高效液相色谱-串联质谱法测定化妆品中10种生物碱

Determination of ten alkaloids in cosmetics by high performance liquid chromatography-tandem mass spectrometry

建立高效液相色谱-串联质谱同时测定化妆中10种生物碱的分析方法。实验优化了提取条件、净化方式和仪器条件等参数。样品经80%(v/v)甲醇水溶液超声提取,离心后过滤。采用Waters BEH C 18 色谱柱分离,在多反应监测模式下测定,外标法定量。结果显示,在各自范围内,10种生物碱具有良好的线性关系,相关系数( R 2)> 0.990 0 ,方法的检出限为5.0~12.5 μ g/kg ,定量限为12.5~50.0 μ g/kg 。在1倍、2倍和6倍定量限的加标水平下,10种生物碱的回收率为70.91%~116.75%,相对标准偏差为0.49%~9.98%( n =6)。该方法操作简单,适用于化妆品中10种有毒生物碱的快速筛查和定量分析。

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of ten alkaloids in cosmetics. Extraction conditions, purification methods and instrumental parameters were optimized. The samples were ultrasonically extracted with 80%(v/v) methanol aqueous solution. The extracts were separated and filtered after centrifugation. The analytes were separated on a Waters BEH C 18 column, and detected in the selected reaction monitoring mode. Ten alkaloids were quantified by the external standard method. The ten alkaloids showed good linearity with correlation coefficients ( R 2) greater than 0.990 0 . The limits of detection (LODs) and the limits of quantification (LOQs) of the ten alkaloids were in range of 5.0-12.5 μ g/kg and 12.5-50.0 μ g/kg , respectively . The average spiked recoveries in the cosmetics ranged from 70.91% to 116.75%, and the relative standard deviations (RSDs) ranged from 0.49% to 9.98%. The method can be used for the rapid screening and quantitative analysis of ten alkaloids in cosmetics.