液相色谱-串联质谱法同时测定化妆品中非法添加标准外的3种糖皮质激素

Simultaneous Detection of 3 other Standard Glucocorticoids Illegally added in Cosmetics by Liquid Chromatography-Tandem Mass Spectrometry

目的建立同时测定化妆品中非法添加标准外的3种糖皮质激素的液相色谱-串联质谱(LC-MS/MS)法。方法样品经前处理后,采用Agilent ZORBAX SB-C18(2.1 mm×100 mm,1.8μm)色谱柱分离;以0.1%乙酸乙腈溶液和0.1%乙酸水溶液为流动相,梯度洗脱,通过多反应监测(MRM)模式进行检测。结果 3种糖皮质激素在0.05～0.80μg·mL^(-1)范围内线性良好,相关系数r均大于0.999,方法检出限在0.002～0.004 mg·kg^(-1)之间。平均回收率为78.7%～106.8%,相对标准偏差RSD(n=6)为1.4%～1.8%。结论本方法准确可靠、快速灵敏,适用于化妆品中标准以外的3种糖皮质激素的同时测定。

OBJECTIVE To develop an liquid chromatography-tandem mass spectrometry (LC-MS/MS)method for the simultaneous detection of 3 other standard glucocorticoids illegally added in cosmetics.METHODS The samples were pretreated, separated by using a Agilent ZORBAX SB-C18 (2.1mm×100mm,1.8μm)column,followed by gradient elution with 0.1% acetic acid in acetonitrile and 0.1% acetic acid solution as the mobile phase,and were detected with electrospray ionization in multiple reaction monitoring (MRM)mode.RESULTS The calibration curves for the 3cosmetics were linear in the range of 0.05-0.80μg·mL^-1,the correlation coefficients were over 0.999.The average recoveries and RSD (n=6)were 78.7%-106.8% and 1.4%-1.8%,respectively. CONCLUSION The method is accurate,fast,sensitive and suitable for the detection of the 3 other standard glucocorticoids illegally added in cosmetics.