UPLC-MS/MS法同时测定泽泻药材中16个成分

目的：建立超高效液相色谱串联三重四极杆质谱法（UPLC-MS/MS）同时测定泽泻药材中16个主要成分（16-氧代泽泻醇A、16-氧代-24-乙酰泽泻醇A、泽泻醇C、泽泻醇F、23-乙酰泽泻醇C、11-去氧泽泻醇C、泽泻醇L、24-乙酰泽泻醇F、泽泻醇A、24-乙酰泽泻醇A、23-乙酰泽泻醇L、泽泻醇G、泽泻醇B、23-乙酰泽泻醇B、11-去氧泽泻醇B和11-去氧-23-乙酰泽泻醇B）的含量。方法：采用UPLC-MS/MS法，正离子多反应监测（MRM）模式进行含量测定。色谱条件：采用Cortecs C₁₈色谱柱（2.1 mm×100 mm，1.6 μm），流动相为乙腈（A）-0.1%甲酸水溶液（B），梯度洗脱，流速0.25 mL·min^-1，柱温40℃。结果：在所设定的色谱条件下，10 min内定量分析泽泻药材中上述16个主要成分，在考察的浓度范围内呈良好的线性关系（r>0.998 1），回收率和RSD分别在96.0%~104.3%和2.4%~4.4%范围内，精密度、重复性、稳定性考察也符合分析要求。24批样品中上述16个成分含量测定结果依次为0.009~0.668 mg·g^-1、0.001~0.009 mg·g^-1、0.021~0.229 mg·g^-1、0.004~0.094 mg·g^-1、0.100~0.342 mg·g^-1、0.016~0.048 mg·g^-1、0.009~0.044 mg·g^-1、0.002~0.090 mg·g^-1、0.023~1.133 mg·g^-1、0.012~0.596 mg·g^-1、0.003~0.023 mg·g^-1、0~0.018 mg·g^-1、0.489~2.313 mg·g^-1、0.833~2.138 mg·g^-1、0.043~0.341 mg·g^-1、0.037~0.186 mg·g^-1。结论：本研究所建立的同时测定泽泻药材中16个成分的UPLC-MS/MS定量分析方法简便、快捷、准确，为泽泻药材质量控制提供新的技术手段。

Objective:To establish a UPLC-MS/MS method for simultaneous determination of 16 major components(16-oxo-alisol A,16-oxo-alisol A 24-actetate,alisol C,alisol F,alisol C 23-acetate,11-deoxy-alisol C,alisol L,alisol F 24-actetate,alisol A,alisol A 24-acetate,alisol L 23-acetate,alisol G,alisol B,alisol B 23-acetate,11-deoxy-alisol B and 11-deoxy-alisol B 23-acetate)in Alismatis Rhizoma. Methods:The UPLC-MS/MS assay was performed on a Waters Cortecs C₁₈(2.1 mm×100 mm,1.6 μm)column with acetonitrile-water(containing 0.1% formic acid)as mobile phase by gradient elution at a flow rate of 0.25 mL·min^-1. The column temperature was set at 40℃. MS detection was performed with multiple reaction monitoring(MRM)mode using positive electrospray ionization. Results:Under the optimized chromatographic conditions,good separation for 16 target compounds was obtained within 10 min. Satisfactory linearity was achieved with wide linear range and fine determination coefficient(r>0.998 1), the recoveries were ranged from 96.0% to 104.3% with the RSDs within 2.4%-4.4%. Contents of the analytes in the samples were 0.009-0.668 mg·g^-1,0.001-0.009 mg·g^-1,0.021-0.229 mg·g^-1,0.004-0.094 mg·g^-1,0.100- 0.342 mg·g^-1,0.016-0.048 mg·g^-1,0.009-0.044 mg·g^-1,0.002-0.090 mg·g^-1,0.023-1.133 mg·g^-1,0.012-0.596 mg·g^-1,0.003-0.023 mg·g^-1,0-0.018 mg·g^-1,0.489-2.313 mg·g^-1,0.833-2.138 mg·g^-1,0.043-0.341 mg·g^-1 and 0.037-0.186 mg·g^-1,respectively. Conclusion:The proposed UPLC-MS/MS method for simultaneous determination of 16 major components in Alismatis Rhizoma was simple,fast and accurate,which offered a new approach for quality control of Alismatis Rhizoma.