化妆品中18种香豆素类物质的液相色谱检测和质谱确证

Determination and Verification of 18 Coumarins in Cosmetics by Liquid Chromatography and Mass Spectrometry

建立了化妆品中18种香豆素类物质的高效液相色谱检测方法。将膏乳和水剂样品用甲醇溶解,粉剂和唇膏类样品采用四氢呋喃-甲醇(体积比1∶1)混合溶液溶解,超声提取。采用C18色谱柱分离18种香豆素类物质,以乙腈和0.05mol/L乙酸铵(含质量分数0.25%乙酸)溶液为流动相,梯度洗脱分离,在248nm、280nm和320nm波长下分别测定。疑似阳性样品采用高效液相色谱-串联质谱法进行确证。18种香豆素类物质的回归曲线在0.4~50 mg/L范围内线性良好,相关系数均大于0.99,检出限为0.5~1.0 mg/kg,四种基质的方法回收率为80.1%~119.4%。该方法简便、可靠,能够满足化妆品中18种香豆素类物质的检测要求。

A high performance liquid chromatography method had been developed for the determination of 18 coumarins in cosmetics.The cream and water samples were dissolved in methanol,and the powder and lipstick samples were dissolved in a tetrahydrofuran-methanol(volume ratio 1/1)mixed solution and ultrasonically extracted.18 Kinds of coumarins were separated by C18 column with acetonitrile and 0.05 mol/L ammonium acetate(containing mass fraction of 0.25%acetic acid)solution as mobile phase by gradient elution,measured at 248 nm,280 nm and 320 nm,respectively.Suspected positive samples were confirmed by liquid chromatography-tandem mass spectrometry.The detection limit was 0.5-1.0 mg/kg.In the range of 0.4-50 mg/L,the calibration curves of 18 coumarins showed good linearity with the correlation coefficients higher than 0.99.The recoveries were 80.1%-119.4%.The method is simple and reliable,and can be used for the detection of 18 kinds of coumarin substances in cosmetics.