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建立了超高效液相色谱-静电场轨道阱高分辨质谱(UPLC Orbitrap HRMS)法测定琥珀酸曲格列汀(1)原料药及其中间体2以及位置异构体3。采用Eclipse Plus-C_(18)色谱柱,以0.05 mol/L的乙酸铵缓冲液∶乙腈(45∶55)为流动相。质谱采用加热电喷雾离子源,正离子扫描模式,扫描范围m/z 200~500,监测离子分别为[M+H]~+m/z 358.167±0.003(1)、[M+H]~+m/z 294.044±0.003(2)、[M+H]~+m/z 358.167±0.003(3)。1琥珀酸盐在100~5 000 ng/ml范围内线性关系良好,有关物质2和3在1~50 ng/ml范围内线性关系良好,平均回收率分别为99.48%、97.51%和97.22%,RSD分别为1.63%、1.94%和2.17%;检测限均为0.01 ng/ml。本法定性可靠,定量准确,灵敏度高。
A UPLC Orbitrap HRMS method was developed for the determination of the active drug tranextrin succinate (1), its intermediate 2 and its positional isomer 3. Using Eclipse Plus-C_ (18) column, 0.05 mol / L ammonium acetate buffer: acetonitrile (45:55) as mobile phase. The mass spectrometry was performed with a heated electrospray ionization source and a positive ion scanning mode with a scan range of m / z 200-500 and monitored ions of [M + H] ~ + m / z 358.167 ± 0.003 (1), [M + H] m / z 294.044 ± 0.003 (2), [M + H] ~ + m / z 358.167 ± 0.003 (3). 1 succinate showed a good linearity in the range of 100-5000 ng / ml. The linearity of the related substances 2 and 3 in the range of 1-50 ng / ml was good, with the average recoveries of 99.48%, 97.51% and 97.22%, respectively. RSD were 1.63%, 1.94% and 2.17%, respectively. The detection limits were both 0.01 ng / ml. The statutory and reliable, quantitative and accurate, high sensitivity.