高效液相色谱-串联质谱法(HPLC-MS)测定苦丁茶中的孔雀石绿和隐色孔雀石绿

Determination of Malachite Green and Leucomalachite Green in Kudingcha by HPLC-MS

建立高效液相色谱串联质谱法测定苦丁茶中孔雀石绿及其代谢物的分析方法。样品经乙腈提取,中性氧化铝固相萃取柱净化后用高效液相色谱串联质谱检测,内标法定量。结果表明,孔雀石绿在1.088~54.400μg/L,隐色孔雀石绿1.056~52.800μg/L质量浓度范围内,线性关系良好(R>0.999)。孔雀石绿和隐色孔雀石绿的检出限分别为0.40μg/kg与2.5μg/kg,平均回收率为91.82%~106.70%,RSD≤12.6%。对抽检的5份苦丁茶进行孔雀石绿和隐色孔雀石绿检测,总含量范围为20.90×10^(3)~5.87×10^(3)μg/kg。该方法操作简单、准确可靠、灵敏度高、重复性好,可用于苦丁茶中孔雀石绿及其代谢物的测定。

To establish a method for the determination of residual malachite green and leucomalachite green in kudingcha by high performance liquid chromatography tandem mass spectrometry.The kudingcha was extracted by acetonitrile,purified by neutral alumina solid phase extraction column,filtered by 0.22μm microporous membrane and detected by high performance liquid chromatography tandem mass spectrometry.The results showed that the linear relationship of the two compounds was good in the concentration range of 1.088~54.400μg/L(malachite green),1.056~52.800μg/L(leucomalachite green),and both correlation coefficient were greater than 0.999.The limits detection of malachite green and leucomalachite green were 0.40μg/kg and 2.5μg/kg,the recoveries were 91.82%~106.70%,and the relative standard deviation was less than 12.6%.Malachite green and leucomalachite green were detected in 5 samples sampled by supervision,the total content range was 20.90×10^(3)~5.87×10^(3)μg/kg.Conclusion:The method is simple,accurate,reliable,sensitive and reproducible,and is suitable for the detection of malachite green and leucomalachite green in kudingcha.