三波长切换法同时测定仙灵骨葆胶囊中淫羊藿苷等5种活性成分含量

Simultaneous Determination of Epimedium Glycoside and Other 4 Kinds of Active Ingredients in Xianling Gubao Capsules by Three Wavelength Switching Method

目的建立三波长切换法同时测定仙灵骨葆胶囊中淫羊藿苷等5种活性成分含量的方法。方法采用Waters Atlantis T3 C18色谱柱(250mm×4.6mm,5μm);以乙腈(A)-0.05%甲酸溶液(B)为流动相进行梯度洗脱(0~5 min,12%~20%A;5~15 min,20%~55%A;15~35 min,55%A;35~55 min,55%~76%A;55.1 min,12%A;55.1~60 min,12%A);检测波长:0~30 min为212 nm,>30~42 min为246 nm,>42~60 min为270 nm;柱温:30℃;流速:1.0 m L/min。结果川续断皂苷Ⅵ、补骨脂素、异补骨脂素、朝霍定C、淫羊藿苷分别在101.6~3048 ng、8.7~261 ng、7.9~237 ng、117.2~3516 ng、78~2340 ng范围内线性关系良好;仪器精密度、稳定性、重复性试验中RSD均小于3%;平均回收率分别为99.83%、100.35%、100.59%、100.60%、99.72%,RSD均小于3%。结论该测定方法准确度、灵敏度高,分离效果理想,可为完善仙灵骨葆胶囊质量评价标准提供依据。

Objective To establish the method for simultaneous determination of epimedium glycoside and other4kinds of active ingredients in Xianling Gubao Capsules by three wavelength switching method.Methods An Waters Atlantis T3C18column(4.6mm×250mm,5μm)was used with the mixture of acetonitrile-0.05%formic acid solution as the mobile phase in gradient elution(0-5min,12%-20%A;5-15min,20%-55%A;15-35min,55%A;35-55min,55%-76%A;55.1min,12%A;55.1-60min,12%A).Detection wavelength was as follow:0-30min,212nm;30-42min,246nm;42-60min,270nm.The flow rate was1.0mL/min.The column temperature was30℃.Results The calibration curves of asperosaponinⅥ,psoralen,angelicin,epimedin C,and icariin were in good linearity among the ranges of101.6-3048ng,8.7-261ng,7.9-237ng,117.2-3516ng,78-2340ng,respectively.In the instrument precision test,stability test,repeatability test,the RSD was less than3%.The average recoveries were99.83%,100.35%,100.59%,100.60%,99.72%,respectively,and all the RSD were less than3%.Conclusion The method is sensitive,accurate,and separation effect is good,which can provide a basis for quality evaluation standard of Xianling Gubao Capsules.