PRiME HLB-UPLC-MS/MS法测定祛痘类化妆品中9种磺胺类药物

PRiME HLB-UPLC-MS/MS Method for Rapid Determination of 9 Sulfonamides in Anti-acne Cosmetics

本文建立了基于超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)测定祛痘类化妆品中违法添加9种磺胺类药物的分析方法。样品经饱和氯化钠溶液分散破乳,以乙腈为提取溶剂,PRi ME HLB滤过式进行净化,采用MRM采集模式进行定性和定量检测,外标法定量。结果显示:9种磺胺类药物在各自线性范围呈良好的线性关系,相关系数(R^(2))均大于0.9959,检出限为0.0171~1.222μg/kg,定量限为0.0543~4.400μg/kg,3个添加水平的回收率为62.4%~89.4%,相对标准偏差为2.3%~9.4%。该分析方法前处理简单、重现性好、灵敏度高,适用于祛痘类化妆品中违法添加9种磺胺类药物的快速筛查。

An analysis method was established for rapid screening of 9 kinds of sulfonamides mixed illegally in antiacne cosmetics by ultra-high performance hydrophilic interaction liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)in this paper.The sample was dispersed and emulsified by saturated sodium chloride and extracted by acetonitrile,then purified by PRi ME HLB,a method of direct filtration.After that,qualitative detection and quantitative detection of the sample were carried out through MRM acquisition mode,and external standard method was used for quantitative detection.The result displayed that the analytes showed good linearities at their respective linear ranges,with their correlation coefficients(R^(2))no less than 0.9959,and the detection limit and quantitation limit of 0.0171~1.222μg/kg and 0.0543~4.400μg/kg,respectively.At the same time,the spiked recoveries for analytes at three spiked levels were 62.4%~89.4%,and the relative standard deviations were 2.3%~9.4%.This analysis method is suitable for the rapid determination of 9 kinds of sulfonamides in anti-acne cosmetics due to simple pretreatment,good reproducibility and high sensitivity.