UPLC-MS/MS测定化妆品中7种禁用物质残留

Determination of seven prohibited substances residues in cosmetics by ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法同时测定化妆品中醋酸曲安奈德、氢化可的松、米诺地尔、螺内酯、坎利酮、雌酮、黄体酮等7种禁用物质残留。以Waters Acquity UPLC BEH C18色谱柱(1.7μm×2.1 mm×50 mm)进行分离,以甲醇和0.2%甲酸水溶液为流动相梯度洗脱,流速为0.2 mL·min^-1,进样量为1μL,采用多反应监测(MRM)扫描方式进行测定。在超高效液相色谱-串联质谱分析过程中以保留时间和离子对(母离子和两个子离子)信息比较定性,以母离子和响应值高的子离子进行定量。所建立的方法在相应的浓度范围内浓度和峰面积的线性关系良好,线性相关系数为0.999 5~0.9999,加标回收率在87.43%~99.24%(n=3)之间,相对标准偏差为1.25%~3.28%(n=6),检出限范围为0.041~3.26μg·kg^-1,定量限范围为0.14~10.87μg·kg^-1。该方法准确、可靠,适用于化妆品中多种禁用物质的同时测定。

A method to determine 7 kinds of prohibited substances residues in cosmetics was established by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry(UPLC-MS/MS).Methods:The UPLC separation was carried out on a Waters Acquity UPLC?BEH C18 column(1.7μm×2.1 mm×50 mm)by gradient elution using methanol and 0.2%formic acid.The flow rate is 0.2 mL·min^-1 and sample injection amount is 1μL.The multiple reaction monitoring(MRM)scanning method was performed.Retention times and charge-mass ratio of compounds(parent ion and two daughter ions)were used for qualitative analysis,and the peak areas of parent ion and daughter ions on high intensity were used for quantitative analysis by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry.The established method has a good linear relationship between concentration and peak area in the corresponding concentration range.The linear correlation coefficients were from 0.9995 to 0.9999.The recoveries were between 87.43%and 99.24%,and the relative standard deviations were from 1.25%to 3.28%.The detection limit were from 0.041μg·kg^-1 to 3.26μg·kg^-1.The limit of quantitation were from 0.14μg·kg^-1 to 10.87μg·kg^-1.In conclusion,the method had accurate and reliable detection results and was suitable for the simultaneous determination of various prohibited substances in cosmetics.