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    气相色谱-串联质谱法测定防晒化妆品中12种紫外线吸收剂

    GC-MS/MS Determination of 12 UV Absorbers in Sunscreening Cosmetics

    • 摘要: 称取防晒化妆品样品5.0 g,加入饱和氯化钠溶液1 mL,充分混匀后用二氯甲烷为溶剂先后2次萃取样品中12种紫外线吸收剂(UVA)。每次萃取用二氯甲烷5 mL,涡旋振荡60 s,超声萃取30 min,并高速离心5 min。收集并合并2次萃取的上清液,吹氮蒸发至近干,用二氯甲烷溶解残渣并定容至1.0 mL。采用DB-5MS色谱柱为分离柱,进样量为1 μL,在80~300℃区间采用程序升温模式可在30 min内对所测12种UVA实现分离;在电子轰击离子源和选择反应监测模式条件下进行串联质谱测定。测得12种UVA的线性范围均在0.01~1.0 mg·L-1之间,检出限(3S/N)在1.0~3.0 μg·kg-1之间。在不含目标物的空白防晒化妆品中加入12种UVA的混合标准溶液后,按方法分析求得其回收率及测定值的相对标准偏差(n=6),测得两者的结果依次在93.0%~100%之间和1.2%~4.1%之间。

       

      Abstract: A portion (5.0 g) of the sunscreening cosmetic sample was mixed thoroughly with 1 mL of saturated NaCl solution and extracted twice with CH2Cl2 (5 mL for each extraction) to transfer 12 UV absorbers (UVA) into the organic solvent by swirling for 60 s, extracting ultrasonically for 30 min and centrifuging for 5 min with high speed. The supernatants from the 2 extractions were combined and evaporated to near dryness by N2-blowing. The residue was dissolved and made its total volume to 1.0 mL with CH2Cl2. An aliquot of 1 μL of the CH2Cl2 solution was introduced to the chromatographic column of DB-5MS for separation of the 12 UVA under the mode of programed temperature elevation in the temperature interval from 80℃ to 300℃. A clear-cut separation of the 12 UVA was fulfilled within 30 min and their determination was carried out by MS/MS under the modes of EI-ionization source and selected reaction monitoring. Linearity ranges for the 12 UVAs were found same between 0.01-1.0 mg·L-1. Values of their detection limits (3S/N) found were in the range of 1.0 to 3.0 μg·kg-1. Test for recovery and precision was performed by addition of mixed standard solution of the 12 UVA to a blank sunscreening cosmetic sample, giving results of recovery in the range from 93.0% to 100%, and results of RSDs (n=6) in the range from 1.2% to 4.1%.

       

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