超高效液相色谱-串联质谱法测定化妆品中6种生物碱

Determination of 6 Alkaloids in Cosmetics by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了一种同时测定化妆品中6种生物碱(秋水仙碱、萝芙碱、藜芦定、西伐丁、麦角胺、麦角克碱)的超高效液相色谱-串联质谱分析方法。试样用0.1%甲酸-乙腈混合溶剂超声提取,Cleanert PCX固相萃取柱净化,经Thermo Hypersil GOLD色谱柱分离后在多反应监测模式下检测。结果表明:6种生物碱在0.2~20μg/L范围内线性关系良好(r2>0.999 0),方法定量下限为2.0~5.3μg/kg,3个加标水平下的平均回收率为83.9%~101.1%,相对标准偏差为0.7%~6.6%。该方法快速准确、灵敏度高,适用于化妆品中生物碱的安全性评价。

An ultra performance liquid chromatography-tandem mass spectrometric（ UPLC-MS/MS） method was developed for the determination of six alkaloids,e. g. colchicine,raubasine,veratridine,cevadine,ergotamine and ergocristine in cosmetics. The samples were ultrasonically extracted with a mixed solvent of 0. 1% formic acid-acetonitrile,then cleaned up with a Cleanert PCX solid phase extraction column. After separated on a Thermo Hypersil GOLD column,the analytes were detected in multiple reaction monitoring（ MRM） mode. Six alkaloids showed good linearities（ r2 〉0. 999 0） in the range of 0. 2-20 μg/L. The limits of quantitation（ LOQs） of the method for six alkaloids were in the range of 2. 0-5. 3 μg/kg. The average recoveries for six alkaloids at three spiked levels ranged from 83. 9% to 101. 1% with relative standard deviations of 0. 7%-6. 6%.The method was rapid,accurate and sensitive,and could be applied in the safety evaluation on alkaloids in cosmetics.