Department of Chemistry, Lomonosov Moscow State University, Leninskie gory, 1/3, 119991 Moscow, Russia; Central Scientific Methodological Veterinary Laboratory, Orangereynaya st., 23, 111622 Moscow, Russia.
Department of Chemistry, Lomonosov Moscow State University, Leninskie gory, 1/3, 119991 Moscow, Russia.
Food Chem. 2022 Sep 1;387:132866. doi: 10.1016/j.foodchem.2022.132866. Epub 2022 Mar 31.
A quantitative multi-class multi-residue analytical method was developed for the determination of veterinary drugs in milk by high-performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS). A total of 132 veterinary drugs investigated belonged to almost 15 classes including sulfonamides, β-lactams, tetracyclines, quinolones, macrolides, nitrofurans, nitroimidazoles, phenicols, lincosamides, pleuromutilins, macrocyclic lactones, quinoxaline antibiotics, benzimidazoles, anthelmintics, coccidiostats and some others. A magnetic solid-phase extraction procedure was developed using magnetic hypercrosslinked polystyrene (HCP/FeO) for the sample preparation prior to HPLC-MS/MS without deproteinization step. The results indicated recoveries of 85-107% for 14 sulfonamides, 85-120% for 13 β-lactams, 89-115% for 4 tetracyclines, 82-119% for 14 quinolones, 82-115% for 8 macrolides, 97-109% for 4 nitrofurans, 84-115% for 10 nitroimidazoles, 89-114% for 3 phenicols, 86-111% for 3 lincosamides, 97-102% for 2 pleuromutilins, 72-88% for 4 macrocyclic lactones, 87-104% for 4 quinoxaline antibiotics, 76-119% for 21 benzimidazoles, 79-115% for 12 anthelmintics, 81-118% for 12 coccidiostats and 75-119 % for 5 unclassified drugs, with relative standard deviations (RSDs) of less than 20%, and the LOQs ranged from 0.05 to 1 μg kg. This methodology was then applied to field-collected real milk samples and trace levels of some veterinary drugs were detected.
建立了一种高效液相色谱-串联质谱法(HPLC-MS/MS)测定牛奶中 132 种兽药的多残留分析方法。所研究的兽药共 15 类,包括磺胺类、β-内酰胺类、四环素类、喹诺酮类、大环内酯类、硝基呋喃类、硝基咪唑类、酚类、林可酰胺类、截短侧耳素类、聚醚类、喹喔啉类抗生素、苯并咪唑类、驱虫药、抗球虫药等。采用磁性超交联聚苯乙烯(HCP/FeO)作为固相萃取材料,在不进行蛋白沉淀的情况下,建立了一种用于 HPLC-MS/MS 前处理的磁性固相萃取方法。结果表明,14 种磺胺类药物的回收率为 85%-107%,13 种β-内酰胺类药物的回收率为 85%-120%,4 种四环素类药物的回收率为 89%-115%,14 种喹诺酮类药物的回收率为 82%-119%,8 种大环内酯类药物的回收率为 82%-115%,4 种硝基呋喃类药物的回收率为 97%-109%,10 种硝基咪唑类药物的回收率为 84%-115%,3 种酚类药物的回收率为 89%-114%,3 种林可酰胺类药物的回收率为 86%-111%,2 种截短侧耳素类药物的回收率为 97%-102%,4 种聚醚类药物的回收率为 72%-88%,4 种喹喔啉类抗生素的回收率为 87%-104%,21 种苯并咪唑类药物的回收率为 76%-119%,12 种驱虫药的回收率为 79%-115%,12 种抗球虫药的回收率为 81%-118%,5 种未分类药物的回收率为 75%-119%,相对标准偏差(RSD)均小于 20%,检出限(LOQs)为 0.05-1μg/kg。该方法随后应用于采集的实际牛奶样品中,检测到一些兽药的痕量水平。