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Sensitive Screening Method for Determination of Pyrethroids in Chicken Eggs and Various Meat Samples by Gas Chromatography and Electron Capture Detection
Journal of Agricultural and Food Chemistry ( IF 5.7 ) Pub Date : 2018-09-12 00:00:00 , DOI: 10.1021/acs.jafc.8b04851 Valeria Nardelli 1 , Francesco Casamassima 1 , Giuseppe Gesualdo 1 , Donghao Li 2 , Wadir M. V. Marchesiello 3 , Donatella Nardiello 3 , Maurizio Quinto 2, 3
Journal of Agricultural and Food Chemistry ( IF 5.7 ) Pub Date : 2018-09-12 00:00:00 , DOI: 10.1021/acs.jafc.8b04851 Valeria Nardelli 1 , Francesco Casamassima 1 , Giuseppe Gesualdo 1 , Donghao Li 2 , Wadir M. V. Marchesiello 3 , Donatella Nardiello 3 , Maurizio Quinto 2, 3
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A sensitive and reproducible screening analytical method is described for the determination of six pyrethroids (phenothrin, permethrin, cyfluthrin, cypermethrin, deltamethrin, fenvalerate) in egg and meat samples by gas chromatography and electron capture detection (GC-ECD). A fast cleanup procedure, based on solid-phase extraction has been used, ensuring reduced solvent consumption and time and allowing the simultaneous preparation of multiple sample extracts. Under the optimal chromatographic conditions, an efficient separation was obtained with a total analysis time of less than 60 min, including the extraction-purification steps. Good responses for the six pyrethroids were obtained in a range of 50–500 μg L–1, with linear coefficients higher than 0.9992. Instrumental limits of detection were between 0.22 and 0.63 μg L–1, corresponding to 0.04 and 0.13 μg kg–1 in the matrix. Detection limits in chicken eggs and various meat samples, calculated on spiked samples, were in the range 0.05–0.25 μg kg–1 and 0.07–0.23 μg kg–1, respectively. The validation results confirmed that the proposed GC-ECD method can be used as a reliable screening tool for the determination of pyrethroids in official check analyses. The method was extensively validated following the European directives, demonstrating its conformity in terms of selectivity, sensitivity, recovery, precision, and measurement uncertainty.
中文翻译：
气相色谱和电子捕获检测灵敏筛选方法测定鸡蛋和各种肉类样品中的拟除虫菊酯
描述了一种灵敏且可重复的筛选分析方法，用于通过气相色谱和电子捕获检测（GC-ECD）测定鸡蛋和肉类样品中的六种拟除虫菊酯（苯乙菊酯，苄氯菊酯，氟氟氰菊酯，氯氰菊酯，溴氰菊酯，氰戊菊酯）。已使用基于固相萃取的快速净化程序，以确保减少溶剂消耗和时间，并允许同时制备多种样品萃取物。在最佳色谱条件下，包括萃取-纯化步骤在内，总分析时间少于60分钟，可实现有效分离。在50–500μgL –1范围内获得了对六个拟除虫菊酯的良好响应，其线性系数高于0.9992。仪器的检测限在0.22至0.63μgL –1之间，对应于基质中的0.04至0.13μgkg –1。以加标样品计算的鸡蛋和各种肉类样品中的检出限分别在0.05–0.25μgkg –1和0.07–0.23μgkg –1之间。验证结果证实，建议的GC-ECD方法可作为官方检查分析中测定拟除虫菊酯的可靠筛选工具。该方法已按照欧洲指令进行了广泛验证，证明了其在选择性，灵敏度，回收率，精密度和测量不确定度方面的一致性。
更新日期：2018-09-12
中文翻译：
气相色谱和电子捕获检测灵敏筛选方法测定鸡蛋和各种肉类样品中的拟除虫菊酯
描述了一种灵敏且可重复的筛选分析方法，用于通过气相色谱和电子捕获检测（GC-ECD）测定鸡蛋和肉类样品中的六种拟除虫菊酯（苯乙菊酯，苄氯菊酯，氟氟氰菊酯，氯氰菊酯，溴氰菊酯，氰戊菊酯）。已使用基于固相萃取的快速净化程序，以确保减少溶剂消耗和时间，并允许同时制备多种样品萃取物。在最佳色谱条件下，包括萃取-纯化步骤在内，总分析时间少于60分钟，可实现有效分离。在50–500μgL –1范围内获得了对六个拟除虫菊酯的良好响应，其线性系数高于0.9992。仪器的检测限在0.22至0.63μgL –1之间，对应于基质中的0.04至0.13μgkg –1。以加标样品计算的鸡蛋和各种肉类样品中的检出限分别在0.05–0.25μgkg –1和0.07–0.23μgkg –1之间。验证结果证实，建议的GC-ECD方法可作为官方检查分析中测定拟除虫菊酯的可靠筛选工具。该方法已按照欧洲指令进行了广泛验证，证明了其在选择性，灵敏度，回收率，精密度和测量不确定度方面的一致性。
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