QTRAP-UPLC-MS/MS同时测定玄参不同产地及商品药材中10种核苷类成分的含量

Simultaneous QTRAP-UPLC-MS/MS quantitation of 10 kinds of nucleosides and nucleobases in Scrophulariae Radix from different areas and commercial herbs

目的：建立超高效液相色谱-三重四级杆/线性离子阱质谱（QTRAP-UPLC-MS/MS）同时测定玄参不同产地及商品药材中10种核苷类成分的方法。方法：采用Waters Atlantis T3C18色谱柱（2.1 mm×150mm,3μm）,以甲醇-5 mmol·L^-1醋酸铵（含0.1%冰醋酸）为流动相,0.4 m L·min^-1梯度洗脱,正离子多反应监测（MRM）模式测定。结果：10种核苷类成分的浓度与峰面积的线性关系良好（r2〉0.994 7）;平均加样回收率为94.72%~98.18%。玄参核苷类成分中,以鸟苷、尿苷、腺苷、尿嘧啶含量较高;不同产地及商品药材中核苷类成分含量有所差异。结论：该方法准确、可靠,为玄参药材内在质量的综合评价提供新的方法参考。

Objective： To establish a QTRAP-UPLC-MS /MS method for simultaneous determination of 10 kinds of nucleosides and nucleobases in Scrophulariae Radix from different habitats and commercial herbs. Methods： The analysis was carried out on an Waters Atlantis T3C18column（ 2. 1 mm × 150 mm,3 μm） which was eluted by a mobile phase of methanol-5 mmol·L^-1ammonium acetate（ 0. 1% acetic acid） at a flow rate of 0. 4 m L·min^-1. The target compounds were analyzed by the positive ion multiple reaction monitoring（ MRM） mode. Results： Ten kinds of nucleosides and nucleobases showed a good linearity（ r2〉 0. 994 7） in the range of the tested concentrations. The average recoveries of the ten components were between 94. 72% and 98. 18%. The contents of guanosine,uridine,adenosine and uracil were higher in Scrophulariae Radix. The contents were different from different habitats and commercial herbs. Conclusion： The established method is accurate and reliable,and provides a scientific basis for the quality evaluation of Scrophulariae Radix.