高效液相色谱-串联质谱法测定动物肌肉组织.PDFVIP

248 2010, Vol. 31, No. 08 食品科学 ※分析检测 1 1 , 2 1 张凤清 ，王岩松 * ，范世华 ，周长民 (1.沈阳产品质量监督检验研究院，辽宁沈阳 110022 ；2.东北大学理学院，辽宁沈阳 110004) ：采用液相色谱- 串联质谱(LC-MS/MS)法测定动物肌肉组织中氯霉素，甲砜霉素和氟苯尼考三种药物的残 留量。添加氘代氯霉素(d5- 氯霉素) 作为内标，碱化乙酸乙酯提取，正己烷去除脂肪，省去固相萃取步骤直接上 机定量。选择电喷雾离子源(ESI) ，负离子扫描多反应监测(MRM)模式，并优化了质谱参数，使仪器的灵敏度达 到最高。氯霉素、甲砜霉素和氟苯尼考的检出限均达到0.01 μg/kg 。空白样品中添加氯霉素、甲砜霉素和氟苯尼 考水平为0.02～1 μg/kg 时，三种药品的线性相关系数均大于0.9990 。氯霉素平均回收率为92.8%～97.0% ，甲砜 霉素平均回收率为93.5%～96.6% ，氟苯尼考平均回收率为91.2%～95.9% 。 ：高效液相色谱- 串联质谱；动物肌肉；氯霉素；甲砜霉素；氟苯尼考 High Performance Liquid Chromatography-Tandem Mass Spectrometric Determination of Chloramphenicol, Thiamphenicol and Florfenicol Residues in Animal Muscles 1 1, 2 1 ZHANG Feng-qing ，WANG Yan-song *，FAN Shi-hua ，ZHOU Chang-min (1. Shenyang Supervision and Inspection Institute for Product Quality, Shenyang 110022, China ； 2. College of Sciences, Northeastern University, Shenyang 110004, China) Abstract ：A high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method was developed for the determination of chloramphenicol, thiamphenicol and florfenicol in animal muscles. Samples were spiked with deuterated chloramphenicol-d5 (d5-CAP) as internal standard and extracted with alkaline ethyl acetate. The resulting extract was then treated with n-hexane for the removal of lipids and injected directly into the HPLC-MS/MS system without the requirement of solid- phase extraction clean-up. The electrospray ionization (ESI) mass spectrometry was run in negative ion multiple reaction monitoring mode. Instrumental