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日用化学工业 ›› 2021, Vol. 51 ›› Issue (8): 795-801.doi: 10.3969/j.issn.1001-1803.2021.08.015

• 分析与检测 • 上一篇    下一篇

固相萃取-高效液相色谱法测定化妆品中15种卡因类禁用组分

芦丽(),方方,冯有龙,曹玲   

  1. 江苏省食品药品监督检验研究院,江苏 南京 210008
  • 收稿日期:2020-11-23 修回日期:2021-08-02 出版日期:2021-08-22 发布日期:2021-08-24
  • 通讯作者: 芦丽
  • 基金资助:
    江苏省市场监督管理局科技计划项目(KJ207560)

Determination of 15 caine-type prohibited ingredients in cosmetics by solid phase extraction-high performance liquid chromatography

Lu Li(),Fang Fang,Feng Youlong,Cao Ling   

  1. Jiangsu Institute for Food and Drug Control, Nanjing, Jiangsu 210008, China
  • Received:2020-11-23 Revised:2021-08-02 Online:2021-08-22 Published:2021-08-24
  • Contact: Li Lu

摘要:

建立了不同基质化妆品中15种卡因类局麻药物含量测定的固相萃取-高效液相色谱分析方法。不同基质样品经不同溶剂提取,MCX固相萃取净化,经C18色谱柱(250 mm×4.6 mm×5 μm)分离,流动相采用甲醇-0.01 moL/L磷酸氢二钠水溶液(磷酸调pH 7.0)梯度洗脱,流速1.0 mL/min,检测波长230 nm,柱温30 ℃,标准曲线法定量。结果表明,15种卡因类局麻药物在相应质量浓度范围内线性关系良好,相关系数均大于0.999;检出限为1~13 mg/kg,定量限为3~29 mg/kg。液态水基凝胶类、膏霜乳液类、液态油基类3种不同基质在低、高两个水平的平均加样回收率分别为90.9%~108.0%,87.5%~104.5%和87.7%~105.0%,相对标准偏差RSD分别为0.1%~3.6%,1.1%~8.8%和0.5%~6.0%。该方法高效、准确、耐用,为化妆品中卡因类局麻药物定量筛查提供了一种有效的分析方法。

关键词: 化妆品, 卡因类局麻药物, 高效液相色谱, 固相萃取

Abstract:

A solid phase extraction- high performance liquid chromatographic(HPLC) method was developed for the simultaneous determination of 15 caine-type prohibited ingredients in cosmetics. The samples were extracted by different solvent, then purified by solid phase extraction. Chromatographic separation was achieved on an C18 chromatographic column (250 mm×4.6 mm×5 μm). The column temperature was 30 ℃ through gradient elution with methanol-aqueous solution of 0.01 moL/L Na2HPO4 (pH 7.0) as binary mobile phase at a flow rate of 1.0 mL/min, and the detection wavelength was 230 nm. The standard curve method was used for quantification. The results show that the linear correlation coefficients of the 15 compounds are all greater than 0.999. The LODs of 15 caine-type prohibited ingredients are in the range of 1-13 mg/kg, while the LOQs are in the range of 3-29 mg/kg. The average recoveries at two spiked levels of astringent, milk and oil matrix are in the range of 90.9%-108.0%, 87.5%-104.5% and 87.7%-105.0% respectively, with RSDs of 0.1%-3.6%, 1.1%-8.8% and 0.5%-6.0% respectively. This method is proved to be efficient, accurate and durable, which provids an effective detection technique for 15 caine-type prohibited ingredients in cosmetics

Key words: cosmetics, caine-type local anesthetics, high performance liquid chromatography, solid phase extraction

中图分类号: 

  • TQ658