Determination of metformin hydrochloride, melamine and dicyandiamide in metformin hydrochloride preparations by tandem dual solid phase extraction cartridges-high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry

doi:10.3724/SP.J.1123.2017.10014

Abstract

Abstract:

A method for the confirmation and quantification of metformin hydrochloride and its relative substances melamine and dicyandiamide using tandem dual solid phase extraction (SPE) cartridges and high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry (HPLC-ESI-MSⁿ) was developed. The samples were extracted with anhydrous ethanol containing 0.1% (v/v) acetic acid under ultrasound-assisted conditions. The extracts were concentrated and purified using Cleanert PCX and C18 tandem dual solid phase extraction cartridges, and eluted with 5% (v/v) ammonia methanol solution. The separation was performed on a Kromasil-C18 column (100 mm×4.6 mm, 3.5 μm) with gradient elution. The detection was performed in selected ion monitoring (SIM) mode using electrospray ionization multi-stage mass spectrometry. The external standard method was used for quantification. The extraction solvents, types of SPE cartridges and eluents were optimized by comparing the recoveries under different conditions. The results showed that the detector response of each target compound was linear in corresponding mass concentration ranges with the correlation coefficients (r²) ≥ 0.9992. The limits of detection (LODs) and the limits of quantification (LOQs) of the three analytes were 1.48-13.61 μg/kg and 5.96-45.67 μg/kg, respectively. The recoveries of the three analytes were 65.02%-118.33% spiked at low, medium and high levels. The relative standard deviations (RSDs) were no more than 13.41%. The method is reliable, easy, and has a better purification effect. The method can be applied to the routine analysis of metformin hydrochloride and its relative substances melamine and dicyandiamide in different preparations of metformin hydrochloride.

Key words: dicyandiamide, high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry (HPLC-ESI-MSⁿ), melamine, metformin hydrochloride preparations, tandem dual solid phase extraction (SPE) cartridges

CLC Number:

O658

ZHOU Yanfen, WANG Fanghuan, WANG Zelan, ZHAN Haijuan, LIU Wanyi, MENG Zhe. Determination of metformin hydrochloride, melamine and dicyandiamide in metformin hydrochloride preparations by tandem dual solid phase extraction cartridges-high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(2): 159-166.

References

[1] Mu Y M, Ji L N, Ni G, et al. Chinese Journal of Diabetes, 2014, 22(8):673母义明, 纪立农, 宁光, 等. 中国糖尿病杂志, 2014, 22(8):673
[2] Xu X N, Shi R, Ma Y M. Acta Pharmaceutica Sinica, 2017, 52(6):865许希宁, 石荣, 马越鸣. 药学学报, 2017, 52(6):865
[3] Liu S N, Liu Q, Sun S J, et al. Acta Pharmaceutica Sinica, 2014, 49(11):1554刘率男, 刘泉, 孙素娟, 等. 药学学报, 2014, 49(11):1554
[4] Fang L J, Liu N F. Chinese Journal of Clinical Pharmacology and Therapeutics, 2011, 16(2):232方丽娟, 刘乃丰. 中国临床药理学与治疗学, 2011, 16(2):232
[5] Zhang J, Shen C W, Wang L, et al. Biochem Biophys Res Commun, 2014, 452(3):746
[6] Guo H R, Xu G F, Zhang H. Journal of Modern Oncology, 2017, 25(3):490郭海瑞, 徐桂芬, 张华. 现代肿瘤医学, 2017, 25(3):490
[7] Pharmacopoeia Commission of the People's Republic of China. Pharmacopoeia of the People's Republic of China, Part 2. Beijing:China Medical Science Press, 2015国家药典委员会. 中华人民共和国药典, 二部. 北京:中国医药科技出版社, 2015
[8] Li D G, Ju F L, Li C J. Chemical Analysis and Meterage, 2009, 18(2):24李东刚, 鞠福龙, 李春娟. 化学分析计量, 2009, 18(2):24
[9] Chen M S, Jing W, Lü S Y, et al. Chinese Journal of Analytical Chemistry, 2011, 39(10):1572陈旻实, 井伟, 吕水源, 等. 分析化学, 2011, 39(10):1572
[10] Meng L H, Liu X K, Guo J. China Dairy Industry, 2011, 39(6):60孟兰环, 刘兴凯, 郭军. 中国乳品工业, 2011, 39(6):60
[11] Chen X, Yuan H P, Cao Y H, et al. Chinese Journal of Analytical Chemistry, 2011, 39(9):1418陈新, 袁红萍, 曹玉华, 等. 分析化学, 2011, 39(9):1418
[12] Yun H, Yan H, Zhang Z H, et al. Chinese Journal of Chromatography, 2013, 31(5):404云环, 严华, 张朝晖, 等. 色谱, 2013, 31(5):404
[13] Qu G, Zhang G N, Su Y, et al. Chinese Journal of Analytical Chemistry, 2014, 42(7):1022曲干, 张冠男, 苏艳, 等. 分析化学, 2014, 42(7):1022
[14] Yang J, Ding J F, Zhou Y Y, et al. Food Science, 2014, 35(6):172杨嘉, 丁娟芳, 周元元, 等. 食品科学, 2014, 35(6):172
[15] Zhu X L, Liu J, Yan H, et al. Chinese Journal of Analysis Laboratory, 2013, 32(9):16朱晓玲, 刘杰, 严恒, 等. 分析试验室, 2013, 32(9):16
[16] Meng Z, Shi Z H, Liang S X, et al. Food Control, 2015, 55:158
[17] Men P, Gu X C, Zhai S D. Clinical Medication Journal, 2016, 14(4):30门鹏, 顾歆纯, 翟所迪. 临床药物治疗杂志, 2016, 14(4):30
[18] Gong Z G, Su M, Ji X C, et al. Chinese Journal of Chromatography, 2012, 30(1):33巩志国, 苏敏, 季新成, 等. 色谱, 2012, 30(1):33
[19] Liu L, Zhang Q, Wang H Y, et al. Chinese Journal of Chromatography, 2017, 35(8):860刘丽, 张琦, 王海雁, 等. 色谱, 2017, 35(8):860
[20] Gao Y, Xiu Y, Zhao H X, et al. Journal of Chinese Mass Spectrometry Society, 2017, 38(2):203高月, 修洋, 赵幻希, 等. 质谱学报, 2017, 38(2):203
[21] GB/T 22388-2008
[22] Desmarchelier A, Tessiot S, Bessaire T, et al. J Chromatogr A, 2014, 1337:75
[23] Rahman M M, El-Aty A M A, Choi J H, et al. Food Chem, 2015, 168:445