毛细管气相色谱法测定甘氨双唑钠中有机溶剂残留量

目的：建立测定甘氨双唑钠中Ⅳ，Ⅳ-二甲基甲酰胺及乙醇残留量的毛细管气相色谱法。方法：采用HP．FFAP毛细管色谱柱（30m×0．32mm×0．25岬），氢火焰离子化检测器，二甲基亚砜为溶剂，氮气为载气；程序升温：初始温度为40qC，保持5min，以每分钟8℃的升温速率升至110℃，保持2min，再以每分钟30℃的升温速率升至230℃，保持2min。结果：样品中未检出N，Ⅳ-二甲基甲酰胺，但有乙醇残留，按内标法计算得3批样品中乙醇残留量分别为0．44％、0．46％和0．46％。结论：该方法灵敏、准确、重复性好，可用于甘氨双唑钠中有机溶剂残留量的测定。

Determination of Organic Solvent Residue in Glycididazole Sodium by Capillary GC

Objective： To establish a capillary gas chromatography method for the determination of resi- due of N, N-dimethylformamide（DMF） and alcohol in glycididazole sodium. Methods： HP-FFAP capillary column was used, with FID as detector, DMSO as the solvent and nitrogen as the carrier gas. Temperature programming was used as follows： the initial column temperature was 40 ℃ which was maintained for 5 min, and then raised to 110 ℃ at a rate of 8 ℃ -min-1 for 2 min, and then raised to 230 ℃ at a rate of 30 ℃ .min-1 for 2 min. Results： The DMF content was under the limit of detection, and the residue of alcohol calculated by interal standard method was 0. 44%, 0. 46% and 0. 46% in 3 batches of samples, respectively. Conclusion： The method is sensitive, accurate and highly reproducible. It can be used to determine the organic solvent residue in glycididazole sodium.