阴离子交换树脂纯化三七总皂苷的液质联用分析

对阴离子交换树脂纯化的三七总皂苷(PNS)进行定性和定量研究,采用液质联用技术结合皂苷标准品对纯化后的三七总皂苷中主要单体皂苷类成分进行指认,确定化学物质基础;并通过三重四级杆多反应检测模式,对这些单体皂苷进行定量分析,确定各皂苷所占比例及总皂苷的纯度。阴离子交换树脂纯化的三七总皂苷中主要含有11种皂苷:人参皂苷Rg1[(195.6±3.3)mg·g~(-1)]、人参皂苷Rg2[(58.1±1.1)mg·g~(-1)]、人参皂苷Re[(102.8±3.1)mg·g~(-1)]、人参皂苷Rb1[(105.4±2.2)mg·g~(-1)]、人参皂苷Rd[(85.8±1.1)mg·g~(-1)]、人参皂苷Rh1[(65.7±1.4)mg·g~(-1)]、20-O-Glucosylginsenoside-Rf[(28.0±1.3)mg·g~(-1)]、人参皂苷F1[(28.1±0.6)mg·g~(-1)]、人参皂苷F2[(31.3±0.9)mg·g~(-1)],三七皂苷R1[(118.2±2.7)mg·g~(-1)]和三七皂苷R2[(62.6±0.9)mg·g~(-1)],总皂苷纯度约为88.16%;并且通过质荷比和色谱保留行为推测含有三七皂苷K。利用阴离子交换树脂纯化的三七总皂苷成分明确、纯度较高,可以作为三七总皂苷药物和健康产品开发的原料使用。

HPLC-MS analysis on Panax notoginseng saponins purified by negative ion exchange resin

Objective: To conduct qualitative and quantitative analysis on PNS after purified by negative ion exchange resin. Methods: LC-MS technology and saponin standards comparison were employed to identify major saponins in the purified PNS to understand its chemical basis. Then individual saponin was quantified via MRM mode of HPLC-QqQ-MS to calculate the ratio of each saponin and the purity of PNS. Results: There were generally 11 saponins in the PNS purified by negative ion exchange resin: ginsenoside Rg1(195.6±3.3 mg.g-1), ginsenoside Rg2(58.1±1.1 mg.g-1), ginsenoside Re(102.8±3.1 mg.g-1), ginsenoside Rb1(105.4±2.2 mg.g-1), ginsenoside Rd(85.8±1.1 mg.g-1), ginsenoside Rh1(65.7±1.4mg.g-1), 20-O-Glucosylginsenoside-Rf(28.0±1.3 mg.g-1), ginsenoside F1(28.1±0.6 mg.g-1), ginsenoside F2(31.3±0.9 mg.g-1), notoginsenoside R1(118.2±2.7 mg.g-1) and notoginsenoside R2(62.6±0.9 mg.g-1). The purity of PNS was calculated to approximately 88.16%. In addition, one saponin was tentatively identified as notoginsenoside K according to its m/z value and chromatographic behavior. Conclusions: The constituents of PNS purified by negative ion exchange resin were clarified and its purity was proved to be qualified as raw materials for the development of PNS drugs and health products.