Wong Jon W, Webster Michael G, Bezabeh Dawit Z, Hengel Mathew J, Ngim Kenley K, Krynitsky Alexander J, Ebeler Susan E
Alcohol and Tobacco Laboratory, National Laboratory Center, Alcohol and Tobacco Tax and Trade Bureau (formerly the Bureau of Alcohol, Tobacco and Firearms), Ammendale, Maryland 20705-1250, USA.
J Agric Food Chem. 2004 Oct 20;52(21):6361-72. doi: 10.1021/jf040109g.
A method was developed to determine pesticides in malt beverages using solid phase extraction on a polymeric cartridge and sample cleanup with a MgSO4-topped aminopropyl cartridge, followed by capillary gas chromatography with electron impact mass spectrometry in the selected ion monitoring mode [GC-MS(SIM)]. Three GC injections were required to analyze and identify organophosphate, organohalogen, and organonitrogen pesticides. The pesticides were identified by the retention times of peaks of the target ion and qualifier-to-target ion ratios. GC detection limits for most of the pesticides were 5-10 ng/mL, and linearity was determined from 50 to 5000 ng/mL. Fortification studies were performed at 10 ng/mL for three malt beverages that differ in properties such as alcohol content, solids, and appearance. The recoveries from the three malt beverages were greater than 70% for 85 of the 142 pesticides (including isomers) studied. The data showed that the different malt beverage matrixes had no significant effect on the recoveries. This method was then applied to the screening and analysis of malt beverages for pesticides, resulting in the detection of the insectide carbaryl and the fungicide dimethomorph in real samples. The study indicates that pesticide levels in malt beverages are significantly lower than the tolerance levels set by the United States Environmental Protection Agency for malt beverage starting ingredients. The use of the extraction/cleanup procedure and analysis by GC-MS(SIM) proved effective in screening malt beverages for a wide variety of pesticides.
开发了一种测定麦芽饮料中农药的方法,该方法采用聚合物柱进行固相萃取,并用硫酸镁覆盖的氨丙基柱进行样品净化,随后在选择离子监测模式下进行毛细管气相色谱-电子轰击质谱联用分析[GC-MS(SIM)]。分析和鉴定有机磷、有机卤化物和有机氮农药需要进行三次气相色谱进样。通过目标离子峰的保留时间和定性离子与目标离子的比率来鉴定农药。大多数农药的气相色谱检测限为5-10 ng/mL,线性范围为50至5000 ng/mL。对三种在酒精含量、固形物和外观等性质上存在差异的麦芽饮料进行了加标量为10 ng/mL的强化研究。在所研究的142种农药(包括异构体)中,有85种在这三种麦芽饮料中的回收率大于70%。数据表明,不同的麦芽饮料基质对回收率没有显著影响。然后将该方法应用于麦芽饮料中农药的筛查和分析,在实际样品中检测到了杀虫剂西维因和杀菌剂烯酰吗啉。该研究表明,麦芽饮料中的农药含量显著低于美国环境保护局为麦芽饮料起始原料设定的耐受水平。采用萃取/净化程序并通过GC-MS(SIM)进行分析,在筛查麦芽饮料中的多种农药方面证明是有效的。