摘要
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 QTRAP UPLC-MS/MS method for simultaneous determination of thirteen nucleosides and nucleobases in Pseudostellariae Radix, and analyze their dynamic changes at different periods. METHODS The separation was cartied out on a Waters Atlantis T3 column （2. 1 mm x 150 mm ,3 μm）eluted by a mobile phase of 5 mmol mL-1 of ammonium acetate （B）-methanol（A） at a flow rate of 0. 4 mL min-1 The elntion program is as follows. 0 -4. 5 min ,3% -4% A ;4. 5 -8 min ,4% - 18% A;8 -10 min,18%A;10- 10. 1 rain,18% -3% A;10. 1 -13 min,3% A. The target compounds were analyzed by the positive ion muhiple reaction monitoring （MRM） mode. RESULTS The calibration curves of the 13 nucleosides and nucleobases showed good linearity （ r 〉 0. 991 0） in the ranges of the tested concentrations, and the average recoveries were between 96.46% - 105.07%. The contents of cytidine, uridine, inosine, guanosine, and thymidine in Pseudosteltariae Radix harvested at different periods showed some differences, and the contents were higher in mid-June. CONCLUSION The method is simple, sensitive, accurate and credi- ble, and provides the basis for exploring the quality forming mechanism of Pseudostellariae Radix medicinal materials and the suitable harvest time.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2015年第1期75-79,共5页
Chinese Pharmaceutical Journal
基金
国家自然科学基金资助项目(81274016)
国家科技支撑计划项目(2011BAI13B04)
江苏高校优势学科建设工程资助项目(ysxk-2014)
