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目的建立HPLC-MS测定清眩片中东莨菪亭(1),补骨脂素(2),异茴芹内酯(3),氧化前胡内酯(4),欧前胡素(5),蛇床明素(6)和异欧前胡素(7)含量的方法。方法采用Sapphire C18柱(4.6 mm×150 mm,5μm);柱温30℃;甲醇-0.1%甲酸水溶液(72∶28)为流动相,以800μL.min-1等度洗脱;质谱条件:采用电喷雾离子源进行正离子模式检测,多反应监测模式(MRM)用于定量测定。结果在14 min内清眩片中7个香豆素类有效成分完全分离;峰面积与浓度呈良好的线性关系;加样回收率(n=3)分别为99.05%,99.57%,101.8%,101.2%,100.9%,102.1%和98.74%。RSD值分别为1.08%,1.16%,1.77%,1.24%,1.37%,1.02%和0.97%。结论该方法简便,准确,重现性好,专属性高,可用于清眩片的质量控制。
OBJECTIVE To establish a HPLC-MS method for the determination of scopolamine (1), psoralen (2), anisoflavanide (3), preanolactone (4), imperatorin (5) Cinnabarin (6) and isoimperatorin (7) content of the method. The method was performed on a Sapphire C18 column (4.6 mm × 150 mm, 5 μm) with a column temperature of 30 ° C and methanol-0.1% formic acid aqueous solution (72:28) as eluent to elute with 800 μL · min- Electrospray ionization positive ion mode detection, multiple reaction monitoring mode (MRM) for quantitative determination. Results The results showed that the active constituents of seven coumarins were completely separated in Qing dynasty tablets within 14 min. The peak area and concentration showed a good linear relationship. The recoveries (n = 3) were 99.05%, 99.57% and 101.8%, respectively, 101.2%, 100.9%, 102.1% and 98.74%. RSD values were 1.08%, 1.16%, 1.77%, 1.24%, 1.37%, 1.02% and 0.97%, respectively. Conclusion The method is simple, accurate, reproducible and highly specific and can be used for the quality control of Qinghuang tablets.