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目的建立超高效液相色谱-三重四级杆线性离子肼复合质谱(QTRAP UPLC-MS/MS)同时测定太子参中13种核苷类成分含量的方法,分析不同生长期太子参中核苷类成分积累的动态变化。方法采用Waters Atlantis T3色谱柱(2.1 mm×150 mm,3μm),以5 mmol·m L-1醋酸铵(B相)-甲醇(A相)为流动相,0.4 m L·min-1梯度洗脱:0~4.5 min,3%~4%A;4.5~8 min,4%~18%A;8~10 min,18%A;10~10.1 min,18%~3%A;10.1~13 min,3%A。正离子多反应监测(MRM)模式测定。结果 13种核苷类成分的浓度与峰面积的线性关系良好(r>0.991 0);加样回收率为95.52%~105.07%。太子参核苷类成分中,以胞苷、尿苷、肌苷、鸟苷、胸苷含量较高;不同生长期太子参核苷类成分含量有所差异,6月中旬含量相对较高。结论该方法简便、灵敏,结果准确、可靠,为探索太子参药材的品质形成机制及确定药材适宜采收期提供依据。
Objective To establish a method for simultaneous determination of 13 nucleoside components in Radix Pseudostellariae by ultra performance liquid chromatography-triple quadrupole linear-ion-hydrazine mass spectrometry (QTRAP UPLC-MS / MS) Accumulation of dynamic changes. Methods A Waters Atlantis T3 column (2.1 mm × 150 mm, 3 μm) was used with a mobile phase of 5 mmol·L -1 ammonium acetate (phase B) -methanol (A phase) and a gradient of 0.4 m L · min -1 Off: 0-4.5 min, 3% -4% A; 4.5-8 min, 4-18% A; 8-10 min, 18% A; 10-10.1 min, 18-3% A; min, 3% A. Positive ion multiple reaction monitoring (MRM) mode determination. Results The linear relationship between the concentration of 13 nucleosides and the peak area was good (r> 0.991 0). The recoveries of samples ranged from 95.52% to 105.07%. Pseudostellaria heterophylla glycosides composition, cytidine, uridine, inosine, guanosine, thymidine content higher; different growth stages of Radix Pseudostellaria heterophylla glycosides composition content is somewhat different, mid-June content is relatively high. Conclusion The method is simple, sensitive, accurate and reliable, and provides the basis for exploring the quality forming mechanism of Pseudostellaria heterophylla and determining the proper harvesting period of medicinal materials.