Optimization of the QuEChERS Method for Determination of Pesticide Residues in Chicken Liver Samples by Gas Chromatography-Mass Spectrometry
Optimization of the QuEChERS Method for Determination of Pesticide Residues in Chicken Liver Samples by Gas Chromatography-Mass Spectrometry
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DOI：
10.1007/s12161-014-9966-8
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发表时间：
2015-04
影响因子：
2.9
通讯作者：
J. M. Molina-Ruiz;E. Cieślik;Izabela Wałkowska
中科院分区：
文献类型：
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作者：
J. M. Molina-Ruiz;E. Cieślik;Izabela Wałkowska
本研究的目的是评价快速、简单、廉价、有效、可靠和安全（QuEChERS）方法在脂肪动物基质（如来自波兰Balice国家动物生产研究所的鸡肝脏）中有机氯、有机磷和氨基甲酸酯类农药的测定中的应用。研究了在0.010和0.020 mg kg−1浓度下的农药提取效果，并通过添加不同的d-SPE吸附剂组合（PSA + GCB、PSA + C18、PSA + SAX和PSA + NH2）对分散固相萃取（d-SPE）净化步骤的效率进行了比较。采用气相色谱-离子阱质谱（GC/IT-MS）分析农药残留。所有目标分析物在0 ~ 400 ng mL−1范围内呈线性关系，测定系数为entr2 > 0.997。在0.020 mg kg - 1加峰水平下，样品的回收率较高。加样回收率在70 ~ 120%之间，在0.020 mg kg−1加样水平下，相对标准偏差（RSD）小于15%。在清理步骤中测试的四种不同的吸附剂组合获得了相似的回收率，当（PSA + SAX）组合测试时，回收率更高。检出限（lod）为0.001 ~ 0.005 mg kg - 1，定量限（loq）为0.003 ~ 0.015 mg kg - 1。该方法成功地应用于实际鸡肝样品的农药残留分析；在所有情况下，污染水平均低于欧盟（EU）法规（EC） N 396/2005规定的默认最大残留水平（MRLs）。
The goal of this research was to evaluate the application ofQuick,Easy,Cheap,Effective,Rugged,and Safe(QuEChERS) method for the determination of organochlorine, organophosphate, and carbamate pesticides in fatty animal matrices such as liver of chicken obtained from National Research Institute of Animal Production in Balice (Poland). Pesticides extraction effectiveness was evaluated at two different spiking levels (0.010 and 0.020 mg kg−1) and efficiency of the dispersive solid-phase extraction (d-SPE) clean-up step was evaluated by comparison adding different d-SPE sorbent combinations (PSA + GCB, PSA + C18, PSA + SAX, and PSA + NH2). The analysis of pesticide residues was performed by gas chromatography ion trap mass spectrometry (GC/IT-MS). The linear relation was observed from 0 to 400 ng mL−1and the determination coefficientR2> 0.997 in all instances for all target analytes. Better recoveries were obtained in samples at 0.020 mg kg−1spiking level. The recoveries were in the range 70–120 %, with relative standard deviation (RSD) values lower than 15 % at 0.020 mg kg−1spiking level for most pesticides. Similar recovery ratios were obtained with the four different combinations of sorbents tested in the clean-up step, with better precision when the (PSA + SAX) combination was tested. Limits of detection (LODs) ranged from 0.001 to 0.005 mg kg−1and limits of quantification (LOQs) ranged from 0.003 to 0.015 mg kg−1. The proposed method was successfully applied analyzing pesticide residues in real chicken liver samples; detectable pesticide residues were observed, but in all of the cases, the contamination level was lower than the default maximum residue levels (MRLs) set by European Union (EU), Regulation (EC) N 396/2005.