高效液相色谱-质谱联用法检测猪肉中5种青霉素的残留量  

Determination of 5 penicillin residues in pork by HPLC/MS/MS(trap)

作　　者：范莹莹 其鲁[2] 杨树民 

机构地区：[1]中信国安盟固利电源技术有限公司,北京102200 [2]北京大学,北京100871 [3]国家体委兴奋剂检测中心,北京100029

出　　处：《分析试验室》2007年第12期76-79,共4页Chinese Journal of Analysis Laboratory

基　　金：国家科技部"奥运科技(2008)行动计划"(2002BA904B02)

摘　　要：建立了高效液相色谱与质谱联用法测定猪肉中5种青霉素类药物残留的方法。样品采用体积分数0.5%的乙酸提取,匀浆离心分离后通过XAD-2固相萃取柱净化,甲醇洗脱后,用质谱检测器检测。采用Agilent HC-C18色谱柱（250 mm×4.6 mmi.d.,5μm）,以体积分数0.1%NH3.H2O和乙腈为流动相进行梯度洗脱。在添加水平为0.1、0.2、0.5 mg/kg时,回收率在52%-82.8%之间,相对标准偏差在3.4%-9.2%之间,对于不同的药物,方法的检出限为0.001-0.005 mg/kg。该方法适合于猪肉组织中青霉素类药物残留量的检测。A method was developed for the determination of 5 penicillin residues in pork by high performance liquid chromatography tandem mass spectrometry （HPLC/MS）. The samples were extracted with 0.5 % acetic acid, followed by homogenizing and centrifuging precipitation, cleaned-up with XAD-2 solid-phase extraction column, eluted by methanol. The separation was performed on a Agilent HC-C18 （250 mm × 4.6 mm i.d., 5μm） column with a gradient system of 0.1% ammonia and acetonitrile as mobile phases. At spiked levels are 0.1, 0.2, 0.5 mg/kg, the limits of detection of the method are 1 - 5 ppb for the various antibiotics and recoveries of the spike experiment are from 52% to 82.8 %, precisions are between 3.4 % and 9.2 %. The method is suitable for the determination of residues of penicillins in pork.

关 键 词：高效液相色谱-质谱(HPLC/MS) 青霉素 猪肉 

分 类 号：O657.63[理学—分析化学]