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 mL/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 other 4 kinds of active ingredients in Xianling Gubao Capsules by three wavelength switching method. Methods An Waters Atlantis T3 C18 column (4.6 mm × 250 mm, 5 μm) was used with the mixture of acetonitrile-0.05％ formic acid solution as the mobile phase in gradient elution (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). Detection wavelength was as follow: 0–30 min, 212 nm; 30–42 min, 246 nm; 42–60 min, 270 nm. The flow rate was 1.0 mL/min. The column temperature was 30 ℃. Results The calibration curves of asperosaponin Ⅵ, psoralen, angelicin, epimedin C, and icariin were in good linearity among the ranges of 101.6–3048 ng, 8.7–261 ng, 7.9–237 ng, 117.2–3516 ng, 78–2340 ng, respectively. In the instrument precision test, stability test, repeatability test, the RSD was less than 3％. The average recoveries were 99.83％, 100.35％, 100.59％, 100.60％, 99.72％, respectively, and all the RSD were less than 3％. Conclusion The method is sensitive, accurate, and separation effect is good, which can provide a basis for quality evaluation standard of Xianling Gubao Capsules.
展开▼
