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    超高效液相色谱-串联质谱法测定含海洋生物提取物的化妆品中8种全氟化合物的含量

    Determination of 8 Perfluoroalkyl Compounds in Cosmetics Containing Marine Bioextracts by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 为实现批量含海洋生物提取物的化妆品中多种全氟化合物(PFCs)的快速、准确测定,进行了题示研究。取0.20 g样品,加入约5 mL甲醇,涡旋混匀,超声提取15 min,用甲醇定容至10 mL,于10 ℃离心5 min,上清液过滤过式HLB固相萃取小柱。收集流出液,过0.22 μm有机相滤膜,滤液进入超高效液相色谱-串联质谱仪,其中的8种PFCs在CNW Athena-C18色谱柱上以甲醇-1 mmol·L−1乙酸铵溶液体系作流动相进行梯度洗脱分离,在电喷雾离子源负离子和多反应监测模式下进行质谱分析,基质匹配法定量。结果显示,8种PFCs的质量浓度在0.2~20.0 μg·L−1内和质谱响应值呈线性关系,测定下限(10S/N) 为0.010 μg·g−1。对水剂类、乳液类和霜膏类基质进行加标回收试验,8种PFCs的回收率为79.4%~118%,测定值的相对标准偏差(n=6)为0.10%~8.6%。方法用于80批实际样品的分析,在1批乳液类样品中检出了全氟辛基磺酸和全氟癸烷磺酸(PFDS),检出量分别为0.65,0.55 μg·g−1;在1批霜膏类样品中检出了PFDS,检出量为0.047 μg·g−1

       

      Abstract: To achieve rapid and accurate determination of multiple perfluoroalkyl compounds (PFCs) in batches of cosmetics containing marine bioextracts, the study mentioned by the title was conducted. The 0.20 g of sample was taken, and approximately 5 mL of methanol was added. The mixture was mixed well by vortex, and ultrasonically extracted for 15 min, and its volume was made up to 10 mL with methanol. After centrifuging for 5 min at 10 ℃, the supernatant was passed through filtration-type HLB solid phase extraction column. The eluate was collected, and passed through a 0.22 μm organic phase membrane, and the filtrate was introduced into ultra-high performance liquid chromatograph-tandem mass spectrometer. The 8 PFCs were separated on CNW Athena-C18 column by gradient elution with the mobile phase system consisting of methanol and 1 mmol·L−1 ammonium acetate solution. Mass spectrometric analysis was performed in negative electrospray ionization mode with multiple reaction monitoring mode, and quantification was carried out using the matrix matched method. It was shown that linear relationships between the mass concentrations and mass spectrometry response values of the 8 PFCs were kept in the range of 0.2−20.0 μg·L−1, with lower limits of determination (10S/N) of 0.010 μg·g−1. Spike recovery tests were performed on 3 matrix types (aqueous solutions, emulsions, and creams), giving recoveries of the 8 PFCs in the range of 79.4%−118%, and RSDs (n=6) of the determined values ranged from 0.10% to 8.6%. The proposed method was applied to the analysis of 80 batches of actual samples. Perfluorooctanesulfonic acid and perfluorodecanesulfonic acid (PFDS) in one emulsion sample were detected with detection amounts of 0.65, 0.55 μg·g−1, and PFDS was detected in one cream sample with detection amount of 0.047 μg·g−1.

       

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