朱砂中添加色素的HPLC-Q-TOF/MS分析以及TLC和HPLC检测方法的建立  

Analysis of added pigments in cinnabar by HPLC-Q-TOF/MS and establishment of determination method by TLC and HPLC

作　　者：张燕飞[1] 耿昭[1,2] 黄再强 胡明勋[1] 王甜甜[1] 陈玲[1] 李心怡[1] 蒋运斌[1] 汤韵秋 解云彤 周娟 马逾英[1] 

机构地区：[1]成都中医药大学药学院,成都611137 [2]四川省食品药品检验检测院,成都610079

出　　处：《药物分析杂志》2017年第5期852-861,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：中药安全检测技术及标准平台项目(2014ZX09304307)

摘　　要：目的:采用高效液相色谱-四极杆飞行时间质谱(HPLC-Q-TOF/MS)技术对11批疑似添加色素的朱砂样品中添加色素进行分析鉴定;并建立相应添加色素的TLC和HPLC检测方法。方法:采用正离子扫描方式,依据高分辨质谱提供的准分子离子峰和碎片离子的精确分子质量信息,确证有关物质及其特征碎片离子的分子组成;再结合对照品对照与相关文献数据,鉴定朱砂中添加的色素。采用TLC和HPLC建立朱砂药材中色素的检测方法。结果:应用HPLC-Q-TOF/MS法明确了朱砂中添加的色素为808猩红、金光红C、苏丹红Ⅳ3种偶氮类色素;样品的TLC图谱斑点清晰,分离度好;样品的HPLC图谱中808猩红、金光红C、苏丹红Ⅳ色谱峰分离度好,耐用性好;11批朱砂中均检出有808猩红,7批均检出金光红C,3批检出苏丹红Ⅳ。结论:本实验建立的TLC和HPLC方法简便,专属性强,可为朱砂药材的质量控制提供一定的参考;HPLC-Q-TOF-MS技术可快速鉴别朱砂中添加的色素。Objective： To identify suspiciously added pigments in 11 batches of cinnabar samples by high performance liquid chromatography coupled with quadrupole time of flight tandem mass spectrometry （ HPLC-Q-TOF/MS ）and to establish the corresponding determination method by TLC and HPLC. Methods： Positive ion scanning mode was used in TOF-MS. The pigments were identified based on precise molecular weight of the quasi- molecular ions and their fragment ions, with aid of reference substances and literature review. And the corresponding determination method was established by TLC and HPLC methods. Results： Three azo pigments, namely 808 scarlet, lake red C and sudan 1V were identified. TLC chromatograms showed clear spots with good resolution. HPLC chromatograms of 808 scarlet, lake red C and sudan IV showed good resolution and durability. 808 scarlet was detected in all samples, lake red C was detected in 7 samples and sudan IV was detected in 3 samples. Conclusion： The established TLC and HPLC methods were simple and exclusive, which offered reference for quality control of cinnabar. HPLC-Q-TOF-MS method could identify the pigments in cinnabar accurately and rapidly.

关 键 词：矿物药 朱砂 辰砂 硫化汞 偶氮类色素 金光红C 808猩红 苏丹红Ⅳ 安全监测 液相色谱-四极杆飞行时间串联质谱 薄层色谱法 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]