HPLC法同时测定盐酸赛洛唑啉鼻用喷雾剂主药和抑菌剂含量、递送剂量均一性及有关物质  

Simultaneous determination of the content of main medicine and bacteriostatic agent,the uniformity of delivery dose and related substance in xylometazoline hydrochloride nasal spray by HPLC

作　　者：黄金秋 梁琴 李苗 HUANG Jin-qiu;LIANG Qin;LI Miao(Wuhan Institute for Drug and Medical Device Control,Key Laboratory of State Drug Administration-Key Laboratory of Quality Research and Control of Pharmaceutical Preparation,Wuhan 430075,China;EBE Pharmaceutical Co.,Ltd,Wuhan 430058,China)

机构地区：[1]武汉药品医疗器械检验所,国家药品监督管理局重点实验室-药物制剂质量研究与控制重点实验室,武汉430075 [2]湖北远大天天明制药有限公司,武汉430058

出　　处：《药物分析杂志》2023年第8期1394-1401,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:采用HPLC法同时测定盐酸赛洛唑啉鼻用喷雾剂中盐酸赛洛唑啉、羟苯甲酯和羟苯丙酯的含量,并进行递送剂量均一性和有关物质检查。方法:采用SHISEIDO CAPCELL PEK C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%三乙胺(用冰醋酸调节pH至5.0)(45∶55)为流动相,流速1.0 mL·min^(-1),检测波长220 nm,柱温30℃,进样量10μL。结果:盐酸赛洛唑啉、羟苯甲酯和羟苯丙酯质量浓度分别在5.360~107.2μg·mL^(-1)(r=1.000),2.124~42.48μg·mL^(-1)(r=0.9999),1.034~20.68μg·mL^(-1)(r=1.000)范围内具有良好的线性关系。盐酸赛洛唑啉、羟苯甲酯和羟苯丙酯的平均回收率(n=9)分别为102.2%、101.4%、101.5%。3批样品中盐酸赛洛唑啉的含量分别为101.0%、101.1%、100.5%;羟苯甲酯的含量分别为0.22、0.21、0.21 mg·mL^(-1);羟苯丙酯的含量分别为0.10、0.10、0.10 mg·mL^(-1)。递送剂量均一性10个结果均在平均值的75%~125%。杂质Ⅰ的含量分别为1.6%、1.8%、1.9%。结论:经方法学验证,该方法简便、高效、准确,重复性好,可应用于盐酸赛洛唑啉鼻用喷雾剂的质量控制和标准研究。Objective:To establish an HPLC method for determination of the content of xylometazoline hydrochlo⁃ride,methylparaben and propylparaben,the uniformity of delivery dose and related substance in xylometazoline hydrochloride nasal spray.Methods:SHISEIDO CAPCELL PEK C18(250 mm×4.6 mm,5μm)was adopted with the mobile phase of acetonitrile-0.1%triethylamine(the pH was adjusted to 5.0 with acetic acid)(45∶55)at the flow rate of 1.0 mL·min^(-1).The detection wavelength was 220 nm.The column temperature was 30℃.The injection volume was 10μL.Results:The calibration curves of xylometazoline hydrochloride,meth⁃ylparaben and propylparaben were in good linear relation in the ranges of 5.360-107.2μg·mL^(-1)(r=1.000),2.124-42.48μg·mL^(-1)(r=0.9999),1.034-20.68μg·mL^(-1)(r=1.000),respectively.The average re⁃coveries of xylometazoline hydrochloride,methylparaben and propylparaben were 102.2%,101.4%,101.5%.In the three batches of samples,the content of xylometazoline hydrochloride was 101.0%,101.1%,100.5%,the content of methylparaben was 0.22,0.21,0.21 mg·mL^(-1),and propylparaben was 0.10,0.10,0.10 mg·mL^(-1),respectively.The ten results of the uniformity of delivery dose were between 75%-125%.The content of impurity I was 1.6%,1.8%,1.9%,respectively.Conclusion:The method is simple,rapid,accurate,and reproducible.It can offer reference for quality control and standard research of the drug.

关 键 词：高效液相色谱 盐酸赛洛唑啉 羟苯甲酯 羟苯丙酯 含量测定 递送剂量均一性 有关物质 

分 类 号：R917[医药卫生—药物分析学]