Optimization and Validation of a Multiresidue Pesticide Method in Rice and Wheat Flour by Modified QuEChERS and GC-MS/MS
Optimization and Validation of a Multiresidue Pesticide Method in Rice and Wheat Flour by Modified QuEChERS and GC-MS/MS
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DOI：
10.1007/s12161-015-0214-7
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发表时间：
2016-02-01
影响因子：
2.9
通讯作者：
Garrido-Frenich, Antonia
中科院分区：
文献类型：
--
作者：
Grande-Martinez, Angel;Javier Arrebola-Liebanas, Francisco;Garrido-Frenich, Antonia
采用快速、简便、廉价、有效、坚固和安全（QuEChERS）的方法，使用乙酸乙酯代替乙腈，已被提议用于提取大米和小麦粉中的约100种农药。这种灵敏可靠的方法是基于使用气相色谱-串联质谱法（GC-MS/MS）。根据欧盟SANCO/12571/2013指南和ISO 17025：2005对该方法进行了验证。提取需要预先加水、样品的乙酸乙酯提取和最终净化步骤。大多数化合物的校准曲线在0.003 - 0.150 mg kg（-1）范围内呈线性。超过80%的农药的定量限设定为0.0036 mg kg（-1）。在0.004和0.040 mg kg（-1）下计算回收率，结果始终在70- 116%范围内，精密度值为千分之一货币符号20%。在上述两个浓度下估计扩展不确定度，始终为千分之一货币符号50%。通过对真实的样品的分析，对该方法的适用性进行了评价，没有检测到高于定量限的农药，尽管在其中一些样品中检测到了少量的农药（甲基嘧啶磷、戊唑醇、毒死蜱和甲基毒死蜱）。
An adaptation of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, using ethyl acetate instead of acetonitrile, has been proposed to extract around 100 pesticides in rice and wheat flour. This sensitive and reliable method is based on the use of gas chromatography-tandem mass spectrometry (GC-MS/MS). The method has been validated according to the European Union SANCO/12571/2013 guidelines and ISO 17025:2005. The extraction required a prior water addition, an ethyl acetate extraction of the sample, and a final cleanup step. Calibration curves were linear from 0.003 to 0.150 mg kg(-1) for most compounds. The limit of quantification was set at 0.0036 mg kg(-1) for more than 80 % of the pesticides. Recoveries were calculated at 0.004 and 0.040 mg kg(-1), resulting always in the range 70-116 %, and with precision values a parts per thousand currency sign20 %. The expanded uncertainty was estimated at the two abovementioned concentrations, being always a parts per thousand currency sign50 %. The method applicability has been evaluated by the analysis of real samples, and no pesticides were detected above the limit of quantification, although some minor amounts of pesticides were detected (pirimiphos methyl, tebuconazole, chlorpyrifos, and chlorpyrifos methyl) in some of them.