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日用化学工业（中英文）

日用化学工业（中英文） ›› 2025, Vol. 55 ›› Issue (2): 244-252.doi: 10.3969/j.issn.2097-2806.2025.02.014

• 分析与检测 • 上一篇    下一篇

超高效液相色谱-三重四极杆/线性离子阱质谱法测定化妆品中16种荧光增白剂

宫旭1,刘雪静2,尚姝1,向健华2,吴莉1,冯有龙1,方方1,*()   

  1. 1.江苏省食品药品监督检验研究院，江苏 南京 210019
    2.中国药科大学 中药学院，江苏 南京 211198
  • 收稿日期:2024-04-07 修回日期:2025-01-20 出版日期:2025-02-22 发布日期:2025-02-28
  • 通讯作者: 方方
  • 基金资助:
    江苏省市场监督管理局科技计划项目(KJ207560);江苏省药品监督管理局科研计划项目(202211)

Determination of 16 fluorescent whitening agents in cosmetics by ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry

Xu Gong1,Xuejing Liu2,Shu Shang1,Jianhua Xiang2,Li Wu1,Youlong Feng1,Fang Fang1,*()   

  1. 1. Jiangsu Institute of Food and Drug Control, Nanjing, Jiangsu 210019, China
    2. School of Traditional Chinese Pharmacy, China Pharmaceutical University, Nanjing, Jiangsu 211198, China
  • Received:2024-04-07 Revised:2025-01-20 Online:2025-02-22 Published:2025-02-28
  • Contact: Fang Fang

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摘要：

建立超高效液相色谱-三重四极杆/线性离子阱质谱法（UPLC-QTRAP-MS/MS）测定化妆品中16种荧光增白剂（FWAs）的分析方法。样品经甲醇超声提取后，0.45 μm聚四氟乙烯微孔滤膜过滤，取续滤液用ACE Excel 2 C18（50 mm×2.1 mm，2 μm）色谱柱分离，以乙腈-5 mmoL/L乙酸铵溶液为流动相进行梯度洗脱，采用电喷雾电离，在正、负离子模式下，以多反应监测（MRM）模式定性定量的基础上，联合增强子离子扫描（EPI）模式进行检测，获得化合物更为丰富的二级碎片信息，对目标成分进一步定性确证。分别以水剂、乳液和膏霜为基质进行方法学考察，结果表明，16种FWAs在各自质量浓度范围内线性关系良好，相关系数均大于0.995，检出限为0.005 9~5.6 μg/g，定量限为0.015~14 μg/g。在2个加标水平下，平均回收率为72.1%~115.8%，RSD为0.5%~12.6% （n=6）。利用该方法分析了收集的82批美白类化妆品，6批检出FWAs。本方法操作简单，分析速度快，结果准确，适用于化妆品中16种FWAs的检测，为化妆品安全风险监测和质量监管提供技术支持。

关键词: 荧光增白剂, 超高效液相色谱-三重四极杆/线性离子阱质谱法, 增强子离子扫描, 化妆品

Abstract:

A method for the determination of 16 fluorescent whitening agents （FWAs） in cosmetics by ultra performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry （UPLC-QTRAP-MS/MS） was established. The sample was extracted by methanol, filtered by microporous polytetrafluoroethylene （PTFE） filter membrane after ultrasonic vortex. The separation was performed on ACE Excel 2 C18 （50 mm×2.1 mm, 2 μm） column. Gradient elution was carried out with acetonitrile and 5 mmoL/L ammonium acetate solution as mobile phases. In positive and negative ionization modes of electrospray ionization source （ESI）, multiple reaction monitoring （MRM） mode combined with enhanced product ion （EPI） mode were used for detection. The external standard calibration was used for quantification, based on the retention time and abundance ratio of characteristic ions, and compound-specific fragment information was obtained through EPI to further qualify and confirm the target components. The precision and accuracy of the method were investigated using liquid-based, emulsion-based and cream-based cosmetic as matrices. The results show that 16 FWAs have good linear relationship within their respective mass concentration ranges, with the correlation coefficients greater than 0.995. The detection limits are 0.005 9-5.6 μg/g, and the quantification limits are 0.015-14 μg/g. At the two spiked levels, the average recoveries are 72.1%-115.8%, and the average relative standard deviations are 0.5%-12.6% （n=6）. Using this method, 82 batches of whitening cosmetics collected are analyzed, and 6 batches are detected with FWAs. This method is simple, fast, accurate, and suitable for the detection of 16 FWAs in cosmetics, providing technical support for cosmetic risk monitoring and quality supervision.

Key words: fluorescent whitening agents （FWAs）, UPLC-QTRAP-MS/MS, enhanced product ion scan （EPI）, cosmetic

中图分类号: 

  • TQ658