超高效液相色谱-串联质谱法测定化妆品中13种禁用原料  

Determination of 13 Prohibited Ingredients in Cosmetics by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：毛林芳 MAO Linfang(Fujian Institute for Food and Drug Quality Inspection,Fuzhou 350001,China)

机构地区：[1]福建省食品药品质量检验研究院,福建福州350001

出　　处：《分析测试技术与仪器》2025年第1期55-62,共8页Analysis and Testing Technology and Instruments

摘　　要：采用超高效液相色谱–串联质谱法(UPLC-MS/MS)同时测定化妆品中新康唑等13种禁用原料.样品经过饱和氯化钠溶液分散,乙腈超声提取,上清液用水定容.以0.1%甲酸水–乙腈作为流动相梯度洗脱,采用Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm)色谱柱分离,使用正、负离子扫描,在多反应监测(MRM)模式下进行检测,基质标准曲线外标法定量.结果显示,在水基、乳液和膏霜这3类基质中13种禁用原料线性关系良好,相关系数(r)均大于0.995,检出限为0.2~2μg/kg,定量限为0.6~6μg/kg.3个加标浓度下的回收率为77.50%~120.00%,相对标准偏差为1.3%~7.3%.方法具有前处理简便、灵敏度高、准确可靠等优点,可作为化妆品中13种禁用原料的检测方法.An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous determination of 13 prohibited ingredients(such as econazole)in cosmetics.The samples were dispersed with saturated sodium chloride solution,extracted with acetonitrile under ultrasonication,and the supernatant was diluted with water.Separation was performed on a Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8μm)using a gradient elution with 0.1%formic acid and acetonitrile as the mobile phase.Positive and negative ion scanning was applied in multiple reaction monitoring(MRM)mode for detection,and quantitative determination was conducted via a matrix-matched standard curve with the external standard method.The results demonstrated excellent linearity for the 13 prohibited ingredients in water-based,emulsion,and cream matrices,with correlation coefficients(r)exceeding 0.995.The limits of detection and quantitation were 0.2~2μg/kg and 0.6~6μg/kg,respectively.The recoveries were 77.50%~120.00%,and the relative standard deviations were 1.3%~7.3%.This method offers simple pretreatment,high sensitivity,accuracy,and reliability,and is applicable for efficient and accurate detection of 13 prohibited ingredients in cosmetics.

关 键 词：化妆品 超高效液相色谱–串联质谱法 禁用原料 

分 类 号：O657.63[理学—分析化学]