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

R. Patil, N. Chatterjee, Narayan Kamble, Apurva Nerpagar, Nagnath Langade, Chandrasekar Kandaswamy, S. Presley, K. Banerjee
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引用次数: 2

Abstract

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 C18+150 mg MgSO4. 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.
GC-MS/MS分析禽肉和鸡蛋中农药、多芳烃和多氯联苯的多残留:方法的建立和验证
摘要本研究采用气相色谱-串联质谱(GC-MS/MS)技术,建立了一种检测禽肉和鸡蛋中多类农药、多环芳烃(PAHs)和多氯联苯(PCBs)的可靠分析方法。采用酸化乙腈(10 mL)提取肉(2 g)和蛋(4 g)样品,作为优化样品制备工艺的一部分。清洗包括:在- 20°C冷冻提取物的等分液(5ml),然后用50mg PSA + 100mg C18+ 150mg MgSO4进行分散固相萃取。基质共萃取物被有效去除,方法性能符合欧盟委员会的分析质量控制标准(SANTE/12682/2019)。在225种农药、9种多环芳烃和8种多氯联苯的10和20 ng/g加峰水平下对该方法进行了验证,回收率为70 ~ 120%,精密度rsd≤20%。80%的化合物loq≤10 ng/g。实验室内(涉及6名分析人员)和实验室间验证研究(涉及8个ISO 17025认可实验室)的结果建立了令人满意的坚固性和可重复性。它创造了潜在的应用在商业残留测试实验室的法规遵从性检查的目的。
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