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

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Ⅳ 3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 Ⅳ 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 sudanⅣ 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.

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