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鸡肉和鸡蛋中农药、多环芳烃和多氯联苯的多残留分析:GC-MS/MS 法的开发与验证。

Multiresidue analysis of pesticides, polyaromatic hydrocarbons and polychlorinated biphenyls in poultry meat and chicken eggs by GC-MS/MS: method development and validation.

机构信息

National Reference Laboratory, ICAR-National Research Centre for Grapes, Pune, India.

National Reference Laboratory, ICAR-Central Institute of Fisheries Technology, Kochi, Kerala, India.

出版信息

J Environ Sci Health B. 2022;57(4):263-283. doi: 10.1080/03601234.2022.2047390. Epub 2022 Apr 22.

DOI:10.1080/03601234.2022.2047390
PMID:35452352
Abstract

The study uses gas chromatography with tandem mass spectrometry (GC-MS/MS) to develop a reliable analytical approach for detecting multiclass pesticides, polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) in poultry meat and chicken eggs. The meat (2 g) and egg (4 g) samples were extracted with acidified acetonitrile (10 mL) as part of the optimized sample preparation technique. The cleanup consisted of freezing an aliquot of the extract (5 mL) at -20 °C, followed by dispersive solid phase extraction using 50 mg PSA + 100 mg C+150 mg MgSO. The matrix co-extractives were effectively removed and the method performance met the European Commission's analytical quality control criteria (SANTE/12682/2019). The method was validated at two spiking levels (10 and 20 ng/g of 225 pesticides, 9 PAHs and 8 PCBs), and good recoveries (70-120%) and precision-RSDs (≤20%) were achieved for 90% of the targeted pesticide residues. For 80% of the compounds, the LOQs were ≤10 ng/g. The results of the intra-laboratory (involving six analysts) and inter-laboratory validation studies (involving eight ISO 17025 accredited laboratories) established satisfactory ruggedness and reproducibility. It created potential applications in commercial residue testing laboratories for regulatory compliance check purposes.

摘要

本研究采用气相色谱-串联质谱法(GC-MS/MS)开发了一种可靠的分析方法,用于检测禽肉和禽蛋中的多类农药、多环芳烃(PAHs)和多氯联苯(PCBs)。作为优化的样品制备技术的一部分,将 2 g 肉和 4 g 蛋样品用酸化乙腈(10 mL)提取。净化包括将提取物(5 mL)的等分试样在-20°C 下冷冻,然后用 50 mg PSA+100 mg C+150 mg MgSO 进行分散固相萃取。有效地去除了基质共提取物,该方法的性能符合欧盟委员会的分析质量控制标准(SANTE/12682/2019)。该方法在两个加标水平(225 种农药、9 种 PAHs 和 8 种 PCBs 的 10 和 20 ng/g)进行了验证,90%的目标农药残留的回收率(70-120%)和精密度-RSD(≤20%)良好。对于 80%的化合物,LOQs ≤10 ng/g。实验室内部(涉及六名分析师)和实验室间验证研究(涉及八个经过 ISO 17025 认证的实验室)的结果表明,该方法具有令人满意的稳健性和重现性。它为商业残留检测实验室的法规遵从性检查目的创造了潜在的应用。

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