Zhou Yanfen, Wang Fanghuan, Wang Zelan, Zhan Haijuan, Liu Wanyi, Meng Zhe
School of Chemistry and Chemical Engineering, Ningxia University, State Key Laboratory of High-efficiency Coal Utilization and Green Chemical Engineering, Yinchuan 750021, China.
Inspection & Quarantine General Technical Center of Ningxia Entry-Exit Inspection & Quarantine Bureau, Yinchuan 750001, China.
Se Pu. 2018 Feb 8;36(2):159-166. doi: 10.3724/SP.J.1123.2017.10014.
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-MS) 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 () ≥ 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.
建立了一种使用串联双固相萃取（SPE）柱和高效液相色谱 - 电喷雾电离多级质谱（HPLC - ESI - MS）对盐酸二甲双胍及其相关物质三聚氰胺和双氰胺进行确认和定量的方法。样品在超声辅助条件下用含0.1%（v/v）乙酸的无水乙醇萃取。萃取液使用Cleanert PCX和C18串联双固相萃取柱进行浓缩和纯化，并用5%（v/v）氨甲醇溶液洗脱。在Kromasil - C18柱（100 mm×4.6 mm，3.5 μm）上进行梯度洗脱分离。采用电喷雾电离多级质谱在选择离子监测（SIM）模式下进行检测。采用外标法进行定量。通过比较不同条件下的回收率对萃取溶剂、SPE柱类型和洗脱剂进行了优化。结果表明，各目标化合物的检测器响应在相应质量浓度范围内呈线性，相关系数（）≥0.9992。三种分析物的检测限（LOD）和定量限（LOQ）分别为1.48 - 13.61 μg/kg和5.96 - 45.67 μg/kg。三种分析物在低、中、高加标水平下的回收率为65.02% - 118.33%。相对标准偏差（RSD）不超过13.41%。该方法可靠、简便，具有较好的净化效果。该方法可应用于盐酸二甲双胍不同制剂中盐酸二甲双胍及其相关物质三聚氰胺和双氰胺的常规分析。
