复方水杨酸甲酯苯海拉明喷雾剂中5个活性成分的含量测定  

Simultaneous determination of five active components in compound methyl salicylate and diphenhydramine spray

作　　者：钱敏 宋冬梅 乐健 QIAN Min;SONG Dong-mei;LE Jian(Shanghai Institute for Food and Drug Control,Shanghai 201203,China;National Medical Products Administration Key Laboratory for Quality Analysis of Chemical Drug Preparations,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验研究院,上海201203 [2]国家药品监督管理局化学药品制剂质量分析重点实验室,上海201203

出　　处：《药物分析杂志》2023年第1期70-76,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药品标准提高研究项目(食药监办药化管[2017]139号)。

摘　　要：目的:建立气相色谱法同时测定复方水杨酸甲酯苯海拉明喷雾剂中水杨酸甲酯、薄荷脑、樟脑、麝香草酚和盐酸苯海拉明的含量。方法:采用聚乙二醇20M毛细管色谱柱(30 m×0.53 mm, 1.0μm),氦气为载气,氢火焰离子检测器,程序升温(起始温度为160℃,维持10 min,再以50℃·min^(-1)的速率,升温至230℃,维持12 min),进样口温度200℃;检测器温度250℃,萘为内标。结果:水杨酸甲酯、薄荷脑、樟脑、麝香草酚和盐酸苯海拉明的质量浓度分别在1.504~4.512、1.198~3.594、1.910~5.730、0.148 4~0.445 2、0.091 07~0.273 2 mg·mL^(-1)范围内与各相应成分峰和内标峰的峰面积比值呈良好线性关系(r均>0.999,n均为5);低、中、高3个浓度水平9份样品的平均加样回收率分别为99.0%(RSD=0.65%)、99.9%(RSD=0.62%)、101.6%(RSD=0.73%)、102.5%(RSD=1.1%)、100.1%(RSD=1.8%);精密度、稳定性良好,RSD均<2.0%。样品中5个活性成分的含量均介于标示量的88.0%~103.0%。结论:该方法简便快捷,专属性好,可用于复方水杨酸甲酯苯海拉明喷雾剂的质量控制,为质量标准提高提供参考。Objective: To establish a method for the simultaneous determination of methyl salicylate, menthol, camphor, thymol and diphenhydramine hydrochloride in compound methyl salicylate and diphenhydramine spray by GC. Methods: The GC was performed on a PEG-20M capillary column(30 m×0.53 mm, 1.0 μm) with an FID detector. Helium was used as the carrier gas. Temperature program(maintain the column initial temperature at 160 ℃ for 10 min, then raise the temperature to 230 ℃ at a rate of 50 ℃·min^(-1)and maitaine for 12 min). The inlet temperatrue was 200 ℃. The temperature of detector was 250 ℃. Naphthalene was used as the internalstandard. Results: Methyl salicylate, menthol, camphor, thymol and diphenhydramine hydrochloride showed good linear relationships(r>0.999, n=5) with the ratio of peak area of each component peak and internal standard peak in the concentration ranges of 1.504-4.512 mg·mL^(-1), 1.198-3.594 mg·mL^(-1), 1.910-5.730 mg·mL^(-1), 0.148 4-0.445 2 mg·mL^(-1), 0.091 07-0.273 2 mg·mL^(-1), respectively. The average recoveries of 9 samples at low, medium and high concentrations were 99.0%(RSD=0.65%), 99.9%(RSD=0.62%), 101.6%(RSD=0.73%), 102.5%(RSD=1.1%), 100.1%(RSD=1.8%) respectively. The precision and stability were good with RSDs less than 2.0%. The contents of 5 active ingredients in the samples were all between 88.0% and 103.0% of the labeled amount. Conclusion: The established method is simple, rapid, specific and can be used for the quality control of compound methylsalicylate and diphenhydramine spray, providing reference for the improvement of quality standards.

关 键 词：复方水杨酸甲酯苯海拉明喷雾剂 水杨酸甲酯 薄荷脑 樟脑 麝香草酚 盐酸苯海拉明 萘 气相色谱法 内标法 质量控制 

分 类 号：R917[医药卫生—药物分析学]