Istituto Zooprofilattico Sperimentale della Puglia e della Basilicata , Via Manfredonia 20 , Foggia 71121 , Italy.
Key Laboratory of Natural Resources of the Changbai Mountain and Functional Molecules , Yanbian University , Park Road 977 - 133002 Yanji , China.
J Agric Food Chem. 2018 Oct 3;66(39):10267-10273. doi: 10.1021/acs.jafc.8b04851. Epub 2018 Sep 25.
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, with linear coefficients higher than 0.9992. Instrumental limits of detection were between 0.22 and 0.63 μg L, corresponding to 0.04 and 0.13 μg kg 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 and 0.07-0.23 μg kg, 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.
本文描述了一种用于通过气相色谱和电子俘获检测(GC-ECD)测定鸡蛋和肉类样品中六种拟除虫菊酯(苯醚菊酯、氯菊酯、氯氟氰菊酯、氯氰菊酯、溴氰菊酯、氰戊菊酯)的灵敏且重现性好的筛选分析方法。采用固相萃取快速净化方法,保证了溶剂消耗和时间的减少,并允许同时制备多个样品提取物。在最佳色谱条件下,提取-净化步骤总分析时间不到 60 分钟,即可实现高效分离。六种拟除虫菊酯的响应良好,在 50-500μg/L 范围内,线性系数均高于 0.9992。仪器检测限在 0.22-0.63μg/L 之间,对应于基质中的 0.04-0.13μg/kg。在加标样品中计算得到鸡卵和各种肉类样品中的检测限分别为 0.05-0.25μg/kg 和 0.07-0.23μg/kg。验证结果证实,拟议的 GC-ECD 方法可作为用于在官方检查分析中测定拟除虫菊酯的可靠筛选工具。该方法根据欧洲指令进行了广泛验证,在选择性、灵敏度、回收率、精密度和测量不确定度方面证明了其一致性。