液相色谱-串联质谱法测定蜂蜜中9种青霉素  

Determination of 9 penicillins in honey by high-performance liquid chromatography-tandem mass spectrometry

作　　者：李学民[1] 母健[1] 王蕾[1] 曹彦忠[1] 张进杰[1] 

机构地区：[1]秦皇岛出入境检验检疫局,河北秦皇岛066004

出　　处：《河北大学学报（自然科学版）》2012年第5期492-498,共7页Journal of Hebei University(Natural Science Edition)

基　　金：国家标准研制资助项目(20040032-T-442)

摘　　要：建立了用液相色谱-串联质谱(LC-MS-MS)测定蜂蜜中9种青霉素残留量的分析方法.3g蜂蜜样品用25mL pH=8.5的0.15mol/L磷酸二氢钠缓冲溶液溶解,用Oasis HLB固相萃取柱净化,目标物用乙腈-水(体积比1∶1)洗脱,定容收集液至3mL.采用电喷雾电离,正离子扫描,多反应监测(MRM)模式检测.0.5,1.0,2.0,5.0μg/kg 4个添加水平的回收率为76.9%～104.3%;相对标准偏差为3.29%～9.12%;方法定量限是:青霉素G、乙氧萘青霉素为0.5μg/kg,氧哌嗪青霉素、青霉素V、苯唑青霉素为1.0μg/kg,羟氨苄青霉素、氨苄青霉素、邻氯青霉素、双氯青霉素为2.0μg/kg.A method was described for the determination of 9 penicillins in honey by LC-MS-MS.3.0 g honey samples were dissolved in 25 mL sodium dihydrogen phosphate buffer solution（pH=8.5）,and then cleaned up with Oasis HLB SPE cartridge.The target compounds were eluted with acetonitrile-water（1∶1）,and the elution was determined to a volume of 3 mL.MS detection was performed in the positive ion mode using multiple reaction monitoring（MRM）.Limit of quantification（LOQ） for the method of 9 penicillins was between 0.5-2.0 μg/kg.Average recoveries at four fortification levels（0.5,1.0,2.0,5.0 μg/kg） in honey were 76.9%-104.3%,relative standard deviation were 3.29%-9.12%.

关 键 词：液相色谱-串联质谱 蜂蜜 9种青霉素 

分 类 号：O177.91[理学—数学]