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目的筛选九节龙中九节龙皂苷Ⅰ的最佳提取工艺,并建立HPLC-ELSD法对九节龙皂苷Ⅰ的测定方法。方法采用L_3(3～4)正交试验,以九节龙皂苷Ⅰ提取率和干浸膏得率为检测指标。HPLC-ELSD色谱条件:Phe-nomenexC_(18)(250mm×4.6mm,5μm);流动相为甲醇-水(75:25);体积流量:1.0mL/min;检测器漂移管温度:73.8℃;载气体积流量:2.0L/min。结果最佳提取工艺为75%乙醇,第1次8倍量提取4h,第2次6倍量提取3h。九节龙皂苷Ⅰ在0.88-4.42μg范围内线性关系良好(r=0.9999);样品平均回收率为100.37%,RSD为1.88%(n=6)。结论建立的正交试验优选九节龙的提取方法可行,采用的HPLC-ELSD法测定九节龙皂苷Ⅰ的方法可用于九节龙皂苷Ⅰ的质量控制。
Objective To screen the best extracting technology of Nine-element Diosgenin I from Jiujielongzhong, and establish a HPLC-ELSD method for the determination of Nine Diosgenin I. Methods L3 (3～4) orthogonal test was used to detect the extraction rate of N. japonicum saponin I and dry extract. HPLC-ELSD chromatographic conditions: Phe-nomenexC_(18) (250mm×4.6mm, 5μm); mobile phase methanol-water (75:25); volumetric flow rate: 1.0mL/min; detector drift tube temperature: 73.8°C; Carrier gas volume flow: 2.0L/min. Results The best extraction process was 75% ethanol, the first 8-fold extraction 4h, the second 6-fold extraction 3h. There was a good linearity in the range of 0.88-4.42 μg (r=0.9999) for N. japonicum I. The average recovery of the sample was 100.37%, and the RSD was 1.88% (n=6). [Conclusion] Orthogonal test established by the established method is suitable for the extraction of N. japonicum. HPLC-ELSD method for the determination of N. japonicum I can be used for the quality control of N. japonicum I.