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10μL。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。
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.
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
HUANG Chuanjun;YANG Li;MEI Yong;LUO Lei;LYU Shanshan;ZENG Bocheng;LONG Tao;WANGFeng;ZUO Juan;YUAN Kaichao;TANG Pan;ZHU Feng;CHEN Bo;QIAO Zhiwen(Dept. of PharmaceuticalAffair,Hubei Provincial Hospital of TCM,Wuhan 430061,China;Hubei Institute of TCM,Wuhan 430074,China;Chongqing CISCO Pharmaceutical Research Institute Co.,Ltd.,Chongqing 401520,China)
出处
《中国药房》
CAS
北大核心
2018年第10期1324-1327,共4页
China Pharmacy
基金
重庆市社会民生科技创新专项项目(No.cstc2016shmszx130065)
关键词
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
Jianpi zhixiening granules
HPLC switching walvelength method
Berberine hydrochloride
Baicalin
Content determination
