超高效液相色谱-串联质谱法同时测定化妆品中的22种磺胺类药物

Simultaneous Determination of 22 Sulfonamides in Cosmetics by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

建立了同时测定化妆品中22种磺胺类药物（磺胺胍、磺胺、磺胺嘧啶、磺胺二甲异嘧啶、磺胺醋酰、磺胺噻唑、磺胺吡啶、磺胺甲基嘧啶、磺胺对甲氧嘧啶、磺胺二甲嗯唑、磺胺二甲嘧啶、磺胺甲噻二唑、磺胺甲氧哒嗪、琥珀酰磺胺噻唑、磺胺氯哒嗪、磺胺甲基异嗯唑、磺胺间甲氧嘧啶、磺胺邻二甲氧嘧啶、磺胺二甲异嗯唑、磺胺间二甲氧嘧啶、磺胺喹嗯啉、磺胺硝苯）的超高效液相色谱-串联质谱分析方法。膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品经超声提取后，以Waters ACQUITY UPLC BEH C18色谱柱（50mm×2.1mm，1.7μm）分离后进行UPLC／MS／MS多反应监测模式下的定性及定量分析。22种磺胺类药物的方法检出限为3．5～14.1μg／kg；在低、中、高的3个添加水平范围内的平均回收率为80．3％～103．6％；日内精密度均小于12％，日间精密度均小于15％。

A comprehensive analytical method based on ultra-performance liquid chromatography tandem mass spectrometry has been developed for the simultaneous determination of 22 sulfonamides （ sulfaguanidine, sulfanilamide, sulfadiazine, sulfisomidine, sulfaeetamide, sulfathiazole, sulfapyridine, sulfamerazine, sulfameter, sulfamoxole, sulfamethazine, sulfamethizole, sulfamethoxypyridazine, succinylsulfathiazole, sulfachloropyridazine, sulfamethoxazole, sulfamonomethoxine, sulfadoxine, sulfisoxazole, sulfadimethoxine, sulfaquinoxaline and sulfanitran）. Various cosmetic samples, including cream, lotion, powder, shampoo and lipstick, were extracted under ultrasonication. Qualitative and quantitative analysis was carried out for the analyte under the MRM mode after the chromatographic separation on Waters ACQUITY UPLC BEH C18 （50 mm×2.1mm, 1.7μm） column. The limits of detection for the 22 sulfonamides were 3.5 - 14.1μg/kg. The mean recoveries at the three spiked levels were 80.3% - 103.6% , with the intra-day precision less than 12% and the inter-day precision less than 15%.