杨梅,李玮玲,伍良涌,李梓莹,陈敏余
YANG Mei,LI Weiling,WU Liangyong,LI Ziying,CHEN Minyu

• 1:广州市药品检验所

摘要(Abstract)：

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=0.999 9),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, 5 μm) 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 20 μL.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 1.8-72.2 μg·mL~(-1)(calculated as potassium nitrate, r=0.999 9).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(KeyWords)： 硝酸甘油;高效液相色谱法;游离硝酸根
nitroglycerin;HPLC;free nitrate ion

Abstract:

Keywords:

基金项目(Foundation): 广州市市场监督管理局科技项目(2022jk34)

作者(Author): 杨梅,李玮玲,伍良涌,李梓莹,陈敏余
YANG Mei,LI Weiling,WU Liangyong,LI Ziying,CHEN Minyu

参考文献(References)：

• [1] 赵静，王娜，冯叙桥，等.蔬菜中硝酸盐和亚硝酸盐检测方法的研究进展[J].食品科学，2014,35(8):42-43.
• [2] 廖德丰.硝酸盐和亚硝酸盐的毒理学效应及检测技术研究进展[J].生物学教学，2013,12(38):4-5.
• [3] 杨青霞，王伶，刘富强.硝酸甘油的药理作用及临床应用[J].药品评价，2006,3(3):214-215.
• [4] 高智平，黄慧珍.生脉注射液联用硝酸甘油治疗充血性心力衰竭36例临床观察[J].今日药学，2001,11(6)53-54.
• [5] 王颖彦，罗懿妮，黄洋扬，等.单硝酸异山梨酯与硝酸甘油治疗心衰的Meta-分析[J].今日药学，2015,25(4):249-252.
• [6] 伍良涌，潘锡强.反相高效液相色谱法测定硝酸甘油溶液及其制剂的有关物质[J].临床合理用药杂志，2010,3(20):1-3.
• [7] 伍良涌，潘锡强，黎志芳.中国药典2010年版硝酸甘油系列质量标准修订建议[J].药物分析杂志，2013,33(5):870-873.
• [8] Ph Eur.11.0[S].2023.
• [9] JP 18 [S].2023.
• [10] 赵艳秋，旺甜，尹燕杰，等.硝酸甘油片游离硝酸根离子的测定[J].海峡药学，2020,32(10):77-79.