论文部分内容阅读
目的:建立司帕沙星中甲醇、乙腈、二甲苯和N,N-二甲基甲酰胺4种有机溶剂残留量的测定方法。方法:采用毛细管气相色谱法,以二甲基亚砜为溶剂,石英毛细管柱PEG-20M(15 m×0.53 mm,1.0μm),柱温:60℃恒温6 min,以30℃·min-1的速率升温至150℃恒温8 min;载气:高纯氮气,3.0 ml·min-1;氢气:50 ml·min-1;分流比为4:1。结果:方法平均回收率98.4%-100.1%(RSD<1.98%)。3批样品中4种有机溶剂残留量均符合要求。结论:本法简便灵敏、准确、重复性好,能较好地进行司帕沙星中有机残留量的测定。
Objective: To establish a method for the determination of sparfloxacin in methanol, acetonitrile, xylene and N, N-dimethylformamide. Methods: The capillary gas chromatography was used with dimethylsulfoxide (DMSO) as the solvent and the capillary column was PEG-20M (15 m × 0.53 mm, 1.0 μm). The column temperature was kept at 60 ℃ for 6 min and at 30 ℃ min-1 to a constant temperature of 150 ° C for 8 min; carrier gas: high purity nitrogen, 3.0 ml · min-1; hydrogen: 50 ml · min-1; split ratio of 4: 1. Results: The average recovery was 98.4% -100.1% (RSD <1.98%). Three batches of samples of four organic solvents residues are in line with the requirements. Conclusion: This method is simple, sensitive, accurate and reproducible. It can be used to determine the organic residues in sparfloxacin.