摘要
目的建立丁酸丙酸氢化可的松中4种残留有机溶剂的分离测定方法。方法采用毛细管气相色谱法,FID检测器,DB-Ⅰ石英毛细管柱(30m×0.3mm×1.8μm),载气为氮气,柱温40℃保持9min,以2℃/min升至68℃,再以70℃/min升至230℃,保持13min;测定丁酸丙酸氢化可的松原料中甲醇、丙酮、吡啶和N,N-二甲基甲酰胺的残留量。结果各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r为0.9983～0.9997,平均回收率为98.1%～100.0%。结论本方法灵敏、简便快速、结果准确,可用于丁酸丙酸氢化可的松中残留有机溶剂的检测。
Objective To establish a separation method for the determination of four kinds of residual organic solvents in hydrocortisone butyrate propionate.Methods Capillary gas chromatography was carried out on DB-I silica gel capillary column（30 m × 0.3 mm × 1.8 μm）with FID detector and nitrogen as carrier gas.Column temperature was 40 ℃ for 9 min,then increased to 68 ℃ at the rate of 2 ℃/min,then increased to 230 ℃ at the rate of 70 ℃/min,maintained for 13 min;The amounts of residues including methanol,acetone,pyridine,and N,N-dimethyl formamide in hydrocortisone butyrate propionate were determined.Results Various organic solvents could be effectively separated.A good linear relationship could be achieved in the concentration range examined with r as 0.998 3 to 0.999 7,and the average recovery rate was 98.1% to 100.0%.Conclusion This method is sensitive,rapid,accurate,and suitable for the determination of residual organic solvents in hydrocortisone butyrate propionate.
出处
《现代药物与临床》
CAS
2013年第3期350-352,共3页
Drugs & Clinic
关键词
丁酸丙酸氢化可的松
残留有机溶剂
毛细管气相色谱
hydrocortisone butyrate propionate
residual organic solvent
capillary gas chromatography
