三七三醇皂苷及制剂的LC-MS指纹图谱研究.doc

Study on Fingerprints of PTS and its Preparation by LC-MS LENG Jing1，YANG Hua-rong2， (1. College of Pharmacy?，Chengdu University of Tranditional Chinese Medicine，Chengdu 611137，China.Chengdu Huashen pharmaceutical factory of Co. Ltd，Chengdu 610225，China)ABSTRACT: OBJECTIVE Investigating the chromatographic fingerprints of PTS and its preparation by LC-MS to reach the technical requirements of Quality Control of EU Drug Registeration . METHODS Several batches of PTS and its preparation were determined by HPLC. The analysis was carried out on Waters Symetry Shield C18 column (4.6 mm×250 mm，Ф 5 μm) gradient elution of acetonitrile-water. The detection wavelength was at 203 nm，the flow rate was 1.0 mgmL-1. The similarity was analyzed by similarity evaluation system for chromatographic fingerprint of TCM (Version 2004 A). The main components of the Fingerprints of PTS was confirmed by reference substance and LC-MS. RESULTS The components of PTS can be separated well using this method. This method is precise, reproducible and stability. CONCLUSION This method can fully demonstrate the components of PTS and its preparation and can be applied in the quality control of PTS and its preparation. KEY WORDS: PTS; panax notoginseng tongshu intestinal solution micro-pill capsule; fingerprints; LC-MS CLC number：R284.1 Document code：A Article ID：mg·mL-1，对多批PTS及其制剂进行HPLC测定和方法学考察，采用中药色谱指纹图谱相似度评价系统 2004 A版对测定结果进行相似度评价。采用对照品法和LC-MS法对原料药指纹图谱中的主要色谱峰进行了成分确证。结果 所建立的LC-MS指纹图谱条件能分离PTS的各组分，具有较好的精密度、重复性和稳定性。结论 采用LC-MS指纹图谱能充分展示PTS及其制剂的物质组成，控制产品质量。 关键词: 三七三醇皂苷；三七通舒肠溶微丸胶囊；指纹图谱；LC-MS 中图分类号:R284.1 文献标识码:A 文章编号: 三七三醇皂苷（protoparaxotriol saponins，PTSPTS及制剂的质量控制依据。 1 仪器与试药 Agilent 1100高效液相色谱仪，VWD-DAD检测器，Agilent 1100色谱工作站，四元泵在线脱气系统（美国安捷伦科技有限公司）；型质谱仪； Mettler AE240电子分析天平（十万分之一，德国Mettler公司）PTS共15批，三七通舒肠溶微丸胶囊共10批，均为成都华神集团有限责任公司制药厂生产。三七皂苷R1(批号110745－200415)、人参皂苷Rg1(批号110703－200425)、人参皂苷Re(批号110754－200421)、人参皂苷Rb1(批号11704—200318)、人参皂苷Rf（批号111719－200502）对照品购自中国药品生物制品检定所。 乙腈(色谱纯，美国fisher公司出品)；超纯水。 2