HPLC法测定硝酸甘油溶液及其制剂的游离硝酸根  

Determination of Free Nitrate Ion of Nitroglycerin Solution and Its Preparation by HPLC

作　　者：杨梅 李玮玲[1] 伍良涌[1] 李梓莹 陈敏余 YANG Mei;LI Weiling;WU Liangyong;LI Ziying;CHEN Minyu(Guangzhou Institute for Drug Control,Guangzhou,Guangdong 510160,China)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《今日药学》2023年第9期686-689,693,共5页Pharmacy Today

基　　金：广州市市场监督管理局科技项目(2022jk34)。

摘　　要：目的建立高效液相色谱法测定硝酸甘油溶液及其制剂的游离硝酸根的方法。方法采用季铵盐强阴离子(Welch Ultimate XB-SAX柱,4.6 mm×250 mm,5μm)为填充剂,以35 mmol·L^(-1)磷酸二氢钾(用磷酸调节pH值至3.0)-乙腈(90∶10)为流动相,检测波长为220 nm,进样体积20μL,以外标法计算硝酸甘油溶液及其制剂的游离硝酸根的含量。结果硝酸根在1.8~72.2μg·mL^(-1)(以硝酸钾计)范围内线性关系良好(r=0.9999),定量限为72.2 ng·mL^(-1),检测限为24.1 ng·mL^(-1)。供试品溶液在24 h内稳定,辅料无干扰。结论所建立的方法测定硝酸甘油溶液及其制剂的游离硝酸根简便快捷,能准确测定样品的游离硝酸根。OBJECTIVE To develop HPLC method to determine the free nitrate ion of nitroglycerin solution and its preparation.METHODS The determination was performed on SAX(Welch Ultimate XB-SAX,4.6 mm×250 mm,5μm)column,with 35 mmol·L^(-1)potassium dihydrogen phosphate(adjusting pH to 3.0 with phosphoric acid)as the mobile phase.The detection wavelength was 220 nm.The injection volume was 20μL.The free nitrate ion of nitroglycerin solution and its preparation were quantified by external standard method.RESULTS Nitrate ion had a good linear relationship in the range of 1.8-72.2μg·mL^(-1)(calculated as potassium nitrate,r=0.9999).The limit of quantification was 72.2 ng·mL^(-1).The limit of detection was 24.1 ng·mL^(-1).The test solution was stable in 24 hours,and the auxiliary materials were noninterference.CONCLUSION The method is convenient,quick and accurate,and can be applied to the determination of free nitrate ion in nitroglycerin solution and its preparation.

关 键 词：硝酸甘油 高效液相色谱法 游离硝酸根 

分 类 号：R917[医药卫生—药物分析学]