液相色谱-串联质谱法同时检测防晒化妆品中的11种紫外吸收剂

建立了防晒化妆品中11种紫外吸收剂的液相色谱-串联质谱检测方法。样品经甲醇-乙醇-水(80:10:10, v/v/v)提取,利用Eclipse XDB-C₁₈色谱柱(150 mm×4.6 mm, 5 μm)分离,以乙腈和0.1%甲酸水溶液为流动相,梯度洗脱。采用多反应监测(MRM)模式进行质谱测定,根据保留时间及质谱图上特征离子的相对丰度比进行定性,外标法定量。结果表明:该方法11种紫外吸收剂的定量限范围为200～500 mg/kg,回收率为77.17%～98.32%,相对标准偏差为2.40%～11.11%。该方法对于膏状和乳状防晒化妆品中的11种紫外吸收剂具有较好的适用性。

Determination of 11 ultraviolet absorbents in sun-screening cosmetics by liquid chromatography-tandem mass spectrometry

A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been established for the simultaneous determination of eleven ultraviolet absorbents in sun-screening cosmetics. The cosmetic sample was extracted by methanol-ethanol-water (80:10:10, v/v/v). The extract was separated by reversed-phase high performance liquid chromatography on an Eclipse XDB-C₁₈ chromatographic column (150 mm×4.6 mm, 5 μm) with a gradient elution of acetonitrile and water containing 0.1% formic acid. The analyte was detected by MS/MS with the multiple reaction monitoring (MRM) mode. The qualitative analysis was based on the retention time and the relative abundance ratio of the characteristic ions, and quantitative analysis on calibration curve method. The research results showed that the limits of quantification (LOQ, S/N=10) of the eleven ultraviolet absorbents ranged from 200 to 500 mg/kg and the average recoveries ranged from 77.17% to 98.32% with the relative standard deviations from 2.40% to 11.11%. The method is suitable to detect the eleven ultraviolet absorbents in cream and milky sun-screening cosmetics.