化妆品中双香豆素和环香豆素的高效液相色谱二极管阵列检测器测定

Determination of Dicumarol and Cyclocoumarol in Cosmetics by HPLC/DAD

建立了用高效液相色谱（HPLC）／二极管阵列检测器（DAD）测定化妆品中两种香豆素物质——双香豆素和环香豆素的方法。样品用乙腈-氢氧化钠溶液（0．1mol／L）（体积比9：1）的提取溶液超声提取，高效液相色谱DAD扫描检测，并在306nm波长进行分析。用保留时间结合二种香豆素的紫外光谱定性，外标法定量，并且采用液质联用（LC-MS／MS）确证。双香豆素的回收率为96％～105％，精密度RSD为0．51％～2．08％，定量下限为1ng；环香豆素的回收率为88％～104％，精密度RSD为0．51％～3．36％，定量下限为1ng。

A method for simultaneous separation and determination of two coumarins, dicumarol and cyclocoumarol, in cosmetics by HPLC - diode-array detector （DAD） was developed. The cosmetics were extracted by ultrasonic with acetonitrile -NaOH solution（0. 1 mol/L）（9 ： 1, by volume）, The filtrate was injected into RP - HPLC and detected at A = 306 nm. Qualitative analysis of the coumarins was based on their retention times of the chromatogram and their ultraviolet spectra. Quantitative analysis used external standard methods. Furthermore, the results were affirmed by LC- MS/MS. The recoveries, relative standard deviations and limits of quantitation were 96%- 105% , 0. 51%-2. 08% , 1 ng for dicumarol and 88%- 104% , 0. 51%-3.36% , 1 ng for cyclocoumarol, respectively.