安全监测

药用溴化丁基橡胶塞中溴化物在药液中的迁移*

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  • 重庆市食品药品检验检测研究院,重庆 401121
第一作者 Tel:(023)86072759; E-mail:why751224021@163.com
** Tel:(023)86067359;E-mail:fannqcq@163.com

修回日期: 2021-04-30

  网络出版日期: 2024-07-15

基金资助

* 重庆市科研机构绩效激励引导专项(cstc2019jxjl130040)

Determinnation of bromide in bromobutyl rubber stoppers and its migration in medicines

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  • Chongqing Institute for Food and Drug Control,Chongqing 401121,China

Revised date: 2021-04-30

  Online published: 2024-07-15

摘要

目的: 建立炽灼残渣 - 离子色谱法,考察药用溴化丁基橡胶塞中溴化物及其在药液中的迁移情况。方法: 采用离子色谱柱 Metrosep A Supp 5(250/4.0)和保护柱 Metrosep A Supp 1 Guard/4.0,洗脱液为 3.2 mmol·L-1 碳酸钠溶液与 1.0 mmol·L-1 碳酸氢钠溶液,流速:0.7 mL·min-1,电导检测器,柱温为 30 ℃,进样 量 20 μL。结果: 溴离子浓度为 0.02~5.0 µg·mL-1,线性良好,相关系数 r 为 1.000;溴离子的提取试验与迁 移试验的平均回收率分别为 97.7% 和 101.1%,检测下限为 0.005 μg·mL-1;溴化丁基橡胶塞中溴离子含量 为 0.92%,经加速试验后药品中溴离子最大迁移量为 0.081 µg·d-1结论: 该方法操作简单,结果准确,灵敏度高,重复性好,可应用于药用溴化丁基橡胶塞中溴化物含量的测定及迁移研究。

本文引用格式

吴红洋, 曹汐, 张璞, 张帆, 杨柳, 范能全 . 药用溴化丁基橡胶塞中溴化物在药液中的迁移*[J]. 药物分析杂志, 2021 , 41(6) : 1024 -1028 . DOI: 10.16155/j.0254-1793.2021.06.12

Abstract

Objective: To establish a method of ignition residue-ion chromatography that determines the contents of bromide in bromobutyl rubber stopper and its migration in medicines. Methods: Chromatographic column Metrosep A Supp 5(250/4.0)and guard column Metrosep A Supp 1 Guard/4.0 were used with the eluent of 3.2 mmol·L-1 sodium carbonate and 1.0 mmol·L-1 sodium bicarbonate solution. The flow rate was 0.7 mL·min-1 and the detector was conductivity detector. The temperature of column was 30 ℃ and the injection volume was 20 μL. Results: Bromide had a good linear relationship(r=1.000)in the range of 0.02-5.0 µg·mL-1. The average recoveries of bromide extraction test and migration test were 97.7% and 101.1%,respectively. The limit of detection was 0.005 µg·mL-1. The amount of bromide in bromobutyl rubber stopper was 0.92% and its maximum migration rate in medicines was 0.081 µg·d-1 after accelerated test. Conclusion: The method is simple and accurate with high sensitivity and good repeatability, which can be applied to the extraction and migration studies of bromide in bromobutyl rubber stoppers for medicines.

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