超高效液相色谱-串联质谱法同时测定化妆品中的3种磺脲类物质  

Simultaneous Determination of 3 Sulfonylureas in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：周莉莉[1] 王艳丽[1] 杨颖[1] 薛霞[1] 杨昊[1] 刘桂亮[1] 郑红[1] 张艳侠[1] 卢兰香[1] 

机构地区：[1]山东省产品质量监督检验研究院国家加工食品质量监督检验中心(山东),山东济南250103

出　　处：《分析测试学报》2013年第9期1086-1090,共5页Journal of Instrumental Analysis

基　　金：国家标准委员会计划项目(20101090-T-607);国家质检总局科技计划项目(2009QK246)

摘　　要：建立了同时测定化妆品中3种磺脲类物质（氨磺丁脲、氯磺丙脲及甲苯磺丁脲）的超高效液相色谱-电喷雾串联质谱（UPLC-MS/MS）分析方法。霜剂、水剂、膏剂等不同类型的化妆品样品通过酸化甲醇提取，提取液经离心过滤后用水稀释，超高效液相色谱分离，串联质谱检测，外标法定量，5 min内即可完成3种化合物的分离分析。3种磺脲类化合物在0.001-0.1 mg/L范围内呈良好线性，其相关系数均大于0.999，定量下限均为0.08 mg/kg。在低、中、高3个加标水平下的平均回收率为80.9%-117.0%，相对标准偏差为3.6%-9.7%。A comprehensive ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS）method was developed for the determination of 3 sulfonylureas（carbutamide,chlorpropamide and tolbutamide）in cosmetics.Various cosmetic samples,including cream,aqua and ointment,were extracted with acidified methanol and then diluted with water.The extract was separated with reversed-phase UPLC using a binary eluent under isocratic conditions,and determined by MS/MS under the negative electrospray ionization mode with multiple reaction monitoring.The result indicated that a good separation of three compounds was obtained in 5 min.The calibration curves for 3 sulfonylureas were linear in the range of 0.001-0.1 mg/L with correlation coefficients more than 0.999.The limits of quantitation（LOQs）for 3 sulfonylureas were all 0.08 mg/kg.The mean recoveries at three spiked levels ranged from 80.9% to 117.0% with relative standard deviations（n=6） of 3.6%-97%.Under the optimal conditions,The method has good simplicity,sensitivity and stability,and is suitable for the rapid determination of 3 sulfonylureas in cosmetics.

关 键 词：超高效液相色谱-串联质谱法 化妆品 氨磺丁脲 氯磺丙脲 甲苯磺丁脲 

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