顶空气相色谱法测定利福霉素钠原料中残留溶剂

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

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(30m×0.32mm×0.25μm),柱温采用程序升温,初始温度为40℃,保持5min;然后以10℃.min-1的升温速率升至50℃,保持1min;最后以50℃.min-1的升温速率升至200℃,保持5min;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0.7mL.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0.0100～4.0128mg.mL-1(r=1.0000)、0.0099～3.9766mg.mL-1(r=1.0000);最低检测限分别为0.9910μg.mL-1、1.3996μg.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。

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.