高级检索

    顶空-气相色谱-质谱法测定7种化妆品基质中乙酸乙烯酯的残留量

    Determination of Residue of Vinyl Acetate in Seven Types of Cometics Matrices by Gas Chromatography-Mass Spectrometry with Headspace

    • 摘要: 鉴于乙酸乙烯酯被定义为2B类致癌物而相关检测方法的报道有限,采用题示方法测定唇膏、面霜、按摩精油、啫喱、爽肤水、粉饼、发用摩丝等7种基质样品中乙酸乙酯的残留量。取1.00 g样品置于20 mL顶空瓶中,加入2 g氯化钠、5 mL水,迅速密封,于70 ℃平衡20 min,所得气体采用气相色谱-质谱法分析。在DB-WAX色谱柱上用程序升温条件分离,电子轰击离子源电离,选择离子监测模式检测,基质匹配法定量。结果显示:7种上述基质中乙酸乙烯酯的质量浓度在0.050~2.0 mg·L−1内和峰面积呈线性关系,检出限(3S/N)为0.100 mg·kg−1;按照标准加入法对上述7种空白基质进行回收试验,回收率为88.6%~102%,测定值的相对标准偏差(n=6)为1.4%~6.8%。方法用于30个样品的分析,在1个发用摩丝和3个指甲油(以按摩精油工作曲线定量)中检出了乙酸乙烯酯,检出量分别为0.425,1.23,2.21,0.966 mg·kg−1

       

      Abstract: Given that vinyl acetate is classified as a Group 2B carcinogen and there are limited reports on related detection methods, the described method was used to determine the residue of vinyl acetate in seven types of matrix samples including lipstick, face cream, massage essential oil, gel, toner, powder compact and hair mousse. The 1.00 g of sample was placed in a 20 mL-headspace vial, to which 2 g of sodium chloride and 5 mL of water were added. The mixed solution was quickly sealed and equilibrated at 70 ℃ for 20 min. The resulting gas was then analyzed by a gas chromatography-mass spectrometry. Separation was achieved on a DB-WAX column using a temperature-programmed condition, with electron impact ion source for ionization and selected ion monitoring mode for detection. Quantification was performed using the matrix-matched method. It was shown that linear relationships between values of the mass concentration and peak area of vinyl acetate in the seven matrices mentioned above were kept in the range of 0.050-2.0 mg·L−1, with detection limit (3S/N) of 0.100 mg·kg−1. Recovery tests were conducted on the obove seven blank matrices using the standard addition method, giving recoveries in the range of 88.6%-102%, and RSDs (n=6) of the determined values ranged from 1.4% to 6.8%. The proposed method was applied to the analysis of 30 samples, vinyl acetate was detected in one hair mousse and three nail polishes (quantified using the working curve of massage essential oil) at detection amounts of 0.425, 1.23, 2.21, 0.966 mg·kg−1, respectively.

       

    /

    返回文章
    返回