微波辅助萃取-液相色谱-串联质谱法检测猪肉中四种氟喹诺酮类药物残留  

Determination of four fluoroquinolones residues in pork by LC-MS/MS using microwave-assisted extraction

作　　者：倪永付[1] 朱莉萍[1] 王勇[1] 闫秋成 

机构地区：[1]济宁出入境检验检疫局,山东济宁272000

出　　处：《肉类工业》2012年第9期42-44,共3页Meat Industry

摘　　要：建立了微波辅助萃取-液相色谱-串联质谱法检测猪肉中氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星四种氟喹诺酮类药物残留的方法。样品经微波辅助萃取,正己烷脱脂,无水硫酸钠除水,浓缩提取物至干,用1.0mL0.1%甲酸溶液溶解后上机检测。采用Hypersil GOLD-1.9μm,50 mm×2.1 mm(i.d)色谱柱分离,在多反应监测模式下检测,外标法定量。结果表明:四种氟喹诺酮类药物在浓度10～200μg/L范围内线性关系良好,相关系数r=0.9956～0.9991,定量限为10μg/kg。在不同添加水平下,其平均回收率为88%～101%,变异系数为1.4%～4.1%。Microwave - assisted extraction combined with LC - MS/MS method was established to determine the Ofloxacin, Norfloxacin, Ciprofloxac, Enrofloxaein residues in pork. The sample was extracted by microwave extraction equipment, defatted by n - Hexane, dehydrated by anhydrous sodium sulfate, and dried up. After being dissolved in 1.0mL 0.1% formic acid solution, the sample was performed on Hypersil GOLD - 1.91xm, 50 mm× 2.1 mm （ i. d） column. The analysis was carried out in the multi - reaction monitoring mode and external standard method was used for quantification. The calibration curve of the four fluoroquinolones presented a good linear relation with the peak area in the range of 10 to 200μg/L with the correlation coefficient r =0.9956 -0. 9991, and quantitative limit of this method was 10μg/kg. Under different addition level, the average recoveries were 88% -101% and the variability coefficient were 1.4% -4.1%.

关 键 词：微波辅助萃取 液相色谱-串联质谱 猪肉 氟喹诺酮类 残留 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]