HPLC法同时测定四味姜黄汤散中7种成分的含量

Simultaneous Determination of 7 Components in Siwei Jianghuang Decoction Powder by HPLC

目的:建立同时测定四味姜黄汤散中没食子酸、木兰花碱、鞣花酸、盐酸药根碱、盐酸巴马汀、盐酸小檗碱和姜黄素含量的方法。方法:采用高效液相色谱法。色谱柱为Capcell Pak C18-MGⅡ,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为0.8 m L/min,检测波长为270 nm(0~60 min,没食子酸、木兰花碱、鞣花酸、盐酸药根碱、盐酸巴马汀、盐酸小檗碱)和428 nm(60~70 min,姜黄素),柱温为30℃,进样量为10μL。结果:没食子酸、木兰花碱、鞣花酸、盐酸药根碱、盐酸巴马汀、盐酸小檗碱和姜黄素进样量检测线性范围分别为0.249 6~1.497 6、0.284 0~1.704 0、0.075 6~0.453 6、0.015 9~0.095 9、0.023 6~0.141 6、0.098 2~0.589 0、0.060 4~0.362 4μg(r≥0.999 8);检测限分别为6.24、4.73、7.56、2.36、3.20、6.54、6.04 ng,定量限分别为17.47、16.08、20.86、7.31、10.24、19.62、19.32 ng;精密度、稳定性(12 h)、重复性试验的RSD<2.0%(n=6);加样回收率为95.45%~103.47%,RSD为0.86%~1.98%(n=9)。结论:建立的方法操作简便,结果准确可靠,适用于四味姜黄汤散中没食子酸等7种成分含量的同时测定。

OBJECTIVE： To establish a method for simultaneous determination of gallic acid, magnoflorine, ellagic acid, jatrorrhizine hydrochloride, palmatine hydrochloride, berberine hydrochloride and curcumin in Siwei jianghuang decoction powder. METHODS： HPLC method was adopted. The determination was performed on Capcell Pak C18-MG II column with mobile phase consisted of acetonitrile-0.1% phosphoric acid （gradient elution） at the flow rate of 0.8 mL/min. The detection wavelengths were 270 nm （0-60 min, gallic acid, magnoflorine, ellagic acid, jatrorrhizine hydrochloride, palmatine hydrochloride, berberine hydrochloride） and 428 nm （60-70 min, curcumin）. The column temperature was set at 30 ℃, and sample size was 10 ~tL. RESULTS： The linear ranges of gallic acid, magnoflorine, ellagic acid, jatrorrhizine hydrochloride, palmatine hydrochloride, berberine hydrochloride and curcumin were 0.249 6-1.497 6, 0.284 0-1.704 0, 0.075 6-0.453 6, 0.015 9-0.095 9, 0.023 6-0.141 6, 0.098 2-0.589 0 and 0.060 4-0.362 4 μg （r≥0.999 8）. The limits of detection were 6.24, 4.73, 7.56, 2.36, 3.20, 6.54, 6.04 ng, and the limits of quantitation were 17.47, 16.08, 20.86, 7.31, 10.24, 19.62, 19.32 ng, respectively. RSDs of precision, stability （12 h）, reproducibility tests were lower than 2.0% （n=6）. The recoveries were 95.45%-103.47% （RSD-0.86%-1.98% , n=9）. CONCLUSIONS： Established method is simple, accurate, reliable and suitable for simultaneous determination of 7 components such as gallic acid in Siwei jianghuang decoction powder. KEYWORDS Siwei jianghuang decoction powder; HPLC; Gallic acid; Magnoflorine; Ellagic acid; Jatrorrhizine hydrochloride; Palmatine hydrochloride; Berberine hydrochloride; Curcumin; Content determination