超高效液相色谱-三重四极杆质谱法测定化妆品中14种美白活性成分

Determination of 14 whitening active components in cosmetics by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry

建立了同时测定含油化妆品中14种美白活性成分含量的超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)的方法。以20 mmol/L KH_(2)PO_(4)溶液为提取溶剂对化妆品样品进行超声提取,经HLB固相萃取小柱净化,过0.22μm滤膜。选择shim-pack GIST C18 AQ色谱柱分离,以0.1%甲酸溶液(含5 mmol/L乙酸铵)-甲醇作为流动相梯度洗脱,采用电喷雾电离源正负离子切换模式和多反应监测(MRM)模式检测。在最优条件下,14种美白活性成分在10 min内实现有效分离,在各自线性范围内,14种美白活性成分的线性关系良好,相关系数大于0.999,检出限为0.15~2.5 mg/kg,定量限为0.5~7.5 mg/kg,加标回收率为70%~117%,相对标准偏差在0.2%~12%之间。该方法适用于化妆品中美白活性成分的快速检测。

A method based on ultra high performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS) was developed for the analysis of 14 whitening active components in oilycosmetics. The 14 whitening active components were extracted from cosmetics by supersonic extraction with 20 mmol/L potassium dihydrogen phosphate solution, purified by HLB solid phase extraction column and filtered with 0.22 μm filter membrane.Shim-pack GIST C18 AQ chromatographic column was used for the separation of the whitening active components. Methanol-0.1% formic acid solution(containing 5 mmol/L ammonium acetate)was employed as mobile phase for gradient elution, and the analytes were detected by electrospray ionization source with positive and negative ion alternate scanning mode and multiple reaction monitoring mode(MRM). The results showed that an effective separation was achieved within 10 min under the optimized conditions, 14 whitening active components exhibited good linear relationships in the respective linear range with the correlation coefficient more than 0.999. The limits of detection were in the range of 0.15-2.5 mg/kg, and the limits of quantitation were in the range of 0.5-7.5 mg/kg. The recoveries were from 70% to 117%, and the relative standard deviations were between 0.2% and 12%.