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目的建立聚偏二氯乙烯类药品包装材料中偏二氯乙烯单体含量的顶空气相色谱-电子捕获检测器(GC-ECD)法。方法采用HP-INNOWax(30.0 m×320μm,0.25μm)色谱柱;ECD检测器;顶空平衡温度为80℃,平衡时间为30 min,柱温为50℃,进样口温度为200℃,检测器温度为300℃,电流为1 n A;氦气载气,柱流速为1.0 m L·min-1。结果在2.0~150.0 ng内呈线性关系(r=0.999 2);平均回收率为99.1%,RSD=0.6%。结论顶空GC-ECD可以准确、灵敏地测定聚偏二氯乙烯类药品包装材料中偏二氯乙烯单体的含量。
Objective To establish a headspace gas chromatography-electron capture detector (GC-ECD) method for the determination of vinylidene chloride monomer in polyvinylidene chloride (PVC) packaging materials. Methods The chromatographic column of HP-INNOWax (30.0 m × 320 μm, 0.25 μm) and ECD detector were used. The headspace equilibrium temperature was 80 ℃, the equilibrium time was 30 min, the column temperature was 50 ℃ and the inlet temperature was 200 ℃. The temperature of the instrument was 300 ℃ and the current was 1 nA. The helium carrier gas was at a flow rate of 1.0 m L · min-1. The results showed a linear relationship in the range of 2.0-150.0 ng (r = 0.999 2). The average recovery was 99.1% and the RSD was 0.6%. Conclusion The headspace GC-ECD can accurately and sensitively determine the content of vinylidene chloride monomer in polyvinylidene chloride packaging materials.