超高效液相色谱-串联质谱法同时测定地锦草中8种成分的含量

Simultaneous Determination of Eight Components in Euphorbiae Humifusae Herba by UPLC-MS/MS

目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)用于同时测定地锦草中2种有机酸类和6种黄酮类成分的含量。方法:采用Hypersil GOLD C18(150 mm×3.0 mm,3μm),流动相为0.3%甲酸溶液(A)-乙腈(B),梯度洗脱,流速为0.3 mL/min,柱温为40℃,进样量为2μL;质谱采用ESI源,负离子模式监测,喷雾电压为-3000 V,离子化温度为500℃,多反应监测模式(MRM)用于定量分析。结果:所测定地锦草中的8个成分在测定浓度范围内峰面积和浓度均呈良好的线性关系(r≥0.9910),加样回收率在96.1%~99.9%,精密度、重复性和稳定性良好并符合方法学考察要求。结论:该方法简便、快速、准确、可靠,可用于地锦草中8种成分的含量测定。

To develop a UPLC-MS/MSmethod for simultaneous determination of six flavonoids and two organic acids in Euphorbiae Humifusae Herba.Methods:The analysis was performed on a Hypersil GOLD C18 column(150 mm×3.0 mm,3μm)at 40°C.The mobile phase was 0.3%formic acid solution(A)-hexanenitrile(B)in a gradient elution,which was delivered at a flow rate of 0.3 mL/min.The injection volume was 2μL.For the MS/MS analysis,the ESI source was operated in the negative-ion mode and the ions were monitored in multiple reaction monitoring(MRM)mode.The ionization temperature was 500°C,and the spray voltage was controlled at-3000 V.Result:Calibration curves showed good linearity for all 8 compounds in the settingconcentration(r≥0.9910).The recovery rate was 96.1%~99.9%.The precision,repeatability,stability were all conformed to the validated requirements of methodology.Conclusion:The method simple and convenient,quick,celerity,precise and reliable,can be used for determination of above 8 compounds in Euphorbiae Humifusae Herba.