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目的利用HPLC–电雾式检测器(charged aerosol detector,CAD)联用技术建立知母中知母皂苷BⅡ和菝葜皂苷元的测定方法,并比较知母盐制前后两种成分的变化。方法知母皂苷BⅡ以乙腈–水(25∶75)为流动相,进样量为10μL;菝葜皂苷元以甲醇–水(95∶5)为流动相,进样量为20μL;其他色谱条件均采用Thermo C18柱(250 mm×4.6 mm,5μm),体积流量为1 mL/min,柱温为30℃;Corona参数:氮气压力为241.3 kPa,Filter:High,Range:200 pA。结果知母皂苷BⅡ在0.305~4.880μg线性关系良好,r=0.999 4,平均回收率为99.1%,RSD值为1.2%;菝葜皂苷元在0.490~7.840μg线性关系良好,r=0.999 1,平均回收率为98.0%,RSD值为1.3%。知母中知母皂苷BⅡ为3.16%~5.92%,盐制后为4.15%~7.20%;知母中菝葜皂苷元为0.42%~1.39%,盐制后为0.52%~1.54%。结论 CAD检测器具有较为平稳的基线和较高的灵敏度,更加适用于知母皂苷类及含有较弱或无紫外吸收成分的测定,知母盐制后知母皂苷BⅡ和菝葜皂苷元的量均有所升高。
OBJECTIVE To establish a method for the determination of tartaric saponins BII and Smilagenin in Rhizoma Anemarcelis using HPLC-charged aerosol detector (CAD), and to compare the changes of the two components before and after Rhizoma anemarrhena. Methods The timosaponin B Ⅱ with acetonitrile-water (25:75) as the mobile phase, the injection volume of 10μL; Saponin with methanol - water (95: 5) as the mobile phase injection volume of 20μL; other chromatographic conditions Thermo C18 columns (250 mm × 4.6 mm, 5 μm) were used. The volume flow rate was 1 mL / min and the column temperature was 30 ℃. The Corona parameters were: nitrogen pressure 241.3 kPa, Filter: High, Range 200 pA. Results The results showed that there was a good linearity between 0.305 and 4.880 μg of timosaponin B (r = 0.999 4), the average recovery was 99.1% and the RSD was 1.2%. The linear correlation of sapogenin between 0.490 and 7.840 μg was good (r = 0.999 1) The average recovery was 98.0% with a RSD of 1.3%. Anemarrhena asphodeloides BII was 3.16% ~ 5.92%, salt 4.15% ~ 7.20%; Anemarrhena astigmatis 0.42% ~ 1.39%, 0.52% ~ 1.54% after salt. Conclusion The CAD detector has a relatively stable baseline and high sensitivity, more suitable for the determination of timosaponins and containing weak or no UV absorption components, the amount of timosaponin B Ⅱ and smilagenin All have risen.