首页> 中文期刊>分析测试学报 >超高效液相色谱-串联质谱法测定化妆品中6种生物碱

超高效液相色谱-串联质谱法测定化妆品中6种生物碱

     

摘要

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 Hypereil 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0.2-20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, ve-ratridine, 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.

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