固相萃取-超快速液相色谱-串联质谱法同时测定化妆品中9种抗过敏药物残留  

Determination of Nine Anti-allergy Drugs Residue in Cosmetics by Solid Phase Extraction-Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王燕芹[1] 车文军[2] 王莉[2] 徐春祥[2] 卢剑[2] 

机构地区：[1]南京林业大学理学院,南京210037 [2]江苏省产品质量监督检验研究院,南京210007

出　　处：《分析化学》2013年第3期394-399,共6页Chinese Journal of Analytical Chemistry

基　　金：江苏省质监局科技计划基金(No.KJ103703)资助项目

摘　　要：建立了固相萃取-超快速液相色谱-串联质谱法(SPE-RRLC-MS/MS)同时测定化妆品中9种抗过敏药物残留(多西拉敏、美沙吡林、曲吡那敏、溴苯那敏、苯海拉明、赛克利嗪、二苯拉林、羟嗪和氯苯沙明)的方法。试样经三氯乙酸溶液超声提取、离心、Plexa PCX柱净化后,以甲醇-0.1%甲酸溶液(含5 mmol/L甲酸铵)为流动相,用RRLC进行分离。在电喷雾正离子模式下,以选择反应监测(SRM)方式采集数据进行定性与定量分析。9种药物在1.0～50.0!g/L范围内均呈良好的线性关系,相关系数均大于0.99;在2.0,5.0和20.0!g/kg3个浓度加标水平下的平均回收率为90.6%～103.5%;相对标准偏差(RSD,n=6)为2.5%～6.0%;检出限为0.3～0.6!g/kg,定量限为1.0～2.0!g/kg。A solid phase extraction coupled with rapid resolution liquid chromatography-tandem mass spectrometry （SPE-RRLC-MS/MS） method was developed for the determination of nine anti-allergy drugs, e.g. doxylamine, tripelennamine, brompheniramine, diphenhydramine, chlorphenoxamine, diphenylpyraline, methapyrilene, eyclizine, and hydroxyzine in cosmetics. The samples were extracted with trichloroaeetic acid solution under ultrasonication, centrifuged and cleaned up with Plexa PCX solid phase extraction. The separation of nine anti-allergy drugs was carried out on RRLC using methanol-phosphate buffer as mobile phase. Electrospray ionization mass spectrometry was operated in the positive mode using selective reaction monitoring（SRM） for the qualitative and quantitative analysis of nine anti-allergy drugs. For the nine drugs, the calibration curves were linear between 1.0 to 50.0 μg/L, and the correlation coefficient was more than 0.99. The mean recoveries at spiked levels of 2.0, 5.0, 20.0 μg/kg were in the range of 90.6% - 103.5%, the RSDs were 2.5%-6.0% （n=6）. The limits of detection and quantification were 0.3- 0. 6 μg/kg and 1.0-2.0 μg/kg, respectively.

关 键 词：超快速液相色谱-串联质谱 固相萃取 化妆品 抗过敏药物 

分 类 号：TQ658[化学工程—精细化工] O657.63[理学—分析化学]