柱前衍生化法测定硝酸甘油注射液中亚硝酸盐的含量  

Determination of Nitrite in Nitroglycerin Injection by Precolumn Derivatization

作　　者：陈昊旻 王小婷 周小琴 颜慷祺 王涌杰 黄泽丹 CHEN Hao-min;WANG Xiao-ting;ZHOU Xiao-qin;YAN Kang-qi;WANG Yong-jie;HUANG Ze-dan(Guangzhou Baiyunshan Mingxing Pharmaceutical Company Limited,Guangdong Guangzhou 510250,China)

机构地区：[1]广州白云山明兴制药有限公司,广东广州510250

出　　处：《广州化工》2023年第6期84-86,共3页GuangZhou Chemical Industry

摘　　要：采用柱前衍生化法测定硝酸甘油注射液中亚硝酸根的含量。采用C18色谱柱(250 mm×4.6 mm,5μm);以甲醇-0.02 mol/L乙酸铵(V∶V=35∶65)为流动相;进样体积50μL为色谱条件进行方法学验证,并采用中国药典方法验证方法的准确性。该方法线性良好,亚硝酸根在0.0025~0.03μg范围内(即当进样体积为50μL时,被测定溶液在0.05~0.60μg/mL浓度范围内)与亚硝酸根衍生物色谱峰的峰面积有良好的线性关系,平均加样回收率为90.9%,该方法精密度良好,重复性与中间精密度RSD为1.2%。最低定量限以被测定溶液计算为0.057 ng。供试品溶液在16 h内稳定。本方法简便、准确、快速,适用于硝酸甘油注射液中亚硝酸根的含量测定。The content of nitrite in nitroglycerin injection was determined by pre-column derivatization.C 18 column(250 mm×4.6 mm,5μm)was used.The mobile phase was methanol-0.02 mol/L ammonium acetate(V∶V=35∶65).The sample volume of 50μL was used as the chromatographic condition for methodological verification,and the method of Chinese Pharmacopoeia was used to verify the accuracy of the method.The linearity of the method was good.Nitrite in the range of 0.0025~0.03μg(when the sample volume was 50μL,the measured solution in the range of 0.05~0.60μg/mL)had a good linear relationship with the chromatographic peak area of nitrite derivatives.The average sample recovery was 90.9%.RSD of repeatability and intermediate precision were 1.2%.The lowest limit of quantification was 0.057 ng for the measured solution.The test solution was stable within 16 h.The method was simple,accurate,rapid and suitable for the determination of nitrite in nitroglycerin injection.

关 键 词：高效液相色谱 衍生化 亚硝酸根 含量测定 

分 类 号：R917[医药卫生—药物分析学]