar (U.S.) of materials per sample.
介绍了一种用于测定水果和蔬菜中农药残留的简单、快速且廉价的方法。该方法包括先用10 mL乙腈对10 g样品进行初始单相萃取,然后加入4 g无水硫酸镁和1 g氯化钠进行液液分配。通过使用一种称为分散固相萃取(dispersive-SPE)的快速方法同时去除残留水分并进行净化,即将150 mg无水硫酸镁和25 mg伯仲胺(PSA)吸附剂与1 mL乙腈萃取液简单混合。用PSA进行的分散固相萃取能在一定程度上有效去除食品提取物中的许多极性基质成分,如有机酸、某些极性色素和糖类。然后使用气相色谱/质谱联用仪(GC/MS)对可进行气相色谱分析的农药进行定量和确证分析。对于多种强化农药,包括甲胺磷、乙酰甲胺磷、氧乐果、抑霉唑和噻菌灵等极性很强和碱性的化合物,回收率在85%至101%之间(大多数>95%),重复性通常<5%。使用该方法,一名化学家可以在不到30分钟的时间内制备一批6个预先切碎的样品,每个样品的材料成本约为1美元(美国)。