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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 (10): 1352-1360.doi: 10.3969/j.issn.2097-2806.2025.10.016

• 分析与检测 • 上一篇    

染发产品中14种禁用成分的高效液相色谱法测定及质谱确证

左雪,杨玲,于睿鹏,邸铮,张华珺*()   

  1. 北京市药品检验研究院（北京市疫苗检验中心），北京 102206
  • 收稿日期:2024-10-15 修回日期:2025-10-28 出版日期:2025-10-22 发布日期:2025-12-03
  • 通讯作者: 张华珺

Determination of 14 prohibited ingredients in hair dye products by HPLC and verification by LC-MS/MS

Xue Zuo,Ling Yang,Ruipeng Yu,Zheng Di,Huajun Zhang*()   

  1. Beijing Institute for Drug Control （Beijing Center for Vaccine Control）, Beijing 102206, China
  • Received:2024-10-15 Revised:2025-10-28 Online:2025-10-22 Published:2025-12-03
  • Contact: Huajun Zhang

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摘要：

建立了染发产品中14种禁用成分的高效液相色谱测定方法及液相色谱-串联质谱确证方法。染发产品经亚硫酸氢钠水溶液和乙醇的混合溶液超声提取后，以乙腈-20 mmol/L乙酸铵水溶液为流动相，在TechMate AQUA-STIII （4.6 mm×250 mm，5 µm）色谱柱上进行梯度洗脱，采用二极管阵列检测器进行分析，检测波长为240，290和616 nm，外标法定量。阳性样品采用液相色谱-串联质谱法进行进一步确证。14种禁用成分线性关系良好，相关系数（r）均大于0.999。14种成分的方法检出限为2.4~52 mg/kg，定量限为10~207 mg/kg。在2个不同含量水平下，各成分的精密度和48 h内稳定性良好，峰面积RSD均小于5%。在乳膏和液体类基质中，各成分在4个不同含量添加水平下的平均回收率为89.4%~112.8%，RSD值为0.4%~4.6%。在该实验条件下，14种禁用成分的检测不受染发产品中常用准用染发剂的干扰。

关键词: 禁用成分, 染发产品, 高效液相色谱法, 液相色谱-串联质谱法

Abstract:

A method for the determination of 14 prohibited ingredients in hair dye products by high performance liquid chromatography （HPLC） and liquid chromatography-tandem mass spectrometry （LC-MS/MS） was developed. The hair dye product was ultrasonically extracted in mixed solvent of aqueous sodium bisulfite solution and ethanol. The mobile phase for HPLC determination was acetonitrile and 20 mmol/L ammonium acetate. Chromatographic separation was carried out on a TechMate AQUA-STIII column （4.6 mm×250 mm, 5 µm） by isocratic elution. The detection wavelengths of the diode array detector were 240, 290 and 616 nm. Quantification was performed by external standard method. Further verification for positive sample was performed by LC-MS/MS. The 14 prohibited ingredients have good linearities, with the correlation coefficients （r） higher than 0.999. The limits of detection （LODs） of the 14 ingredients are from 2.4 mg/kg to 52 mg/kg, and the limits of quantification （LOQs） are from 10 mg/kg to 207 mg/kg. At two different content levels, the precision and stability within 48 hours of each target ingredient is good, with the relative standard deviation （RSD） less than 5%. The average spiked recoveries at four levels in both cream and liquid substrates are from 89.4% to 112.8%, with the RSDs from 0.4% to 4.6%. Under the conditions of this experiment, the detection of 14 prohibited ingredients is not affected by the interference of frequently-used permitted dyes in hair dye products.

Key words: prohibited ingredients, hair dye products, high performance liquid chromatography, liquid chromatography-tandem mass spectrometry

中图分类号: 

  • TQ658