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HPLC法同时测定金蝉止痒胶囊中盐酸小檗碱、黄芩苷和蛇床子素的含量
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篇名: HPLC法同时测定金蝉止痒胶囊中盐酸小檗碱、黄芩苷和蛇床子素的含量
TITLE:
摘要: 目的:建立同时测定金蝉止痒胶囊中盐酸小檗碱、黄芩苷和蛇床子素含量的方法。方法:采用高效液相色谱法。色谱柱为Hypersil BDS C18,流动相为甲醇-乙腈-0.1%磷酸溶液-三乙胺(50 ∶ 30 ∶ 19 ∶ 1,V/V/V/V),流速为1.0 mL/min,检测波长为265 nm(盐酸小檗碱)、280 nm(黄芩苷)、322 nm(蛇床子素),柱温为30 ℃,进样量为10 μL。结果:盐酸小檗碱、黄芩苷和蛇床子素检测进样量线性范围分别为80~800 ng(r=0.999 8)、60~600 ng(r=0.999 9)、60~600 ng(r=0.999 6);定量限分别为80、60、60 ng,检测限分别为24、20、20 ng;中间精密度、稳定性、重复性试验的RSD均小于2.0%;加样回收率分别为97.4%~98.3%(RSD=0.33%,n=6)、98.4%~99.6%(RSD=0.42%,n=6)、96.9%~99.0%(RSD=0.92%,n=6);耐用性试验的RSD均小于1.2%。结论:该方法操作简便、准确,精密度、稳定性、重复性、耐用性好,可用于金蝉止痒胶囊中盐酸小檗碱、黄芩苷和蛇床子素含量的同时测定。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of the content of berberine hydrochloride,baicalin and osthole in Jinchan zhiyang capsules. METHODS: HPLC method was adopted. The determination was performed in Hypersil BDS C18 column with mobile phase consisted of methanol-acetonitrile-0.1% phosphoric acid-three triethylamine (50 ∶ 30 ∶ 19 ∶ 1,V/V/V/V) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 265 nm (berberine hydrochloride), 280 nm (baicalin) and 322 nm (osthole). The column temperature was set at 30 ℃, and sample size was 10 μL. RESULTS: The linear range of berberine hydrochloride, baicalin and osthole were 80-800 ng(r=0.999 8), 60-600 ng(r=0.999 9), 60-600 ng(r=0.999 6), respectively. RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The limits of quantitation were 80,60,60 ng, respectively, and the limits of detection were 24,20,20 ng, respectively. The recovery rates were 97.4%-98.3%(RSD=0.33%,n=6), 98.4%-99.6%(RSD=0.42%,n=6) and 96.9%-99.0%(RSD=0.92%,n=6), respectively. RSDs of durability tests were all lower than 1.2%. CONCLUSIONS: The method is simple, accurate, precise, stable, reproducible and durable. It can be used for simultaneous determination of berberine hydrochloride,baicalin and osthole in Jinchan zhiyang capsules.
期刊: 2018年第29卷第12期
编辑: 黄传俊,梅勇,杨莉,罗磊,曾博程,龙涛,袁开超,谯志文,陈小雪
AUTHORS: HUANG Chuanjun,MEI Yong,YANG Li,LUO Lei,ZENG Bocheng,LONG Tao,YUAN Kaichao,QIAO Zhiwen,CHEN Xiaoxue
关键字: 金蝉止痒胶囊;高效液相色谱法;盐酸小檗碱;黄芩苷;蛇床子素;含量测定
KEYWORDS: Jinchan zhiyang capsules; HPLC; Berberine hydrochloride; Baicalin; Osthole; Content determination
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