顶空气相色谱法测定马来酸氟吡汀中有机溶剂残留

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。

Guangxi Institute for Food and Drug Control, Nanning 530021, China

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.