超高效液相色谱-串联四极杆质谱法筛查青黛中非法掺入的染色物质

Determination of Illegally Added Dye in Indigo Naturalis by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

中文关键词:  超高效液相色谱-质谱联用法  青黛  染色物质

英文关键词:UPLC-MS/MS  indigo naturalis  dye

中文摘要:

      建立了超高效液相色谱-质谱联用法测定青黛中非法掺入的染色物质孔雀石绿、隐色孔雀石绿、天青A、天青B、天青C和亚甲基蓝的检测方法.样品经乙腈溶液（含5%甲酸）提取，采用超高效液相色谱-串联三重四极杆质谱（UPLC-MS/MS）的多反应监测模式（MRM）进行定性和定量检测，其中孔雀石绿、隐色孔雀石绿内标法定量，天青A、天青B、天青C、亚甲基蓝外标法定量.6种染色物质测定的线性范围在1~30 ng/mL之间，孔雀石绿、隐色孔雀石绿、天青A、天青B、天青C、亚甲基蓝的检出限分别为0.5、0.5、1.0、1.0、1.0、1.0 ng/g，定量限分别为1.0、1.0、2.0、2.0、2.0、2.0 ng/g，3个水平的回收率在79.7%~119.7%之间，精密度的RSD%在0.7%~1.8%之间.方法前处理简单，灵敏度高，适用青黛中非法掺入的染色物质孔雀石绿、隐色孔雀石绿、天青A、天青B、天青C和亚甲基蓝的快速检测.

英文摘要:

      A method for the rapid determination of dyes for malachite green, leucomalachite green, azure A, azure B, azure C, methylene blue, which are illegally mixed with indigo naturalis is set up. The samples were extracted with 5% formic acid in acetonitrile, and the qualitative and quantitative detections were carried out using ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) in the multi reaction monitoring mode(MRM). Among them, malachite green and leucomalachite green were quantified using the internal standard method, and azure A, azure B, azure C and methylene blue were quantified using the external standard method. The linear range of the 6 dyes was 1~30 ng/mL, the detection limits of malachite green, leucomalachite green, azure A, azure B, azure C, methylene blue were 0.5、0.5、1.0、1.0、1.0、1.0 ng/g respectively, and the quantitative limits for malachite green, leucomalachite green, azure A, azure B, azure C, methylene blue were 1.0、1.0、2.0、2.0、2.0、2.0 ng/g respectively, the recoveries of the three levels ranged from 79.7% to 119.7%, and the RSD% of precision ranged from 0.7% to 1.8%. The pretreatment of this method is simple, and its sensitivity is high. The method is suitable for the fast detection and analysis of dyes malachite green, leucomalachite green, azure A, azure B, azure C, methylene blue, which are illegally mixed in indigo naturalis.