目的 建立丁酸丙酸氫化可的松中4種殘留有機(jī)溶劑的分離測定方法。方法 采用毛細(xì)管氣相色譜法，F(xiàn)ID檢測器，DB-Ⅰ石英毛細(xì)管柱（30 m×0.3 mm×1.8 μm），載氣為氮?dú)?，柱?0 ℃保持9 min，以2 ℃/min升至68 ℃，再以70 ℃/min升至230 ℃，保持13 min；測定丁酸丙酸氫化可的松原料中甲醇、丙酮、吡啶和N,N-二甲基甲酰胺的殘留量。結(jié)果 各有機(jī)溶劑均能得到有效分離，在所考察的濃度范圍內(nèi)線性關(guān)系良好，r為0.998 3～0.999 7，平均回收率為98.1%～100.0%。結(jié)論 本方法靈敏、簡便快速、結(jié)果準(zhǔn)確，可用于丁酸丙酸氫化可的松中殘留有機(jī)溶劑的檢測。

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.