Han R W, Zheng N, Yu Z N, Wang J, Xu X M, Qu X Y, Li S L, Zhang Y D, Wang J Q
College of Food Science and Engineering, Qingdao Agricultural University, Qingdao, Shandong, China.
Ministry of Agriculture - Laboratory of Quality & Safety Risk Assessment for Dairy Products (Beijing), Beijing, China; Ministry of Agriculture - Milk and Dairy Product Inspection Center (Beijing), Beijing, China; State Key Laboratory of Animal Nutrition, Institute of Animal Science, Chinese Academy of Agricultural Sciences, Beijing, China.
Food Chem. 2015 Aug 15;181:119-26. doi: 10.1016/j.foodchem.2015.02.041. Epub 2015 Feb 14.
A selective and rapid method has been developed to determine, simultaneously, 38 veterinary antibiotic residues in raw milk by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). One milliliter of raw milk was diluted with 0.5 mL water and 3 mL acetonitrile, then purified using an Oasis HLB cartridge. The eluates were evaporated by nitrogen drying and then reconstituted to 4 mL with water/acetonitrile (8:1) before being injected into the UPLC-MS/MS system. The results indicated recoveries of 68-118% for 14 β-lactams, 79-118% for eight quinolones, 71-106% for eight sulfonamides, 76-116% for four tetracyclines, 78-106% for three macrolides, and 88-103% for one lincosamides, with coefficients of variation less than 15% for intraday and interday precisions. The limit of quantification for all antibiotics was 0.03-10 μg kg(-1). This methodology was then applied to field-collected real raw milk samples and trace levels of four antibiotics were detected.
已开发出一种选择性快速方法，通过超高效液相色谱 - 串联质谱法（UPLC-MS/MS）同时测定生乳中的38种兽用抗生素残留。取1毫升生乳，用0.5毫升水和3毫升乙腈稀释，然后使用Oasis HLB柱进行净化。洗脱液经氮气吹干后，用水/乙腈（8:1）复溶至4毫升，再注入UPLC-MS/MS系统。结果表明，14种β-内酰胺类抗生素的回收率为68 - 118%，8种喹诺酮类抗生素的回收率为79 - 118%，8种磺胺类抗生素的回收率为71 - 106%，4种四环素类抗生素的回收率为76 - 116%，3种大环内酯类抗生素的回收率为78 - 106%，1种林可酰胺类抗生素的回收率为88 - 103%，日内和日间精密度的变异系数均小于15%。所有抗生素的定量限为0.03 - 10 μg kg⁻¹。该方法随后应用于现场采集的实际生乳样品，检测到了痕量水平的4种抗生素。
