高效液相色谱-串联质谱法测定蜂蜜中的红霉素及其代谢物  

Determination of Erythromycin A and Its Metabolites in Honey by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张晓燕[1] 郑定钊 袁芳[1] 刘艳[1] 黄娟[1] 许蔚[1] 杨雯筌[1] 丁涛[1] 陈磊[1] 吴斌[1] 

机构地区：[1]江苏出入境检验检疫局动植物与食品检测中心国家蜂产品基准实验室,江苏南京210001 [2]福建工贸学校,福建福州350002

出　　处：《分析测试学报》2013年第9期1131-1134,共4页Journal of Instrumental Analysis

基　　金：国家质检总局科技资助项目(2011IK209)

摘　　要：建立了高效液相色谱-串联质谱法检测蜂蜜中红霉素及其代谢物红霉素A烯醇醚和脱水红霉素A的测定方法。以pH 7.0的磷酸盐缓冲液为提取剂，经HLB小柱净化富集后，采用高效液相色谱串联质谱法测定蜂蜜中红霉素及其代谢物的含量。该方法前处理简单，采用内标法定量，方法的线性范围为2.0～100.0 μg/L，相关系数大于0.996，红霉素及其两种主要代谢物的检出限和定量下限分别为0.5 μg/kg和2.0 μg/kg，回收率范围为70.5%-109.2%，RSD小于10%。方法的回收率稳定且重现性较好，可用于蜂蜜中红霉素及其代谢物的检测。A high performance liquid chromatography-tandem mass spectrometric method for the determination of erythromycin A and its metabolites including erythromycin A enolether and anhydroerythromycin A was developed.The sample was extracted with pH 7.0 phosphate buffer and cleaned-up with HLB column.The detection of target compounds was performed by LC-MS with electrospray positive ionization under the multiple reaction monitoring（MRM） mode.The internal standard method was used for quantitative analysis.Under the optimal conditions,the calibration curves were linear in the range of 2.0-100.0 μg/L with correlation coefficients more than 0.996.The limits of detection and the limits of quantitation were 0.5 μg/kg and 2.0 μg/kg,respectively.The recoveries of three compounds at fortified levels of 2.0,5.0 and 10.0 μg/kg ranged from 70.5% to 109.2% with RSDs less than 10%.The method,with higher recoveries and good precision,was suitable for the determination of erythromycin A and its metabolites in honey.

关 键 词：蜂蜜 红霉素 代谢物 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]