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日用化学工业（中英文）

日用化学工业（中英文） ›› 2023, Vol. 53 ›› Issue (2): 239-244.doi: 10.3969/j.issn.1001-1803.2023.02.016

• 分析与检测 • 上一篇    

气相色谱-质谱法测定化妆品中苯甲酸酯类和对羟基苯甲酸酯类16种防腐剂

吕稳1,2,张静雅1,2,胡贝1,2,*(),刘红1,2,黄伟1,2   

  1. 1.湖北省药品监督检验研究院，湖北 武汉 430075
    2.湖北省药品质量检测与控制工程技术研究中心，湖北 武汉 430075
  • 收稿日期:2022-02-08 修回日期:2023-02-02 出版日期:2023-02-22 发布日期:2023-02-23

Determination of 16 preservatives of benzoates and parabens in cosmetics by GC-MS

Lü Wen1,2,Zhang Jingya1,2,Hu Bei1,2,*(),Liu Hong1,2,Huang Wei1,2   

  1. 1. Hubei Institute for Drug Control, Wuhan, Hubei 430075, China
    2. Hubei Engineering Research Center for Drug Quality Control, Wuhan, Hubei 430075, China
  • Received:2022-02-08 Revised:2023-02-02 Online:2023-02-22 Published:2023-02-23
  • Contact: *Tel.: +86-27-87705269, E-mail: 303710958@qq.com.

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摘要：

建立了测定化妆品中苯甲酸酯类和对羟基苯甲酸酯类防腐剂的气相色谱-质谱（GC-MS）方法。样品经饱和氯化钠和乙酸乙酯提取，离心后取上清液用乙腈定容。提取液经HP-5ms毛细管色谱柱（30 m×250 μm×0.25 μm）分离，采用选择离子监测模式（SIM）扫描测定，外标法定量。16种防腐剂在相应的线性范围内线性关系良好，其中苯甲酸酯类的检出限和定量限分别为0.3 μg/g和1 μg/g，对羟基苯甲酸酯类的检出限和定量限分别为0.6 μg/g和2 μg/g。实验选取了3种基质在两个水平下验证方法的回收率和精密度，16种防腐剂的加标回收率为85.4%~113.8%，相对标准偏差（RSD，n=6）≤10.9%。检测的50批婴幼儿类化妆品中对羟基苯甲酸甲酯和对羟基苯甲酸丙酯的使用频率最高，分别为50%和36%，添加量均符合规定。

关键词: 化妆品, 气相色谱-质谱法, 苯甲酸酯类, 对羟基苯甲酸酯类, 防腐剂

Abstract:

A method for the determination of benzoate and paraben preservatives in cosmetics by gas chromatography-mass spectrometry （GC-MS） was established. The sample was extracted by saturated sodium chloride and ethyl acetate, then the supernatant was fixed to volume with acetonitrile after centrifugation. The extracted solution was separated by the chromatographic column of HP-5ms （30 m×250 μm×0.25 μm）. The determination was carried out under the mode of selected ion monitoring （SIM） and the external standard method was used for quantitative determination. All the 16 preservatives show good linearity in the corresponding range, the LOD and LOQ of benzoates are 0.3 μg/g and 1 μg/g, respectively, and the LOD and LOQ of parabens are 0.6 μg/g and 2 μg/g, respectively. Three types of cosmetics are selected to verify the accuracy and precision of the method at two levels. The average spiked recoveries of the 16 preservatives are 85.4%-113.8%, and the corresponding relative standard deviations （RSDs, n=6） ≤10.9%. The use frequency of methylparaben and propylparaben in 50 baby cosmetics are 50% and 36%, respectively, and the maximum contents are lower than the limit of relevant requirements.

Key words: cosmetics, gas chromatography-mass spectrometry （GC-MS）, benzoate, paraben, preservatives

中图分类号: 

  • TQ658