盐酸溴己新滴丸工艺优选及其盐酸溴己新含量测定

Optimization of Preparation Process of Bromhexin Hydrochloride Dropping Pills and Content Determination of Bromhexin Hydrochloride in the Pills

目的优选盐酸溴己新滴丸制备工艺,并建立测定其中盐酸溴己新含量的高效液相色谱(HPLC)法。方法采用单因素试验法优选滴丸制备工艺。色谱柱为Eclipse XDB-C_(18)柱(150 mm×4.6 mm,5μm),流动相为醋酸溶液(以三乙胺调pH至3.2)-甲醇(45∶55,V/V),流速为1.0 mL/min,检测波长为247 nm,柱温为30℃,进样量为10μL。结果优选的滴丸制备工艺为,聚乙二醇(PEG)4000∶PEG 6000=1∶1(m/m),冷凝剂为液状石蜡,其温度为(10±2)℃,药物∶基质=1∶15(m/m),药液滴制温度控制在90~95℃,滴制距离为(10±2)cm,滴速以每滴3~4 s为佳。盐酸溴己新质量浓度在0.0412~0.2060 mg/mL范围内与峰面积线性关系良好(r=0.9994,n=5);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为100.14%,RSD为1.34%(n=9)。3批样品的平均含量分别为每丸含2.57,2.80,2.60 mg。结论优选的该滴丸制备工艺可行,且效果好;所建HPLC法操作简单、专属性强、准确可靠,可用于盐酸溴己新滴丸中盐酸溴己新的含量测定。

Objective To optimize the preparation process of Bromhexin Hydrochloride Dropping Pills,and to establish a high-performance liquid chromatography(HPLC)method for the content determination of bromhexin hydrochloride in the Pills.Methods The preparation process of dropping pills was optimized by the single factor test.The chromatographic column was Eclipse XDB-C_(18) column(150 mm×4.6 mm,5μm),the mobile phase was acetic acid solution(adjusted to pH 3.2 with triethylamine)-methanol(45∶55,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 247 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The optimal preparation process of the drop pills was as follows:polyethylene glycol(PEG)4000∶PEG6000=1∶1(m/m),the condensing agent was liquid paraffin,the temperature was(10±2)℃,the drug∶matrix was 1∶15(m/m),the dropping temperature was controlled at 90-95℃,the dropping distance was(10±2)cm,and the best dropping speed was 3-4 s per drop.The linear range of bromohexidine hydrochloride was 0.0412-0.2060 mg/mL(r=0.9994,n=5).The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery of bromohexidine hydrochloride was 100.14% with an RSD of 1.34%(n=9).The average contents of the three batches of samples were 2.57,2.80 and 2.60 mg/pill,respectively.Conclusion The optimal preparation process of the dropping pills is feasible and has good effect.The established HPLC method is simple,specific,accurate and reliable,which can be used for the content determination of bromhexin hydrochloride in Bromhexin Hydrochloride Dropping Pills.