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(4.6mm×150mm,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14min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 develop a method for the determination of scopoletin ( 1 ) , psoralen ( 2 ) , isoimpinnellio ( 3 ) , oxypeucedanin ( 4 ), imperatorin ( 5 ), enidimine ( 6 ) and isoimperatorin ( 7 ) in Qingxuan tablets by HPLC-MS. METHODS The samples were separated on a Sapphire Ci8 column (4. 6 mm×150mm, 5 μm ) by gradient elution using methanol and 0. 1% aqueous formic acid as the mobile phase at a flow rate of 800 μL·min^-1. The column temperature was 30℃. Multiple-reaction monitoring (MRM) scanning was employed for quantification with switching electrospray ion source polarity in positive modes. RESULTS The complete separation was obtained within 14 rain for the seven compounds. The regression equations showed linear relationships between the peak area and content of each compound. The average recoveries (n = 3 ) of the compounds listed above were 99. 05% , 99. 57% , 101.8% , 101.2% , 100. 9% , 102. 1% and 98.74%, and the RSDs were 1.08% , 1.16% , 1.77% , 1.24% , 1.37%, 1.02% and 0. 97% , respectively. CONCLUSION The method is simple, accurate and highly reproducible, and can be used for the determination of seven coumarins in Qingxuan tablets.