| 李樾,许凯,宋晓松,杨锐,肖新月,孙会敏.药用辅料蔗糖中亚硫酸盐检测方法的建立[J].中国药事,2021,35(9):1046-1051 |
| 药用辅料蔗糖中亚硫酸盐检测方法的建立 |
| Establishment of Sulfite Detection Method for Pharmaceutical Excipient Sucrose |
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| DOI：10.16153/j.1002-7777.2021.09.012 |
| 中文关键词: 药用辅料 蔗糖 亚硫酸盐 离子色谱 |
| 英文关键词: medicinal excipient sucrose sulfites ion chromatography |
| 基金项目:药典会质量标准提高课题(编号 2020Y015) |
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| 摘要点击次数: 653 |
| 全文下载次数: 9 |
| 中文摘要: |
| 目的：建立适宜的蔗糖中亚硫酸盐测定法，提高现行药典标准。方法：采用IonPac AS11-HC 阴离子分析柱并配加IonPac AG11-HC保护柱，柱温 25 ℃，以10.0 mmol·L-1的KOH作为淋洗液，流速1.0 mL·min-1，检测器为电导检测器，检测器温度30 ℃，抑制器为自动再生抑制模式，抑制电流40 mA，进样量 25 μL。结果：离子色谱法测定亚硫酸钠质量浓度在1~20 μg·mL-1范围内线性良好， 回归方程为Y=0.0434X-0.0211，r=0.9993，精密度RSD为0.5%，稳定性RSD为1.5%，回收率范围为 93.5%~99.3%，检出限0.1 μg·mL-1，定量限0.25 μg·mL-1。8批样品中1号、2号、3号及5号样品结果分别为8.1、9.8、12. 0及10.4 μg·g-1，其余各批样品均为未检出亚硫酸盐。结论：所建方法可行、准确，可用于测定蔗糖中亚硫酸盐的含量。 |
| 英文摘要: |
| Objective: To establish a suitable method for the determination of sulfite in sucrose and improve the standard of current pharmacopoeia. Methods: IonPac AS11-HC anion analysis column and IonPac AG11-HC protection column were used. The column temperature was 25 ℃, and 10.0 mmol·L−1 KOH was used as the eluent. The flow rate was 1.0 mL·min−1. The detector was a conductivity one and the detector temperature was 30 ℃. The suppressor was an automatic regeneration inhibition mode. The inhibition current was 40 mA, and the injection volume was 25 μL. Results: The determination of sulfite concentration by ion chromatography showed good linearity in the range of 1-20 μg·mL-1. The regression equation was Y=0.0434X-0.0211, r=0.9993. The RSD of precision was 0.5%, and the RSD of stability was 1.5%, and the recovery was 93.5%-99.3%. The limit of detection was 0.1 μg·mL-1 and the limit of quantitation was 0.25 μg·mL-1. The results of No. 1, No. 2, No. 3 and No. 5 samples were 8.1, 9.8, 12.0 and 10.4 μg·g−1, respectively. No sulfite was detected in the other batches of samples. Conclusion: This method is feasible and accurate, which can be used to determine sulfite content in sucrose. |
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