| 刘欢,王世欣,许美杰,等.褐藻胶硫酸酯中甲酰胺残留溶剂的含量测定[J].中国海洋药物,2020,39(3):46-50. |
| 褐藻胶硫酸酯中甲酰胺残留溶剂的含量测定 |
| Determination of residual formamide in alginate sulfate |
| 投稿时间：2019-10-11 修订日期：2019-12-18 |
| DOI： |
| 中文关键词: 褐藻胶硫酸酯 气相色谱-质谱联用 甲酰胺 |
| English Keywords:Alginate sulfate Gas chromatography-mass spectrometry Formamide |
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| 中文摘要: |
| 建立一种褐藻胶硫酸酯中甲酰胺残留溶剂含量的检测方法。方法：采用气相色谱-质谱（GC-MS）联用的检测分析方法，色谱柱：VF-WAXms毛细管色谱柱，规格：30 m×0.25 mm×0.25 μm；进样口温度：250 ℃；柱温：初始温度50 ℃，维持2 min，以30 ℃/min速率升至200 ℃，维持5 min；接口温度：280 ℃；载气：氦气，纯度≥99.999%，流速：1 mL/min；进样方式：不分流进样；进样量：1.0 μL；离子源：EI；测定模式：选择离子扫描（SIM），定性离子（m/z）：45、44、29，定量离子（m/z）：45。结果：对照品中甲酰胺与溶剂峰分离良好，供试品溶液中均有甲酰胺检出。结论：该方法操作简便、灵敏，峰分离情况良好，经方法学验证该方法准确、稳定、可靠，可用于褐藻胶硫酸酯中甲酰胺溶剂残留含量的测定。 |
| English Summary: |
| Establish a method for the content determination of residual formamide in alginate sulfate. Methods Gas chromatography-mass spectrometry (GC-MS) as the detection and analysis method, column: VF-WAXms capillary column, size: 30 m × 0.25 mm × 0.25 μm; inlet-temperature: 250 oC; Temperature programming: initial temperature 50 oC, retention time 2 min, increase to 200 oC at 30 oC /min for 5 min; interface temperature: 280 oC; carrier gas: helium, purity ≥99.999%, flow rate: 1 mL/min; Sample mode: splitless injection; injection volume: 1.0 μL; ion source: EI; measurement mode: selective ion monitoring (SIM), qualitative ion (m/z): 45, 44, 29, quantitative ion (m/z): 45. Result The separation of formamide and solvent peaks was good in the reference substance, and the formamide was detected in the test sample solutions. Conclusion The GC-MS method is simple, sensitive and has good peak separation. The method is proved to be accurate, stable and reliable by methodology validation. It can be used for the determination of residual formamide in alginate sulfate. |
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