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机构地区:[1]辽宁出入境检验检疫局技术中心,辽宁大连116001 [2]大连工业大学生物与食品工程学院,辽宁大连116033
出 处:《色谱》2013年第5期410-415,共6页Chinese Journal of Chromatography
基 金:国家质量监督检验检疫总局项目(2009IK-149)
摘 要:建立了防硒化妆品中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(150mm×4.6mm,5μm)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200~500mg/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硒化妆品中的11种紫外吸收剂具有较好的适用性。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 chromatogra- phy on an Eclipse XDB-C~ chromatographic column ( 150 mm x4.6 mm, 5μm) 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 quantifica- tion ( 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.
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