朱砂染色现状分析
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篇名: 朱砂染色现状分析
TITLE:
摘要: 目的:分析朱砂药材及饮片染色现状,为朱砂药材及饮片的品质和临床安全应用提供参考依据。方法:采用薄层色谱法(TLC)对药材和饮片中苋菜红、胭脂红、赤藓红、酸性红73、808猩红、靛玉红进行定性鉴别。采用高效液相色谱-质谱联用法(HPLC-MS)检测药材及饮片中的808猩红。HPLC条件:色谱柱为Acquity UPLC BEH C18,流动相为乙腈-0.1%甲酸(70 ∶ 30,V/V),流速为0.3 ml/min,检测波长为520 nm;MS条件:离子源为电喷雾离子源,扫描方式为正离子扫描,检测方式为全扫描二级质谱,雾化器压力为30 psi,干燥气为氮气,离子喷雾电压为4 000 V,碰撞能为30 V,进样量为5 μl。采用容量法测定药材及饮片中硫化汞(HgS)的含量。结果:苋菜红、胭脂红、赤藓红、酸性红73、808猩红、靛玉红的TLC斑点清晰,分离良好。18批样品中有4批808猩红染色,有6批HgS含量不达标(其中3批同时为808猩红染色)。结论:目前市场中流通的朱砂药材及饮片存在染色掺杂和HgS含量不达标等质量问题,应引起重视。
ABSTRACT: OBJECTIVE: To analyze the dyeing status of cinnabar and its pieces, and provide reference for its quality clinical safetey appicaton. METHODS: TLC was used for the qualitative identification of amaranth, carmine, erythrosine, acid red 73, 808 udan and indirubin. HPLC-MS was used to detect the 808 udan : HPLC conditions were as follows, column was Acquity UPLC BEH C18 with mobile phase of cetonitrile-0.1% formic acid (70 ∶ 30,V/V) at a flow rate of 0.3 ml/min, the detection wavelength was 520 nm; MS conditions were as follows, ion source was electrospray ionization source, scanning mode was positive ion scanning with full scanning tandem mass spectrometry, nebulizer pressure was 30 psi, drying gas was nitrogen, ion spray voltage was 4 000 V, collision energy was 30 V, and the injection volume was 5 μl. The volumetric method was used for content determination of HgS. RESULTS: TLC spots of amaranth, carmine, erythrosine, acid red 73, 808 udan and indirubin were clear and well-separated. 4 batches of 808 udan dyeing were included in the 18 batches of samples, 6 batches had non-compliance contents (including 3 batches of 808 udan dyeing). CONCLUSIONS: Dyeing-doped and other quality problems exist in the cinnabaris in markets, which should be noticed.
期刊: 2016年第27卷第27期
作者: 邢潇,刘治民,徐彤彤,谷妲,梁玉冰,张鑫,杨建龙
AUTHORS: XING Xiao,LIU Zhimin,XU Tongtong,GU Da,LIANG Yubing,ZHANG Xin,YANG Jianlong
关键字: 朱砂;染色;硫化汞;质量
KEYWORDS: Cinnabar; Dyeing; HgS; Quality
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