氧弹燃烧-离子色谱法测定药用卤化丁基橡胶塞中的卤素含量

目的：建立氧弹燃烧-离子色谱法测定药用卤化丁基橡胶塞中的氯、溴含量。方法：采用离子色谱IonPac AS11分析柱（4 mm×250 mm），IonPac AG11保护柱（4 mm×50 mm），以30 mmol·L^-1氢氧化钾溶液为淋洗液，流速1 mL·min^-1，柱温30℃，电导检测器检测。结果：被测物氯离子和溴离子能得到很好的分离，空白对照无干扰，氯离子和溴离子质量浓度分别在0.05~20.0 mg·L^-1（r=0.999 3）和0.2~32.0 mg·L^-1（r=0.998 9）范围内与峰面积呈良好的线性关系，平均回收率（n=6）分别为105.2%和103.7%，检测下限分别为0.01和0.03 mg·L^-1。3批氯化丁基橡胶塞中氯离子含量为0.39%~0.54%，3批溴化丁基橡胶塞中溴离子含量为0.57%~0.75%。结论：该方法可应用于药用卤化丁基橡胶塞中氯和溴的含量测定。

Objective:To establish a method of oxygen bomb-ion chromatography for determination of chloride and bromide contents in halogenated butyl rubber stoppers. Methods:An ion chromatography method was developed, and an IonPacAS11 anion chromatography column(4.0 mm×250 mm) with an AG-11 guard column(4.0 mm×50 mm) was adopted, with the eluent of 30 mmol·L^-1 potassium hydroxide solution. The flow rate was 1 mL·min^-1 and the detector was conductivity detector. Results:Chloride ion and bromide ion were well separated. The calibration curves of chloride and bromide showed good linear relationships in the ranges of 0.05-20.0 mg·L^-1(r=0.999 3) and 0.2-32.0 mg·L^-1(r=0.998 9);the average recoveries(n=6) of chloride and bromide were 105.2% and 103.7%. The LODs of chloride and bromide were 0.01 mg·L^-1 and 0.03 mg·L^-1. The contents of chloride ion in three batches of chlorinated butyl rubber stoppers were 0.39%-0.54%. The contents of bromide ion in three batches of brominated butyl rubber stoppers were 0.57%-0.75%. Conclusion:The method can be used for the determination of chloride and bromide contents in halogenated butyl rubber stoppers.