盐酸二甲双胍肠溶胶囊中二甲胺残留量的测定

摘要/Abstract

摘要： 目的：建立盐酸二甲双胍肠溶胶囊中二甲胺残留量的柱前衍生HPLC测定方法。方法：用十八烷基硅烷键合硅胶为填充剂，以1.0%甲酸溶液-乙腈为流动相，采用梯度洗脱程序，检测波长为265 nm。结果：在选定的色谱条件下，二甲胺在0.254～4.065 μg·mL-1的浓度范围内线性关系良好（r>0.999）；精密度试验的RSD为1.6%，稳定性试验的RSD为1.5%；回收率为100.3%（n=9，RSD<1.5%）。二甲胺的检测限为0.050 8 μg·mL-1，在测定的3批样品中，3批均检出二甲胺分别为0.01%，0.04%，0.02%。结论：本方法专属性强，准确度高，重现性好，能控制盐酸二甲双胍肠溶胶囊中二甲胺残留量。

关键词: 高效液相色谱法, 盐酸二甲双胍, 二甲胺, 柱前衍生

Abstract: Objective：To establish pre-column derivatization and HPLC method for the determination of dimethylamine in Metforminhydrochloride enteric-coated capsules.Methods：With octadecylsilane chemically bonded silica as filler， With 1.0% formic acid solution (A) and acetonitrile (B) as mobile phase， ingradientelution，and the detectionwavelength was 265 nm. Results： In the spectrum of the selectedconditions，A good linearity observed in the range of 0.254~4.065 μg·mL-1 (r＞0.999)dimethylamine. The RSD of the precision was 1.6%，The RSD of stability test was 1.5%；The recovery was 100.3%（n=9，RSD<1.5%）. The limit of detection was 0.050 8 μg·mL-1.The test results of 3 batches of samples was 0.01%，0.04%，0.02%. Conclusion： The method is specific， accurate and reproducible for the determination of dimethylamine in metformin hydrochloride enterin-coated capsules.

Key words: HPLC, Metformin hydrochloride, Dimethylamine, Pre-column derivation

中图分类号:

R917

甘加明李永平黄诺哲黄莹严全鸿. 盐酸二甲双胍肠溶胶囊中二甲胺残留量的测定[J]. 中国药物评价, 2020, 37(1): 31-35.

参考文献

[1]王天歌.中国成人糖尿病流行与控制现状及危险因素研究[D].上海交通大学，2014.
[2]于波.型糖尿病治疗的首选药物-二甲双胍[J].赤峰学院学报自然科学版, 2015, 31(3):94-95
[3]周盛鹏，周俊枝，江婕，等.二甲双胍在型糖尿病治疗中的基石地位—— 糖尿病全球防治指南及共识声明的解读[J].中国全科医学, 2007, 10(6):470-471
[4]许同桃，温委委，陶永，等.盐酸二甲双胍的合成工艺研究[J].化工时刊, 2010, 24(9):17-19
[5]罗海英，陈亚精，林静佳，等.高效液相色谱法测定工作场所空气中的二甲胺[J].中国卫生检验杂志, 2014, 24(12):1691-1693
[6]杨忠莲，高宝玉，王燕，等.聚合氯化铁-聚环氧氯丙烷-二甲胺复合絮凝剂在模拟染料废水处理中的絮体特性研究[J].功能材料, 2012, 43(14):1936-1940
[7]Sacher F，Lenz S.Brauch HAnalysis of Primary and Secondary Aliphatic Amines in Waste Water and Surface Water by Gas Chromatography-Mass Spectrometry after Derivatization with 2，4-Dinitrofluorobenzene or Benzenesulfonyl Chloride[J].Journal of Chromatorgraphy A, 1997, 764(1):85-93
[8]Abalos M，Bayona J N，Ventura F， Development of a Solid-Phase Microextraction GC-NPD Procedure for the Determination of Free Volatile Amines in Wastewater and Sewage-Polluted Waters[J].Anal Chem，1999，71(16)：3531-3537.
[9]皇雪娟，吴娟娟，朱雄.法测定马来酸阿法替尼中二甲胺残留量[J].海峡药学, 2018, 30(2):68-70
[10]国家药典委员会.中华人民共和国药典2015年版（二部）[S]. 北京：中国医药科技出版社，2015：859.
[11]The united states pharmacopoeial convention US.Pharmacopoeia National Formulary USP41-36[S].US Pharmacopoeia Convention，2017：2614-2618.
[12]The japanese pharmacopoeia expert commtitees.The Japanese Pharmacopoeia Seventeenth Edition[S].The Japanese Ministiy of Health，Labour and Welfare，2017：1222-1223.
[13]British pharmacopoeia commission.British Pharmacopoeia 2018[S].British Pharmacopoeia Commission，2017：Ⅱ~235-237.
[14]Council of europe.European Pharmacopoeia 9.0[S].Strasbourg：European Directorate for the quality of Medicines & Heath Care council of Europe，2016：3014-3015.
[15]冯超，张友谊，徐雪，等.柱前衍生化-法测定盐酸二甲双胍原料中有关物质二甲胺[J].中国新药杂志, 2015, 24(10):1191-1196
[16]张琳，平贵臣，于晓明，等.氯甲酸-9-芴甲酯柱前衍生脂肪胺类化合物的反相高效液相色谱分析[J].现代仪器，2004，2：14-16，18.