在线固相萃取净化-液相色谱-串联质谱法测定猪肉中10种大环内酯类抗生素  

Liquid chromatography-tandem mass spectrometry method for determination of 10 macrolide antibiotics in pork samples using on-line solid phase extraction purification

作　　者：张晓光 刘东 刘红冉 李强 李立理 王丽霞 张岩 ZHANG Xiaoguang;LIU Dong;LIU Hongran;LI Qiang;LI Lili;WANG Lixia;ZHANG Yan(Hebei Food Inspection and Research Institute,Key Laboratory of Food Safety of Hebei Province,Shijiazhuang 050091,China;Shijiazhuang Food and Drug Inspection Institute,Shijiazhuang 050011,China)

机构地区：[1]河北省食品检验研究院河北省食品安全重点实验室,河北石家庄050091 [2]石家庄市食品药品检验所,河北石家庄050011

出　　处：《色谱》2017年第10期1055-1061,共7页Chinese Journal of Chromatography

基　　金：国家科技支撑计划项目(2015BAK36B03);河北省食品药品监督管理局科技项目(QN2015001;PT2014005)~~

摘　　要：建立了在线固相萃取净化-液相色谱-串联质谱检测猪肉中10种大环内酯类抗生素残留的方法。样品经过乙腈提取,提取液40℃旋蒸至干后,分析物用2 mL磷酸盐缓冲液溶解,溶解液经在线固相萃取柱(HLB柱)富集净化,甲醇洗脱,然后转移至XBridge BEH C18色谱柱上,以10 mmol/L乙酸铵水溶液和乙腈溶液为流动相进行分离,最后用串联四极杆质谱检测。结果表明,10种大环内酯类抗生素在0.1~200μg/L范围内呈现良好的线性关系,相关系数均大于0.990。方法的检出限范围为0.05~0.30μg/kg,定量限范围为0.10~1.00μg/kg;添加水平为0.10~10.0μg/kg时,方法回收率为69.6%~115.2%,相对标准偏差(RSD)<10%。该方法可以作为猪肉中大环内酯类抗生素的检测方法。A high performance liquid chromatography-tandem mass spectrom etry(HPLC-MS/MS)method based on-line solid phase extraction(SPE)purification was established to determine10macrolide antibiotics in pork samples.The samples were extracted with acetonitrile,and the extracts were dried with rotary evaporator at40℃,then the analytes were dissolved with2m Lphosphate buffer.The solutions were purified and concentrated by on-line SPE with HLB cartridges.The analytes were eluted with methanol,and then transferred to XBridge BEH C18column,separated with the mobile phases of10mmol/Lammonium acetate aqueous solution and acetonitrile.Finally,the target analytes were detected by tandem mass spectrometry.The results showed that good linearity was obtained in the range of0.1-200ug/L for the10macrolide antibiotics with correlation coefficients better than0.990.The lim its of detection were in range of0.05-0.30ug/kg and the lim its of quantitation were in range of0.10-1.00ug/kg.The recoveries of the method were in range of69.6%-115.2%at the spiked levels of0.10-10.0ug/kg fo rall analytes,with the relative standard deviations less than10%.The developed method can be used for the determ ination of the10macrolide antibiotics in pork samples.

关 键 词：在线固相萃取 液相色谱-串联质谱法 大环内酯类抗生素 猪肉 

分 类 号：O658[理学—分析化学]