褐藻胶硫酸酯中甲酰胺残留溶剂的含量测定

Determination of residual formamide content in alginate sulfate

目的建立1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×0.25μm;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:1.0μL;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。

Objective To establish a method for the content determination of residual formamide in alginate sulfate.Methods Gas chromatography-mass spectrometry(GC-MS)was applied as the detection and analysis method,column:VF-WAXms capillary column,size:30 m×0.25 mm×0.25μm;inlet-temperature:250℃;temperature programming:initial temperature 50℃,retention time 2 min,increase to 200℃at 30℃/min for 5 min;interface temperature:280℃;carrier gas:helium,purity≥99.999%,flow rate:1 mL/min;sample mode:splitless injection;injection volume:1.0μL;ion source:EI;measurement mode:selective ion monitoring(SIM),qualitative ion(m/z):45,44,29,quantitative ion(m/z):45.Results 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 was simple,sensitive and had good peak separation.The method was proved to be accurate,stable and reliable by methodology validation.It could be used for the determination of residual formamide in alginate sulfate.