顶空气相色谱法测定利福霉素钠原料中残留溶剂

目的 建立利福霉素钠原料中残留溶剂的检测方法.方法 采用气相色谱顶空进样法,DB-FFAP毛细管柱（30 m×0.32 mm×0.25 μm）,柱温采用程序升温,初始温度为40℃,保持5 min;然后以10℃·min-1的升温速率升至50℃,保持1 min；最后以50℃·min-1的升温速率升至200℃,保持5 min;进样口温度为200℃,FID检测器温度为250℃,分流比为20∶1,N2流速为0.7 mL· min-1.结果 异丙醇和乙酸丁酯分离度良好,顶空进样检测的色谱峰面积与浓度线性关系良好,线性范围分别为0.0100～4.0128 mg,mL-1（r＝1.0000）、0.0099～3.9766 mg· mL-1（r=1.0000）；最低检测限分别为0.9910 μg·mL-1、1.3996 μg·mL-1；3种浓度的平均加样回收率为95.9％～101.9％（n=3,RSD为0.84％～2.34％）；重复性RSD为0.31％～1.72％（n=3）.结论 该方法选择性强、重复性好、灵敏度高、操作方便,可以作为利福霉素钠原料中残留溶剂的质控方法.

Determination of Residual Organic Solvents in Rifamycin Sodium Raw Materials by Headspace Gas Chromatography

Objective To establish a method for the content determination of the residual organic solvents in Rifamycin Sodium raw materials. Methods Headspace GC was adopted. The determination was separated on a DB-FFAP capillary column （30 m× 0.32 mm× 0.25 μm） using temperature programming as follow： the temperature was initially kept at 40 ℃ for 5 minutes, then raised to 50 ℃ at the rate of 10 ℃ · min-1 and kept for 1 minutes, and finally the temperature was raised to 200 ℃ at the rate of 50 ℃ · min-1 and kept for 5 minutes. FID was used as detector at 250 ℃, the inlet temperature was 200 ℃, and the split ratio was 20 ： 1. Results Isopropyl alcohol and butyl acetate were completely separated. The method had good linear relationship with the ranges of 0. 0100-4. 0128 mg · mL-1 for isopropylalcohol （r = 1.0000）, 0.0099-3.9766 mg · mL-1 for butyl acetate （r = 1.0000）. The detection limits were 0. 9910 μg · mL-1 and 1. 3996 μg · mL-1, respectively. The average recoveries were in the range of 95. 9%-101. 9% with RSD of 0.84%-2.34%. The range of repeatability RSD was 0.31%-1.72 % （n = 3 ）. Conclusion The established method is selective, reproducible, sensitive and convenient, which can be used for the quality control of the residual organic solvents in Rifamycin Sodium raw materials.