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日用化学工业(中英文) ›› 2025, Vol. 55 ›› Issue (8): 1072-1077.doi: 10.3969/j.issn.2097-2806.2025.08.015

• 分析与检测 • 上一篇    下一篇

高效液相色谱法同时测定化妆品中5种禁用酚类

洪灯1,2,周江3,*(),严媛1,尚凡贞1,刘婷1,王良莉1,谢文1,2   

  1. 1.浙江省检验检疫科学技术研究院,浙江 杭州 311215
    2.杭州海关技术中心,浙江 杭州 311215
    3.义乌市标准化研究院,浙江 义乌 322000
  • 收稿日期:2025-02-16 修回日期:2025-07-14 出版日期:2025-08-22 发布日期:2025-08-28
  • 基金资助:
    杭州海关科研项目资助(2020HZ04);海关总署科研项目资助(2024HK085)

Simultaneous determination of 5 prohibited phenols in cosmetics by high performance liquid chromatography

Deng Hong1,2,Jiang Zhou3,*(),Yuan Yan1,Fanzhen Shang1,Ting Liu1,Liangli Wang1,Wen Xie1,2   

  1. 1. Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou, Zhejiang 311215, China
    2. Technic Center of Hangzhou Customs, Hangzhou, Zhejiang 311215, China
    3. Yiwu Institute of Standardization, Yiwu, Zhejiang 322000, China
  • Received:2025-02-16 Revised:2025-07-14 Online:2025-08-22 Published:2025-08-28
  • Contact: *E-mail: 8849409@qq.com.

摘要:

建立了一种高效液相色谱-二极管阵列检测器(HPLC-DAD)同时测定化妆品中2, 4, 6-三硝基苯酚、2, 4, 6-三氯苯酚、芝麻酚、地乐酚、间苯三酚等5种禁用酚类的方法。样品经甲醇超声提取,高速离心,Eclipse XDB-C18 (250 mm×4.6 mm, 5 μm)分离,以乙腈与0.1% (V/V)磷酸水溶液为流动相进行梯度洗脱,外标法定量。实验结果表明,2, 4, 6-三硝基苯酚在0.125~5.0 μg/mL范围内线性关系良好,相关系数(r)>0.999 9,其余4种禁用酚类在0.25~10.0 μg/mL范围内线性关系良好,相关系数(r)>0.999 8。5种酚类的检出限(LOD)为4~8 mg/kg,定量限(LOQ)为10~20 mg/kg。在低、中、高3个加标水平下,水基类、乳液类、膏霜类、粉类化妆品中5种禁用酚类回收率范围在91.3%~104%,相对标准偏差(RSD)在0.4%~5.1%。本方法具有简便快捷、准确、灵敏等特点,为化妆品中禁用酚类的准确定量提供技术支撑。

关键词: 高效液相色谱, 化妆品, 禁用酚类, 芝麻酚, 2, 4, 6-三硝基苯酚, 2, 4, 6-三氯苯酚

Abstract:

A high performance liquid chromatography (HPLC)-diode array detector (DAD) method was established for the simultaneous determination of 5 kinds of prohibited phenols in cosmetics, including 2, 4, 6-trinitrophenol, 2, 4, 6-trichlorophenol, sesamol, dinoseb, and phloroglucinol. The sample was extracted with methanol in ultrasonic assisted extraction coupled with high speed centrifugation. The separation was performed on Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) using gradient elution with acetonitrile/0.1% (V/V) phosphoric acid solution as the mobile phase, and the content was quantified by external standard method. The results show that 2, 4, 6-trinitrophenol has a good linear relationship in the range of 0.125-5.0 μg/mL with the correlation coefficient higher than 0.999 9, and the other 4 prohibited phenols have good linear relationships in the range of 0.25-10.0 μg/mL with the correlation coefficients all higher than 0.999 8. The limits of detection (LOD) and quantitation (LOQ) of the five phenols are 4-8 mg/kg and 10-20 mg/kg, respectively. The recoveries of 5 kinds of prohibited phenols are ranged from 91.3% to 104%, with the relative standard deviations (RSDs) of 0.4% to 5.1% in water-based, emulsion, cream and powder cosmetics under the three levels of low, medium and high, respectively. The simple-pretreatment, rapid, accurate, high sensitivity method can be used for providing technical support for the accurate quantification of prohibited phenols in cosmetics.

Key words: high performance liquid chromatography (HPLC), cosmetics, prohibited phenols, sesamol, 2, 4, 6-trinitrophenol, 2, 4, 6-trichlorophenol

中图分类号: 

  • TQ658