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目的:建立顶空气相色谱法测定瑞库溴铵中甲醇、乙醚、丙酮、乙腈、二氯甲烷5种有机溶剂残留量的方法。方法:采用DB-624毛细管柱(60 m×0.53 mm×1μm),柱温为70℃,FID检测器,检测器温度为250℃,进样口温度为150℃,顶空平衡温度为90℃,顶空平衡时间为30 min,以水为溶剂。结果:5种溶剂的线性关系良好(r>0.999 6);平均回收率98.5%～99.8%,检测限为0.03～0.41μg·ml~(-1)。结论:方法操作简便,重复性好,准确可靠。
OBJECTIVE: To establish a method for the determination of the residues of five organic solvents, including methanol, diethyl ether, acetone, acetonitrile and methylene chloride in reckuronium bromide by headspace gas chromatography. Methods: The column temperature was 70 ℃ and the FID detector was used with a DB-624 capillary column (60 × 0.53 mm × 1μm). The detector temperature was 250 ℃, the inlet temperature was 150 ℃ and the equilibrium temperature at the headspace was 90 ℃ , The balance time of headspace is 30 min, using water as solvent. Results: The linear relationship between the five solvents was good (r> 0.999 6). The average recovery was 98.5% ~ 99.8%. The detection limit was 0.03 ~ 0.41μg · ml ~ (-1). Conclusion: The method is simple, reproducible, accurate and reliable.