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目的建立顶空毛细管气相色谱法(Headspace gas chromatographic method,HGC),测定阿加曲班中甲醇、乙醇、丙酮与二氯甲烷4种有机溶剂的残留量。方法色谱柱为DB-624毛细管柱(30.0 m×0.25 mm×1.4μm);载气为氮气;FID检测器;采用顶空进样,进样口温度为140℃;采用程序升温:起始温度为40℃,维持4 min,继以每分钟5℃升温至80℃,维持2 min,再以每分钟20℃升温至200℃,维持6 min。结果 4种有机溶剂的分离度符合要求,线性关系良好(r≥0.999 0),平均回收率在100.7%~104.0%范围内,3批阿加曲班样品检测结果均符合限度要求。结论该法简便准确,灵敏度高,适用于阿加曲班原料中残留溶剂的测定。
Objective To establish a headspace gas chromatographic method (HGC) for the determination of the residues of four organic solvents, methanol, ethanol, acetone and methylene chloride in argatroban. Methods The column was DB-624 capillary column (30.0 m × 0.25 mm × 1.4 μm). The carrier gas was nitrogen. The FID detector was operated with headspace sampling. The inlet temperature was 140 ℃. The temperature was maintained at 40 ° C for 4 min, followed by heating at 5 ° C to 80 ° C for 2 min. The temperature was raised to 200 ° C at 20 ° C per minute for 6 min. Results The resolution of the four organic solvents was satisfactory. The linearity was good (r≥0.999 0). The average recoveries ranged from 100.7% to 104.0%. The results of three batches of argatroban samples all met the limits. Conclusion The method is simple, accurate and sensitive. It is suitable for the determination of residual solvents in argatroban raw materials.