HPLC切换波长法同时测定健脾止泻宁颗粒中盐酸小檗碱和黄芩苷的含量
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篇名: HPLC切换波长法同时测定健脾止泻宁颗粒中盐酸小檗碱和黄芩苷的含量
TITLE:
摘要: 目的:建立同时测定健脾止泻宁颗粒中盐酸小檗碱和黄芩苷含量的方法。方法:采用高效液相色谱切换波长法。色谱柱为Hypersil BDS C18,流动相为甲醇-0.45%磷酸溶液-三乙胺(50 ∶ 49 ∶ 1,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),柱温为30 ℃,进样量为10 μL。结果:盐酸小檗碱和黄芩苷检测进样量线性范围分别为60.3~312.8 ng(r=0.999 7)、81.5~368.9 ng(r=0.999 9);定量限分别为0.666 8、0.774 0 ng,检测限分别为0.222 6、0.258 0 ng;中间精密度、稳定性、重复性试验的RSD均小于1.0%;加样回收率分别为96.48%~99.30%(RSD=1.06%,n=6)、95.20%~99.39%(RSD=1.66%,n=6);耐用性试验的RSD均小于2.0%。结论:该方法操作简便,精密度、稳定性、重复性、准确度、耐用性均较好,可用于健脾止泻宁颗粒中盐酸小檗碱和黄芩苷含量的同时测定。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of berberine hydrochloride and baicalin in Jianpi zhixiening granules. METHODS: HPLC switching walvelength method was adopted. The determination was performed on Hypersil BDS C18 column with mobile phase consisted of methanol-0.45% phosphoric acid solution-triethylamine (50 ∶ 49 ∶ 1,V/V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 265 nm (berberine hydrochloride) and 280 nm (baicalin). The column temperature was set at 30 ℃, and sample size was 10 μL. RESULTS: The linear range of berberine hydrochloride and baicalin were 60.3-312.8 ng(r=0.999 7) and 81.5-368.9 ng(r=0.999 9). The limits of quantitation were 0.666 8,0.774 0 ng, and the limits of detection were 0.222 6,0.258 0 ng, respectively. RSDs of intermediate precision, stability and repeatability tests were all lower than 1.0%. The recoveries were 96.48%-99.30%(RSD=1.06%,n=6) and 95.20%-99.39%(RSD=1.66%,n=6), respectively. RSDs of durability test were all lower than 2.0%. CONCLUSIONS: The method is simple, precise, stable, reproducible, accurate and  durable. It can be used for simultaneous determination of  berberine hydrochloride and baicalin in Jianpi zhixiening granules.
期刊: 2018年第29卷第10期
作者: 黄传俊,杨莉,梅勇,罗磊,吕姗珊,曾博程,龙涛,王凤,左娟,袁开超,唐攀,朱锋,陈波,谯志文
AUTHORS: HUANG Chuanjun,YANG Li,MEI Yong,LUO Lei,LYU Shanshan,ZENG Bocheng,LONG Tao,WANG Feng,ZUO Juan,YUAN Kaichao,TANG Pan,ZHU Feng,CHEN Bo,QIAO Zhiwen
关键字: 健脾止泻宁颗粒;高效液相色谱切换波长法;盐酸小檗碱;黄芩苷;含量测定
KEYWORDS: Jianpi zhixiening granules; HPLC switching walvelength method; Berberine hydrochloride; Baicalin; Content determination
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