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日用化学工业(中英文) ›› 2025, Vol. 55 ›› Issue (6): 811-816.doi: 10.3969/j.issn.2097-2806.2025.06.016

• 分析与检测 • 上一篇    

超高效液相色谱-三重四极杆/线性离子阱串联质谱法测定睫毛相关化妆品中的7种前列腺素类似物

宫旭*(),孙晶,冯有龙   

  1. 江苏省食品药品监督检验研究院,江苏 南京 210019
  • 收稿日期:2024-07-04 修回日期:2025-05-16 出版日期:2025-06-22 发布日期:2025-07-01
  • 基金资助:
    江苏省食品药品监督管理局科研项目(202316)

Determination of 7 prostaglandin analogsin eyelash-related cosmetics by UPLC-QTRAP-MS/MS

Xu Gong*(),Jing Sun,Youlong Feng   

  1. Jiangsu Institute of Food and Drug Control, Nanjing, Jiangsu 210019, China
  • Received:2024-07-04 Revised:2025-05-16 Online:2025-06-22 Published:2025-07-01
  • Contact: E-mail: gongxuyaoxue@163.com.

摘要: 建立了基于超高效液相色谱-三重四极杆/线性离子阱质谱(UPLC-QTRAP-MS/MS)的分析方法,用于测定睫毛相关化妆品中的7种前列腺素类似物。样品经甲醇超声提取后,利用ACE Excel 2 C18 (100 mm×2.1 mm,2 μm)色谱柱进行分离,流动相为乙腈和5 mmol/L乙酸铵(添加0.05%甲酸)溶液,采用梯度洗脱程序。在ESI+模式,多反应监测(MRM)联合增强子离子扫描(EPI)模式下采集数据,基质匹配标准曲线外标法定量,在保留时间和离子对相对丰度比定性的基础上,通过EPI谱图比对,对目标成分进一步确证。结果表明,7种前列腺素类似物在各自相应的线性范围内呈良好的线性相关性,相关系数r均超过0.999,检出限为0.002 0~0.020 μg/g,定量限为0.005 0~0.050 μg/g。在3个加标水平下,平均回收率为87.3%~107.0%,RSD为0.7%~5.4% (n=6)。利用该方法分析了收集的9批睫毛相关化妆品,1批检出比马前列素。

关键词: 超高效液相色谱-三重四极杆/线性离子阱质谱, 增强子离子扫描, 前列腺素类似物, 睫毛滋养, 化妆品

Abstract:

A method based on ultra-high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry (UPLC-QTRAP-MS/MS) has been developed for the detection and quantification of 7 prostaglandin analogs in eyelash-related cosmetics. Samples were extracted with methanol via ultrasonic extraction and separated on an ACE Excel 2 C18 (100 mm× 2.1 mm, 2 μm) column using a mobile phase of acetonitrile-5 mmol/L ammonium acetate (containing 0.05% formic acid) in a gradient elution mode. Data were collected in the ESI+ mode using multiple reaction monitoring (MRM) combined with enhanced product ion scanning (EPI). Quantification was performed using matrix-matched external standard calibration curves, with both retention times and the ratios of ion pair abundances serving as the basis for qualitative assessments. Further confirmation of target components was achieved through comparison of EPI spectra. The results reveal a strong linear correlation for the 7 prostaglandin analogs within their respective linearity ranges, with the correlation coefficients exceeding 0.999. Sensitivity is characterized by the detection limits ranging from 0.002 0 to 0.020 μg/g and quantitation limits from 0.005 0 to 0.050 μg/g. The average recoveries at three spiked levels are found to be between 87.3% and 107.0%, with the RSDs varying from 0.7% to 5.4% (n=6). This method is used to analyze 9 batches of eyelash-related cosmetics, and 1 batch is found to contain bimatoprost. The developed method, distinguished by its operational straightforwardness, analytical precision, and detection sensitivity, is adeptly applicable for the quantitative determination and qualitative screening of the 7 prostaglandin analogs in cosmetics.

Key words: ultra-high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry, enhanced product ion scan, prostaglandin analogs, eyelash enhancing, cosmetics

中图分类号: 

  • TQ658