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

CJI (Traditional Chinese Medicine) - - Chinese Journal Of Information On Traditional Chin -

冯良,褚书豪,汪小彩

河南中医药大学第三附属医院药剂科,河南 郑州 450008

摘要: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,5 —m);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。关键词:仙灵骨葆胶囊;淫羊藿苷;川续断皂苷Ⅵ;补骨脂素;异补骨脂素;朝霍定C

DOI:10.3969/j.issn.1005-5304.2017.10.016

中图分类号:R284.1 文献标识码:A 文章编号:1005-5304(2017)10-0068-04

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

CHU Shu-hao, WANG Xiao-cai (Pharmacy Department, Third Affiliated Hospital of Henan University of Chinese Medicine, Zhengzhou 450008, China)

Abstract: 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 —m) 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.

Key words: Xianling Gubao Capsules; icariin; asperosaponin Ⅵ; psoralen; angelicin; epimedin C

仙灵骨葆胶囊是淫羊藿、续断、丹参、知母、补骨脂、地黄6种中药经现代工艺技术制成的胶囊剂,具有滋补肝肾、活血通络、强筋壮骨功效,临床用于骨质疏松和骨质疏松症、骨折、骨关节炎、骨无菌性坏死等病症的治疗[1-3]。目前,仙灵骨葆胶囊的质量主要以淫羊藿苷、补骨脂素、异补骨脂素含量衡 量[4-6],而对其他成分或多种成分同时测定的研究报道甚少。淫羊藿苷、朝霍定C是淫羊藿的主要成分,检测波长 270 nm[7-8];川续断皂苷Ⅵ是续断的主要成分,检测波长 212 nm[9-10];补骨脂素、异补骨脂素是补骨脂的主要成分,检测波长246 nm[11-12]。这 5 种成分检测波长不一致且差异较大,不能采用常规方法检

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