目的采用顶空气相色谱法测定亚甲基二膦酸(MDP)中乙醚和吡啶的残留量。方法采用DB-624色谱柱(30 m×0.32 mm,1.8μm),柱温采用程序升温,检测器(FID)温度为250℃,载气为氮气,流速2 mL·min-1,分流比为20∶1。结果MDP中乙醚、吡啶线的性范围分别为0.0196～0.980 mg·mL-1(r=0.9996)、2.72～89.90μg·mL-1(r=0.9996),平均回收率分别为100.5%、97.9%。结论所用方法操作简便、结果准确、灵敏度及重复性好。 Objective To determine the residues of diethyl ether and pyridine in methylene diphosphonic acid (MDP) by headspace gas chromatography. Methods The column temperature was programmed with a DB-624 column (30 m × 0.32 mm, 1.8 μm). The temperature of the detector (FID) was 250 ℃, the carrier gas was nitrogen and the flow rate was 2 mL · min- 20: 1. Results The average recoveries of diethyl ether and pyridine in MDP ranged from 0.0196 to 0.980 mg · mL -1 (r = 0.9996) and from 2.72 to 89.90 μg · mL -1 (r = 0.9996), with the average recoveries of 100.5% and 97.9% . Conclusion The method used is simple, accurate, sensitive and reproducible.