摘要
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Ion Pac AS11分析柱(4 mm×250 mm),Ion Pac 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~(-1)1 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.
引文
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