超高效液相色谱串联质谱法测定化妆品中禁用药物华法林及其盐类

Determination of warfarin and its salts in cosmetics by Ultra performance liquid chromatography tandem mass spectrometry

本研究建立了化妆品中禁用药物华法林及其盐类的超高效液相色谱串联质谱分析方法。膏霜和乳液类试样依次经氯化钠破乳和溶剂超声辅助萃取,水剂类试样直接经溶剂超声辅助萃取后,萃取液经微孔滤膜过滤后,采用ACQUITY BEH Phenyl色谱柱(2.1 mm×50 mm,1.7μm)分离,以0.1%甲酸-水和甲醇为流动相梯度洗脱,洗脱液经电喷雾离子化和多反应监测模式分析,外标法定量。结果表明,在0.1~10.0 mg/kg范围内,目标物信号强度与其质量浓度(以华法林计)呈良好线性关系(r>0.99),检出限和定量限分别为0.05和0.10 mg/kg,在低、中、高3个添加浓度水平下,华法林的回收率为88.3%~113.7%,相对标准偏差小于7.0%(n=6)。该方法可为化妆品质量安全控制提供科学依据和技术支持。

In this study,a methodology for the determination of warfarin and its salts in cosmetics was developed by ultra performance liquid chromatography tandem mass spectrometry.Cream and emulsion samples were subjected to sodium chloride demulsification and solvent-ultrasound-assisted extraction,water samples were directly subjected to solvent ultrasound-assisted extraction,and the obtained extraction solution was filtered by microporous membrane and separated by an ACQUITY BEH Phenyl column(2.1 mm×50 mm,1.7μm)using 0.1%formic acid-water and methanol as mobile phase by gradient elution.The eluent was analyzed by electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode,and quantified by external standard method.The results showed that there was a good linear relationship(r>0.99)between the signal intensity of the analyte and mass concentration(measured by warfarin)in the range of 0.1-10.0 mg/kg.The limits of detection(LOD)and quantitation(LOQ)were 0.05 and 0.10 mg/kg,respectively.The recoveries of warfarin were 88.3%-113.7%at low,medium and high spiked concentrations and the relative standard deviations(RSDs)were less than 7.0%(n=6).This method can provide scientific basis and technical support for the quality and safety control of cosmetics.