风寒感冒颗粒中含量测定方法研究

目的:建立测定风寒感冒颗粒中盐酸麻黄碱、盐酸伪麻黄碱和葛根素含量的HPLC法,制定含量参考限度。方法:盐酸麻黄碱、盐酸伪麻黄碱含量以Sunfire C 18(4.6 mm×250 mm,5μm)为色谱柱,乙腈-0.02 mol·L^-1磷酸二氢钾溶液(含0.2%三乙胺,用磷酸调pH至2.7)(3∶97)为流动相,检测波长210 nm,柱温30℃;葛根素含量以Agilent ZORBAX Eclipse plus C 18(4.6 mm×250 mm,5μm)为色谱柱,甲醇-水(24∶76)为流动相;检测波长250 nm,柱温30℃。结果:三种成分进样量分别在0.0226~0.4514μg、0.0168~0.3359μg、0.1670~1.2524μg范围内线性关系良好(r为0.9999~1.0000);精密度、重复性、稳定性试验的RSD均小于2%;平均回收率分别为99.91%、99.79%、101.51%,RSD均小于3%。结论:新建立的方法专属性强,稳定性好,重复性好,可用于该制剂中盐酸麻黄碱、盐酸伪麻黄碱和葛根素的含量测定,测定了280批次样品的数据,拟定了含量参考限度值。

Study on the Determination Method of Fenghan ganmao Granules

Objective:To establish an HPLC method for the determination of ephedrine hydrochloride,pseudoephedrine hydrochloride and puerarin in Fenghan Ganmao Granules,and to set a reference limit for the contents.Methods:The contents of ephedrine hydrochloride and pseudoephedrine hydrochloride were determined by using Sunfire C 18 column(4.6 mm×250 mm,5μm)under the isocratic elution of acetonitrile-0.02 mol·L^-1potassium dihydrogen phosphate solution(containing 0.2%triethylamine,and adjusting the pH to 2.7 with phosphoric acid)(3∶97).The detection wavelength was 210nm,and the column temperature was 30℃.The content of puerarin was determined by using Agilent ZORBAX Eclipse plus C 18 column(4.6 mm×250 mm,5μm)under the isocratic elution of methanol-water(24∶76).The detection wavelength was 250 nm and the column temperature was 30℃.Results:The linear ranges of ephedrine hydrochloride,pseudoephedrine hydrochloride and puerarin fell into 0.0226-0.4514μg,0.0168-0.3359μg and 0.1670-1.2524μg,respectively(r as 0.9999-1.0000).The RSDs of the precision,repeatability and stability were less than 2%,and the average recoveries of ephedrine hydrochloride,pseudoephedrine hydrochloride and puerarin were 99.91%,99.79%,101.51%,respectively(RSD less than 3%).Conclusion:The established method has the strong specificity,good stability and good reproducibility.It can be used for the determination of ephedrine hydrochloride,pseudoephedrine hydrochloride and puerarin in Fenghan Ganmao Granules.280 batches of samples have been determined,and the content reference limits have been set.