冻干粉针用溴化丁基胶塞中溴化物的迁移及安全性评价 |
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引用本文: | 马艳,何小玲,黄武平,余秋玲,牟琼.冻干粉针用溴化丁基胶塞中溴化物的迁移及安全性评价[J].分析测试技术与仪器,2021,27(4):286-291. |
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作者姓名: | 马艳 何小玲 黄武平 余秋玲 牟琼 |
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作者单位: | 重庆市计量质量检测研究院,重庆 401123 |
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基金项目: | 重庆市计量质量检测研究院自立项目(2020(研)-3) |
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摘 要: | 建立了对溴化丁基胶塞中溴化物的提取方法,考察了胶塞中溴化物在冻干粉中的浸出水平. 采用IonPac AS 11-HC色谱柱(4.0 mm×250 mm)和IonPac AS 11-HC保护柱(4.0 mm×50 mm),24 mmol/L KOH淋洗液等度洗脱,AERS 500(4 mm)阴离子抑制器及电导检测器,抑制器电流60 mA,柱温30 ℃,流速1.0 mL/min. 溴化物在0.2~10.0 mg/L浓度范围内线性关系良好(r=0.999 9),检出限(LOD)为0.007 mg/L. 冻干粉针用溴化丁基胶塞以30%异丙醇水溶液为提取溶剂,80 ℃下保持7 h后测定提取液中溴化物含量. 冻干粉采用超纯水复溶后直接测定溴化物迁移量,迁移试验平均回收率为98.1%~104.3%,相对标准偏差(RSD,n=6)为2.9%~4.3%. 方法可用于包材相容性研究中实际样品的检测.
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关 键 词: | 离子色谱法 溴化丁基胶塞 冻干粉 溴化物 包材相容性 |
收稿时间: | 2021-10-07 |
Migration and Safety Evaluation of Bromide in Bromobutyl Rubber Stopper for Freeze-Dried Powder Injection |
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Affiliation: | Chongqing Academy of Metrology and Quality Inspection, Chongqing 401123, China |
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Abstract: | The extraction method of bromide in bromobutyl rubber stopper has been established, and the leaching level of bromide in freeze-dried powder was investigated. A chromatographic column IonPac AS 11-H (4.0 mm×250 mm) and a guard column IonPac AS 11-HC (4.0 mm×50 mm), and a 24 mmol/L potassium hydroxide solution were used for the isocratic elution. Bromide was detected by suppressed conductivity with an AERS 500(4 mm) suppressor at a current of 60 mA. The column temperature was 30 ℃ and the flow rate was 1.0 mL/min. The calibration curve showed a good linearity (r=0.999 9) in the range of 0.2~10.0 mg/L and the limit detection (LOD) was 0.007 mg/L. The brominated butyl rubber stopper was extracted by 30% isopropanol aqueous solution at 80 ℃ for 7 hours. The freeze-dried powder was redissolved in ultrapure water to detect the amount of bromide migration directivity. The average recoveries of the migration test were between 98.1% and 104.3%, and the relative standard deviations (RSD, n=6) were from 2.9% to 4.3%. The method can be used for the detection of real samples in the compatibility test of packaging materials. |
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