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建立了同时测定中成药都梁滴丸中5-甲氧基补骨脂素、8-甲氧基补骨脂素和欧前胡素的超高效液相-串联质谱检测方法。都梁滴丸以甲醇超声提取45 min,提取液稀释后经Waters Oasis HLB固相萃取小柱净化,采用WatersACQUITY UPLC BEHC18(50 mm×2.1 mm,1.7μm)色谱柱,以乙腈(A)和水(B)为流动相进行梯度洗脱。采用电喷雾电离正离子模式,多反应监测模式检测,以保留时间和离子比定性,外标法定量。方法的定量限8-甲氧基补骨脂素和5-甲氧基补骨脂素均为0.3 mg/kg;欧前胡素为0.75 mg/kg。3种化合物在25~500μg/L范围内均呈线性,相关系数r>0.99。在高,中,低三种添加水平的平均回收率为82.0%~107.4%日内精密度(RSD%)为1.1%~12%。
A method for the simultaneous determination of 5-methoxypsoralen, 8-methoxypsoralen and imperatorin in Chinese medicine Doudie pills was established. Both of them were ultrasonically extracted with methanol for 45 min. The extracts were diluted and purified by a Waters Oasis HLB solid phase extraction cartridge. The column was eluted with a Waters ACQUITY UPLC BEHC18 (50 mm × 2.1 mm, 1.7 μm) column with acetonitrile (A) and water (B) gradient elution of the mobile phase. Using electrospray ionization positive ion mode, multi-reaction monitoring mode detection, retention time and ion ratio qualitative, external standard method. The limits of quantitation of the method were 0.3 mg / kg for 8-methoxy psoralen and 5-methoxy psoralen, and 0.75 mg / kg for imperatorin. Three compounds were linear in the range of 25 ~ 500μg / L, the correlation coefficient r> 0.99. The average recoveries of high, medium and low levels were 82.0% -107.4%. Intraday precision (RSD%) ranged from 1.1% to 12%.