HPLC法测定度米芬原料的有关物质  

Determination of related substances in domiphen bromide raw material by HPLC

作　　者：陈聪[1] 刘玉虎 王磊 CHEN Cong;LIU Yuhu;WANG Lei(Department of Pharmacy,Suzhou Hospital of Anhui Medical University(Suzhou Municipal Hospital of Anhui Province),Suzhou 234000,China;School of Pharmacy,Bengbu Medical University,Bengbu 233030,China)

机构地区：[1]安徽医科大学附属宿州医院(安徽省宿州市立医院)药剂科,宿州234000 [2]蚌埠医学院药学院,蚌埠233030

出　　处：《西北药学杂志》2023年第3期39-43,共5页Northwest Pharmaceutical Journal

基　　金：安徽省教育厅高校学科(专业)拔尖人才学术资助项目(编号:gxbjZD2021059)。

摘　　要：目的 建立高效液相色谱法检测度米芬原料的有关物质。方法 用Agilent 5TC C_(18)色谱柱;以乙腈为流动相A,0.03 mol·L^(-1)磷酸二氢钠+0.01 mol·L^(-1)十二烷基硫酸钠(磷酸调节pH至3.0)为流动相B,梯度洗脱;流速为1.0 mL·min^(-1);柱温为40℃;检测波长为220 nm;进样量为20μL。结果 度米芬与有关物质苯酚(1)、N,N-二甲基-2-苯氧基乙胺(2)、溴化N,N-二甲基-N-(2-苯氧乙基)-1-十烷铵(3)、溴化N,N-二甲基-N-(2-苯氧乙基)-1-十四烷铵(4)及强制破坏产物均能完全分离。苯酚、N,N-二甲基-2-苯氧基乙胺、溴化N,N-二甲基-N-(2-苯氧乙基)-1-十烷铵和溴化N,N-二甲基-N-(2-苯氧乙基)-1-十四烷铵分别在0.020 9~5.220μg·mL^(-1)(r=0.999 9)、0.018 5~4.620μg·mL^(-1)(r=0.999 6)、0.019 8~4.960μg·mL^(-1)(r=0.999 7)、0.017 4~4.340μg·mL^(-1)(r=0.999 4)范围内线性关系良好;定量限分别为18.19、12.38、15.34、13.81 ng·mL^(-1),检测限分别为6.13、4.79、5.26、3.94 ng·mL^(-1);苯酚、N,N-二甲基-2-苯氧基乙胺、溴化N,N-二甲基-N-(2-苯氧乙基)-1-十烷铵、溴化N,N-二甲基-N-(2-苯氧乙基)-1-十四烷铵平均回收率分别为99.74%、100.08%、99.19%、98.79%,RSD分别为0.56%、1.12%、0.91%、1.42%(n=12)。结论 所建立的方法操作便捷,结果准确,灵敏度高,专属性强,可用于度米芬原料有关物质的质量控制。Objective To establish an HPLC method for the detection of related substances in domiphen bromide raw material.Methods An Agilent 5TC C_(18) column was used,acetonitrile as mobile phase A,0.03 mol·L^(-1) sodium dihydrogen phosphate and 0.01 mol·L^(-1) sodium dodecyl sulfate(pH3.0 adjusted with phosphoric acid) as mobile phase B,in gradient elution,with flow rate of 1.0 mL·min^(-1).The column temperature was 40 ℃,the detection wavelength was 220 nm,and the injection volume was 20 μL.Results Domiphen bromide was completely separated from related substances,phenol(1),N,N-dimethyl-2-phenoxyethylamine(2),N,N-dimethyl-N-(2-phenoxyethyl)-1-tetradecane ammonium bromide(3) and N,N-dimethyl-N-(2-phenoxyethyl)-1-tetradecane ammonium bromide(4).Phenol,N,N-dimethyl-2-phenoxyethylamine,N,N-dimethyl-N-(2-phenoxyethyl)-1-tetradecane ammonium bromide and N,N-dimethyl-N-(2-phenoxyethyl)-1-tetradecane ammonium bromide showed good linear relationships in the ranges of 0.020 9-5.220 μg·mL^(-1)(r=0.999 9),0.018 5-4.620 μg·mL^(-1)(r=0.999 6),0.019 8-4.960 μg·mL^(-1)(r=0.999 7) and 0.017 4-4.340 μg·mL^(-1)(r=0.999 4),respectively.The limits of the quantification were 18.19,12.38,15.34 and 13.81 ng·mL^(-1),respectively.The limits of the detection were 6.13,4.79,5.26 and 3.94 ng·mL^(-1),respectively.The recoveries were 99.74%,100.08%,99.19% and 98.79% with the RSDs of 0.56%,1.12%,0.91% and 1.42%,respectively(n=12).Conclusion The method is sensitive and specific,which can be used to detect the related substances in domiphen bromide raw material.

关 键 词：度米芬 苯酚 N N-二甲基-2-苯氧基乙胺 溴化N N-二甲基-N-(2-苯氧乙基)-1-十烷铵 溴化N N-二甲基-N-(2-苯氧乙基)-1-十四烷铵 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]