超高效液相色谱-串联质谱法同时测定防晒剂化妆品16种紫外线吸收剂

Determination of 16 UV-absorbents in sun-screening cosmetics by ultra-performance liquid chromatography-tandem mass spectrometry

目的建立了防晒剂化妆品中16种紫外线吸收剂的超高效液相色谱-串联质谱分析方法。方法样品经少量四氢呋喃提取,用甲醇∶水(3∶1,V/V)定容,涡旋超声提取后,采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm)分离,以0.1%甲酸甲醇-0.1%甲酸水溶液为流动相,梯度洗脱。采用多反应监测(MRM)模式进行质谱确认,根据保留时间和特征离子的相对丰度比进行定性,外标法定量。结果 16种紫外线吸收剂在20 ng/ml^500 ng/ml响应值与浓度呈良好线性关系,方法定量限为1.4μg/g^8.6μg/g,以样品的空白中加入低、中、高3个水平点的平均回收率为82.1%~97.2%,相对标准偏差(RSD)为1.4%~6.6%。结论该方法适用膏状、乳状防晒剂化妆品,灵敏度高,重现性好。用于防晒剂化妆品中16种紫外线吸收剂的检测具有良好的适应性。

Objective An analytical method for the simultaneous determination of sixteen ultraviolet filters in sun-screening cosmetics was established by ultra—performance liquid chromatography—tandem mass spectrometry(UPLC—MS/MS).Methods The cosmetic sample was extracted by a small amount of tetrahydrofuran and conducted for constant volume with methanol:water(3:1,V/V).After vortex ultrasonic extraction,the extraction was separated using a Waters ACQUITY UPLC BEH C18 column(2.1mm×50mm,1.7μm)with a gradient elution of 0.1%formic acid methanol and 0.1%formic acid aqueous solution.The analyte was confirmed by MS/MS in the multiple reaction monitoring(MRM)mode.The qualitative analyte was based on the retention time and the relative abundance ratio of the characteristic ions and quantitative analysis on calibration curve method.Good linear relationship displayed within 20 ng/ml-500 ng/ml for all of target components.Results The LOQ level for 16 UV-absorbents was within 1.4μg/g-8.6μg/g,and recoveries were within 82.1%-97.2%,with relative standard deviations(RSD)of 1.4%-6.6%.Conclusion The method is suitable for creamy or milky sunscreen cosmetics due to its high sensitivity and good reproducibility.It can be used for the detection of 16 UV-absorbents in cosmetics.