Lin Weixuan, Sun Xingquan, Ma Jie
Liaoning Entry-Exit Inspection and Quarantine Bureau, Dalian 116001, China.
Se Pu. 2013 May;31(5):410-5. doi: 10.3724/sp.j.1123.2012.11015.
A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been established for the simultaneous determination of eleven ultraviolet absorbents in sunscreening 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 x 4.6 mm, 5 microm) 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.
建立了一种液相色谱-串联质谱(LC-MS/MS)法同时测定防晒化妆品中的11种紫外线吸收剂。化妆品样品用甲醇-乙醇-水(80:10:10,v/v/v)提取。提取物在Eclipse XDB-C18色谱柱(150 mm×4.6 mm,5μm)上通过反相高效液相色谱分离,以含0.1%甲酸的乙腈和水进行梯度洗脱。采用多反应监测(MRM)模式通过MS/MS检测分析物。定性分析基于保留时间和特征离子的相对丰度比,定量分析采用校准曲线法。研究结果表明,11种紫外线吸收剂的定量限(LOQ,S/N = 10)为200~500 mg/kg,平均回收率为77.17%~98.32%,相对标准偏差为2.40%~11.11%。该方法适用于检测霜状和乳状防晒化妆品中的11种紫外线吸收剂。