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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 (12): 1629-1634.doi: 10.3969/j.issn.2097-2806.2025.12.016

• 分析与检测 • 上一篇    

超高效液相色谱-串联质谱法测定冬虫夏草化妆品中的腺苷和虫草素

何林1,李春艳1,喻文娟2,傅萍1,楚亮1,*()   

  1. 1 四川省药品检验研究院（四川省医疗器械检测中心、四川养麝研究所） 国家药监局化妆品人体评价和大数据重点实验室， 四川 成都 611731
    2 四川省药品技术检查中心（四川省疫苗检查中心）， 四川 成都 610020
  • 收稿日期:2024-12-23 修回日期:2025-12-18 出版日期:2025-12-22 发布日期:2026-01-23

Determination of adenosine and cordycepin in Cordyceps sinensis cosmetics by ultra performance liquid chromatography coupled with tandem mass spectrometry

Lin He1,Chunyan Li1,Wenjuan Yu2,Ping Fu1,Liang Chu1,*()   

  1. 1 NMPA Key Laboratory for Human Evaluation and Big Data of Cosmetics, Sichuan Institute for Drug Control （Sichuan Testing Center of Medical Devices, Sichuan Institute of Musk Deer Breeding）, Chengdu, Sichuan 611731, China
    2 Sichuan Technical Inspection Center for Medical Products （Sichuan Technical Inspection Center for Vaccine）, Chengdu, Sichuan 610020, China
  • Received:2024-12-23 Revised:2025-12-18 Online:2025-12-22 Published:2026-01-23
  • Contact: *E-mail: 158760662@qq.com.

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摘要：

该研究旨在通过超高效液相色谱-串联质谱法（UPLC-MS/MS），建立一种适用于膏霜乳类和液体（水、油）类基质冬虫夏草化妆品中腺苷和虫草素的测定方法，并对市售化妆品进行检测分析。样品经80%甲醇超声提取，水-0.05%甲酸乙腈溶液梯度洗脱，C18超高效色谱柱快速分离后，正离子多反应监测模式（MRM）检测。结果表明，腺苷和虫草素检出浓度分别为0.000 4和0.002 5 mg/kg；在1~20 ng/mL质量浓度范围内，具有良好线性关系；方法低水平回收率为86.8%~108.0%，RSD≤4.8%（n=6），中、高水平回收率为96.6%~112.2%，RSD≤6.9% （n=6）；标准溶液和加标溶液在4 ℃避光保存下72 h内稳定；市售化妆品有3批检出腺苷，全部批次未检出虫草素。

关键词: 冬虫夏草, 化妆品, 腺苷, 虫草素, 超高效液相色谱-串联质谱法, 市场监管

Abstract:

The aim of this study was to develop a method for the quantification of adenosine and cordycepin in Cordyceps sinensis cosmetics using ultra performance liquid chromatography coupled with tandem mass spectrometry （UPLC-MS/MS）. This method is applicable to various cosmetic matrices, including creams, lotions, and both water-based and oil-based liquids, and was employed to detect and analyze commercially available products. Samples were subjected to ultrasonic extraction using 80% methanol, followed by gradient elution with a water-acetonitrile solution （containing 0.05% （V/V） formic acid）. Rapid separation was achieved using a C18 ultra performance liquid chromatography column, and detection was performed in positive ion multiple reaction monitoring （MRM） mode. The detection limits for adenosine and cordycepin were set at 0.000 4 mg/kg and 0.002 5 mg/kg, respectively. Within the mass concentration range of 1 to 20 ng/mL, both compounds demonstrate a strong linear relationship. At low mass concentrations, the recovery rates range from 86.8% to 108.0%, with an RSD of ≤4.8% （n=6）. For medium and high mass concentrations, the recovery rates are between 96.6% and 112.2%, with an RSD of ≤6.9% （n=6）. Standard solutions and spiked solutions remain stable for up to 72 hours when store at 4 ℃ in the dark. Furthermore, adenosine is detected in three batches of commercial cosmetics, while cordycepin is not detected in any of the tested batches. The developed method exhibits high detection efficiency and sensitivity, as well as excellent accuracy and precision, making it a valuable auxiliary regulatory tool for verifying the claims of Cordyceps sinensis cosmetic ingredient additions. The accumulated data can provide robust technical support for the development and revision of raw material standards.

Key words: Cordyceps sinensis, cosmetics, adenosine, cordycepin, ultra performance liquid chromatography coupled with tandem mass spectrometry, market regulation

中图分类号: 

  • TQ658