Citation: 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. doi: 10.3724/SP.J.1123.2017.10014 shu

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

1.
School of Chemistry and Chemical Engineering, Ningxia University, State Key Laboratory of High-efficiency Coal Utilization and Green Chemical Engineering, Yinchuan 750021, China;
2.
Inspection & Quarantine General Technical Center of Ningxia Entry-Exit Inspection & Quarantine Bureau, Yinchuan 750001, China

Received Date: 16 October 2017

Fund Project: Natural Science Foundation of Ningxia (No.NZ16036)

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.
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沈阳化工大学材料科学与工程学院沈阳 110142