Center for Food Safety and Applied Nutrition, Office of Regulatory Science, US Food and Drug Administration, HFS-706, 5100 Paint Branch Parkway, College Park, Maryland 20740-5350, USA.
J Agric Food Chem. 2010 May 26;58(10):5868-83. doi: 10.1021/jf903854n.
A multiresidue method for the analysis of pesticides in fresh produce has been developed using salt-out acetonitrile extraction, solid-phase dispersive cleanup with octadecyl-bonded silica (C(18)), and graphitized carbon black/primary-secondary amine (GCB/PSA) sorbents and toluene, followed by capillary gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS). Quantitation was determined from calibration curves using matrix-matched standards ranging from 3.3 to 6667 ng/mL with r(2) > 0.99, and geometric mean limits of quantitation were typically 8.4 and 3.4 microg/kg for GC-MS/SIM and GC-MS/MS, respectively. Identification was determined by using target and qualifier ions and qualifier-to-target ratios for GC-MS/SIM and two ion transitions for GC-MS/MS. Fortification studies (10, 25, 100, and 500 microg/kg) were performed on 167 organohalogen, organophosphorus, and pyrethroid pesticides in 10 different commodities (apple, broccoli, carrot, onion, orange, pea, peach, potato, spinach, and tomato). The mean percent recoveries were 90 +/- 14, 87 +/- 14, 89 +/- 14, and 92 +/- 14% for GC-MS/SIM and 95 +/- 22, 93 +/- 14, 93 +/- 13, and 97 +/- 13% for GC-MS/MS at 10, 25, 100, and 500 microg/kg, respectively. GC-MS/MS was shown to be more effective than GC-MS/SIM due to its specificity and sensitivity in detecting pesticides in fresh produce samples. The method, based on concepts from the multiresidue procedure used by the Canadian Food Inspection Agency and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe), was shown to be efficient in screening, identifying, and quantitating pesticides in fresh produce samples.
建立了一种多残留方法，用于分析新鲜农产品中的农药，该方法采用盐析乙腈提取、十八烷基键合硅胶（C(18)）、石墨化碳黑/初级-次级胺（GCB/PSA）固相分散净化和甲苯，然后采用气相色谱-质谱在选择离子监测模式（GC-MS/SIM）或串联质谱（GC-MS/MS）下进行分析。使用基质匹配标准，校准曲线的定量范围为 3.3 至 6667ng/mL，相关系数（r(2)）大于 0.99，GC-MS/SIM 和 GC-MS/MS 的几何平均定量限通常分别为 8.4 和 3.4μg/kg。GC-MS/SIM 通过使用目标和定性离子以及定性离子与目标离子的比值进行鉴定，GC-MS/MS 通过两个离子跃迁进行鉴定。在 10 种不同商品（苹果、西兰花、胡萝卜、洋葱、橙子、豌豆、桃子、土豆、菠菜和西红柿）中对 167 种有机卤代物、有机磷和拟除虫菊酯农药进行了 10、25、100 和 500μg/kg 的加标研究。GC-MS/SIM 的平均回收率分别为 90±14%、87±14%、89±14%和 92±14%，GC-MS/MS 的平均回收率分别为 95±22%、93±14%、93±13%和 97±13%。在 10、25、100 和 500μg/kg 时，GC-MS/MS 均优于 GC-MS/SIM，原因在于其在检测新鲜农产品样品中的农药时具有特异性和灵敏度。该方法基于加拿大食品检验局和 QuEChERS（快速、简单、廉价、有效、坚固、安全）多残留程序的概念，被证明在筛选、鉴定和定量新鲜农产品样品中的农药方面非常有效。
