顶空气相色谱法测定马来酸氟吡汀中有机溶剂残留

Determination of Residual Organic Solvents in Flupirtine Maleate by Headspace Gas Chromatography

目的：采用气相顶空色谱法测定马来酸氟吡汀原料药中的甲醇、乙醇和异丙醇3种有机溶剂的残留量。方法：采用DB-624（30 m×0.53 mm,3.0μm）毛细管色谱柱,载气为氮气,程序升温。FID检测器,温度为250℃。进样口温度为200℃。按外标法测定溶剂残留量。结果：甲醇,乙醇和异丙醇分别在2.182-152.74（r=0.999 1）,3.546-248.22（r=0.999 8）和4.082-285.74μg·m^l-1（r=0.999 7）范围内,线性关系良好;平均回收率分别为97.7%（RSD=1.5%）,99.0%（RSD=1.1%）,98.8%（RSD=1.1%）（n=5）。结论：本方法简便、准确,灵敏度高,适用于马来酸氟吡汀原料药中有机溶剂残留量的检测。

Objective：To determine the content of methanol, alcohol and isopropanol in flupirtine maleat by headspace gas chromatography. Methods：The capillary gas chromatography with programming temperature was established with an FID detector and a DB-624（30 m × 0. 53 mm,3. 0 μm） capillary column. The temperature of the injector and the detector was 200℃ and 250℃, respectively. The residual organic solvents were determined by an external standard method. Results： Methanol, alcohol and isopropanol showed good linearity within the range of 2. 182-152. 74（r=0. 999 1）, 3. 546-248. 22（r=0. 9998）and 4. 082-285. 74 μg·ml-1（r=0. 999 7） with the average recovery of 97. 7%（RSD=1. 5%）,99. 0%（RSD=1. 1%）and 98. 8%（RSD=1. 1%）（n=5）, respec-tively. Conclusion：The method is simple, sensitive and accurate, and can be used in the residual solvents detection for flupirtine maleat.