HPLC同时测定化妆品中22种香豆素类化合物及质谱确证

Simultaneous Determination of 22 Coumarins in Cosmetics by HPLC and Verification by Mass Spectrometry

关键词:  化妆品  高效液相色谱法  液相色谱-串联质谱法  香豆素类化合物

Key words:  cosmetics  HPLC  LC-MS/MS  coumarins

摘要:

目的 建立同时测定化妆品中22种香豆素类化合物的HPLC及液相色谱-串联质谱验证方法。方法 采用Agilent Eclipse XDB-Phenyl色谱柱(150mm×4.6mm,3.5μm),流动相为乙腈-0.1%磷酸,梯度洗脱,流速为1.0mL·min^-1,柱温为35℃,检测波长分别为227,310nm。以HPLC结果进行定性筛查,并采用标准曲线法定量,以液相色谱-串联质谱法的结果进行确证。结果 22种香豆素类化合物的线性范围为0.1~10mg·L^-1,相关系数均>0.9993,方法检出浓度为0.1~1.5mg·kg^-1,在低、中、高3种加标水平下,平均回收率为91.4%~114.8%,RSD为0.1%~4.8%。结论 该方法操作简便、准确,适用于膏乳、水剂、粉类及精油类化妆品中22种香豆素类化合物的检测。

Abstract:

OBJECTIVE To establish a method for the simultaneous determination of 22 coumarins in cosmetics by HPLC and verification by LC-MS/MS.METHODS Agilent Eclipse XDB-Phenyl chromatographic column(150 mm×4.6 mm, 3.5 μm)was used for gradient elution at a flow rate of 1.0 mL·min-1 with acetonitrile-0.1% phosphoric acid as the mobile phases. The column temperature was set at 35 ℃. The wavelengths of detection were 227, 310 nm. The results of HPLC were used for qualitative screening, the standard curve method was used for quantification, and the results of LC-MS/MS were used for verification.RESULTS The linear ranges of the 22 coumarins were 0.1-10 mg·L^-1, and the correlation coefficients were >0.999 3.The detection limits were 0.1-1.5 mg·kg^-1. The average recoveriese were 91.4%-114.8% with RSDs of 0.1%-4.8% at low, medium and high spiked levels.CONCLUSION The method is simple, accurate and suitable for the detection of 22 coumarins in creams,lotions, powdery sample and essential oil cosmetics.