毛细管气相色谱法测定丁酸丙酸氢化可的松中有机溶剂残留量  

Determination of residual organic solvents in hydrocortisone butyrate propionate by capillary gas chromatography

作　　者：刘言[1] 孙悦[1] 赵健[2] 

机构地区：[1]天津市药品检验所,天津300070 [2]天津泰普药品科技发展有限公司,天津300193

出　　处：《现代药物与临床》2013年第3期350-352,共3页Drugs & Clinic

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.

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 

分 类 号：R927.2[医药卫生—药学]