National Referral Laboratory, ICAR-National Research Centre for Grapes, Pune 412307, India; Department of Environmental Science, Shivaji University, Kolhapur, India.
National Referral Laboratory, ICAR-National Research Centre for Grapes, Pune 412307, India.
Food Chem. 2019 Jan 30;272:292-305. doi: 10.1016/j.foodchem.2018.08.033. Epub 2018 Aug 9.
This paper reports a unified sample preparation approach for high-throughput multi-residue analysis of veterinary drugs and pesticides in a single sub-sample of bovine milk. The sample (5 g) was deproteinized with acetonitrile before an aliquot (I) was withdrawn, and the remainder was phase-separated using MgSO and NaCl. The acetonitrile layer (II) was recovered and the extracts combined, cleaned, and solvent-exchanged before the concentrations of veterinary drugs and pesticides were measured by ultra-fast liquid chromatography tandem mass spectrometry (UFLC-MS/MS). As a unique approach, extract II was analyzed simultaneously using gas chromatography tandem mass spectrometry (GC-MS/MS). Method performance for 78 drugs and 238 pesticides complied with CD 2002/657/EC and SANTE/11813/2017 guidelines, respectively, with significant savings in time and cost. Thus, it would be ideal for regulatory analysis of analytes ranging from non-polar organochlorine pesticides to polar drugs, including penicillins, quinolones, and tetracyclines.
本文报道了一种高通量多残留分析牛奶奶样中兽药和农药的统一前处理方法。取 5g 牛奶样品，用乙腈沉淀蛋白，取上清液（I），剩余部分用硫酸镁和氯化钠进行液液萃取。回收乙腈层（II），合并提取液，经净化、溶剂交换后，采用超快速液相色谱串联质谱（UFLC-MS/MS）测定兽药和农药的浓度。作为一种独特的方法，同时使用气相色谱串联质谱（GC-MS/MS）分析提取液 II。78 种兽药和 238 种农药的方法性能分别符合指令 2002/657/EC 和 SANTE/11813/2017 的要求，在时间和成本上有显著节省。因此，该方法非常适合从非极性有机氯农药到极性药物（包括青霉素类、喹诺酮类和四环素类）等分析物的监管分析。
