三七原料药材与注射用血栓通(冻干)中皂苷类成分对比分析及转移规律研究

Comparative Analysis and Transfer Research of Saponins in Panax notoginseng and Xueshuantong Injection (Freeze-drying)

  • 摘要: 本研究采用高效液相色谱(HPLC)法和高效液相色谱 串联四极杆飞行时间质谱(HPLC-Q-TOF MS)法研究三七原料药与注射用血栓通(冻干)中的皂苷类成分。通过对比三七原料药材与注射用血栓通(冻干)中的共有峰,以及各皂苷类成分的峰面积比例,探讨由三七原料药材到注射用血栓通(冻干)过程中各皂苷类成分的转化损失。采用Waters XBridge C18色谱柱(4.6 mm×250 mm×5 μm),柱温40 ℃,流速0.35 mL/min,流动相为0.01%甲酸-水(A)-0.01%甲酸-乙腈(B),进行梯度洗脱。其中,HPLC法采用UV检测器,检测波长203 nm;HPLC-Q-TOF MS法在ESI负离子模式下进行数据采集。在该分析条件下,各皂苷类成分分离良好,各色谱峰对称性较高。三七原料药材与注射用血栓通(冻干)中皂苷类成分对比分析结果表明,两者中均含有三七皂苷R1,人参皂苷Rg1、Re、Rg2、Rb1、Rd、F2以及七叶胆苷ⅩⅦ,其峰面积比值分别为2.55、6.88、3.02、9.75、31.30、15.68、15.98、714.34,表明各皂苷类成分由原料药材到最终制剂的转移率存在较大差别,其中转移率最高的成分为三七皂苷R1,而生产过程中损失较大的物质为七叶胆苷ⅩⅦ。

     

    Abstract: The saponins in Panax notoginseng and Xueshuantong injection (freeze-drying) were analyzed using high performance liquid chromatography (HPLC) and HPLC-electrospray ionization-quadrupole-time of flight mass spectrometry (HPLC-Q-TOF MS). Through comparing the number of common peaks and the peak area ratio of saponins in Panax notoginseng and Xueshuantong injection (freeze-drying) to discuss the transformation loss of saponins from Panax notoginseng to Xueshuantong injection (freeze-drying). HPLC method was established to analyze the Xueshuantong injection (freeze-drying), and the analytes were separated on Waters XBridge C18 column (4.6 mm×250 mm×5 μm) at the constant flow rate of 0.35 mL/min. The column temperature was set at 40 ℃. 0.01% FA (A)-0.01% FA-CAN (B) was used as mobile phase for the gradient elution, and the detection wavelength was 203 nm. HPLC-Q-TOF MS was performed in ESI negative ion mode for data acquisition. Under this analytical condition, the saponins in Panax notoginseng were well separated and the chromatographic peaks were highly symmetrical. The comparative analysis of saponins in raw materials of Panax notoginseng and Xueshuantong for injection (freeze-dried) showed that notoginsenoside R1, ginsenosides Rg1, ginsenosides Re, ginsenosides Rg2, ginsenosides Rb1, ginsenosides Rd, ginsenosides F2 and gypenoside ⅩⅦ were detected in Panax notoginseng extract and Xueshuantong for injection (freeze-drying), and the peak area ratios were 2.55, 6.88, 3.02, 9.75, 31.30, 15.68, 15.98, 714.34, respectively. The results showed that the transfer rates of saponins from raw materials to final preparations were significantly different. The highest transfer rate of saponins was notoginsenoside R1, while the most lost substance in the production process was gypenoside ⅩⅦ. The study is helpful to clarify the material migration law of Xueshuantong injection in the production process.

     

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