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[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(30 m×0.3 mm×1.8 μm),载气为氮气,柱温40 ℃保持9 min,以2 ℃/min升至68 ℃,再以70 ℃/min升至230 ℃,保持13 min;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0.998 3~0.999 7,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。
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[Abstract]
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.
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