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目的:建立基于液质联用法的中药材及饮片中常见染色掺假物质的快速筛查方法。方法:采用Poroshell 120 EC-C_(18)色谱柱(3.0 mm×100 mm,2.7μm),以乙腈和0.02 mol·L~(-1)的乙酸铵水溶液为流动相进行梯度洗脱,流速0.4mL·min~(-1),柱温35℃,检测波长为428、483、509、608 nm;采用电喷雾电离源(ESI),正离子模式检测,扫描质谱扫描范围m/z 100~1 000。将胭脂红、偶氮玉红、苋菜红、赤藓红、罗丹明B、酸性红73、诱惑红、中性红、刚果红、甲基红、曙红、新品红、金光红C、橙G、碱性橙Ⅱ、金胺O、金橙Ⅱ、柠檬黄、日落黄、酸性橙Ⅰ、皂黄、碱性橙21、碱性橙22、孔雀石绿、亮绿、亮蓝、结晶紫、专利蓝、亚甲基蓝、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红G、分散红9、808猩红、柑橘红2及松香酸38种已有或可能的染色掺假物质分别依次进行LC-MS/MS(QTOF)分析,结合Mass Hunter PCDL软件建立数据库,以通过软件自动筛选出可疑染色掺假物质。结果:采用所建立的方法快速筛查验证了红花、西红花、血竭、朱砂、延胡索、黄连、蒲黄、五味子、熟地、制首乌、制黄精、全蝎、松花粉、山茱萸、乳香、没药、沉香、乌梅、海金沙、青黛20种中药材及饮片共200余批,对于各种药材及饮片基本实现通用,有效识别了补充检验方法未收载的染色掺假物质,验证了快速筛查方法的可行性。结论:建立的常见染色掺假物质数据库和分析方法具有快速、灵敏、准确的优点,节省了时间和实验成本。
OBJECTIVE: To establish a rapid screening method for common dyed adulterant substances in Chinese herbal medicines and Chinese herbal medicines based on liquid chromatography-mass spectrometry. METHODS: Poroshell 120 EC-C 18 column (3.0 mm × 100 mm, 2.7 μm) was used to elute gradient acetonitrile and 0.02 mol·L -1 ammonium acetate solution with a mobile phase of 0.4 mL · min -1, the column temperature was 35 ℃ and the detection wavelength was 428, 483, 509 and 608 nm. The electrospray ionization source (ESI) and positive ion mode detection 000. Carmine, azuanyu, amaranth, erythrosine, rhodamine B, acid red 73, temptation red, neutral red, congo red, methyl red, eosin, new magenta, golden red C, orange G , Basic Orange II, Auramine O, Gold Orange II, Tartrazine, Sunset Yellow, Acid Orange I, Soap Yellow, Basic Orange 21, Basic Orange 22, Malachite Green, Brilliant Green, Brilliant Blue, Patent Blue, Methylene Blue, Sudan I, Sudan II, Sudan III, Sudan IV, Sudan G, Disperse Red 9,808 Scarlet, Citrus Red 2, and Rosin Acid 38 Available or Possible Dye Adulterants LC-MS / MS (QTOF) analysis followed by Mass Hunter PCDL software was used to establish a database to automatically screen suspiciously dyed adulterant substances by software. Results: The established method was used to screen and verify the contents of safflower, saffron, blood serum, cinnabar, fumarate, berberine, Puhuang, Schisandra, Rehmannia, Polygonum multiflorum, Polygonatum, Scorpio, Frankincense, myrrh, incense, ebony, sea Sands, indigo 20 kinds of Chinese herbal medicines and pieces of a total of more than 200 batches for a variety of medicinal herbs and Pieces basically common, effective identification of the supplementary test methods are not stained dyed material to verify The feasibility of rapid screening methods. Conclusion: The established database of common staining adulterant substances and analysis methods have the advantages of fast, sensitive and accurate, saving time and experiment cost.