LC-MS/MS同时测定四逆汤中11个有效成分

Simultaneous determination of eleven components in Sini Decoction by LCMS /MS

目的建立LC-MS/MS法同时测定四逆汤（生附子、干姜和炙甘草）中11个有效成分（乌头碱、新乌头碱、次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱、乌头原碱、次乌头原碱、甘草苷、甘草酸和6-姜酚）的量。方法四逆汤水提液在Agilent Eclipse XDB-C18色谱柱（4.6 mm×150 mm,5μm）上分离,流动相为乙腈-水（4 mmol/L乙酸铵和0.08%甲酸）,梯度洗脱;地西泮乙腈溶液作为内标。MS采用电喷雾离子源,多反应监测方式进行正离子扫描。结果 11种成分在测定浓度范围内均具有良好的线性关系,平均回收率为95.4%～103%。结论本研究建立的LC-MS/MS定量分析方法可靠准确、灵敏高,可用于四逆汤的质量控制方法。

AIM To establish a liquid chromatography-tandem mass spectrometry（ LC-MS /MS） method for simultaneously determining eleven constituents（ aconitine, mesaconitine, hypaconitine, benzoylaconine,benzoylmesaconine,benzoylhypaconine,aconine,hypaconine,liquirtin,glycyrrhizic acid,glycyrrhetinic acid and6-gingerol） in Sini Decoction（ Aconitum carmichaelii Debx, Zingiber officinale Rosc, Glycyrrhiza uralensis Fisch.）. METHODS The separation of Sini Decoction extract was performed on Agilent Eclipse XDB-C18column（ 4. 6 mm × 150 mm,5 μm） with acetonitrile-water（ 4 mmol /L ammonium acetate and 0. 08% formic acid）in gradient elution manner. Diazepan-acetonitrile was adopted as the internal standard. The mass spectrometer was equipped using electrospray ionization source in positive and multiple-reaction monitoring modes. RESULTS All the constituents showed the good linear relationship with their recoveries of 95. 4% ～ 103%. CONCLUSION The method is accurate,reliable and sensitive and can be used for quality control of Sini Decoction.