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[目的]建立亲水作用色谱-紫外检测器测定氰胺基甲酸甲酯中残留单氰胺和双氰胺的分析方法,为合成工艺优化和产品质量分析提供支撑。[方法]采用HILIC亲水作用色谱柱,以甲醇-10 mmol/L磷酸氢二钠溶液(体积比5∶95,高氯酸调节p H值3.0)为流动相,等度洗脱,流速为0.8 m L/min,检测波长210 nm。[结果]单氰胺在20~200 mg/kg范围呈良好线性,检出限为8 mg/kg,定量限为25 mg/kg,线性相关系数为0.9985;双氰胺在1~200 mg/kg范围呈良好线性,检出限为0.1 mg/kg,定量限为0.3 mg/kg,线性相关系数为0.9996;氰胺基甲酸甲酯在1~200 mg/kg范围呈良好线性,检出限为0.3 mg/kg,定量限为0.9 mg/kg,线性相关系数为0.9992。[结论]该方法简便、灵敏度高、重现性好,可用于氰胺基甲酸甲酯中残留单氰胺和双氰胺的同时测定。
[Objective] To establish a method for the determination of residual cyanamide and dicyandiamide residues in methyl cyanamidate by hydrophilic interaction chromatography-UV detector, which provided support for the synthesis process optimization and product quality analysis. [Method] HILIC hydrophilic interaction column was used to elute isocratic eluate with a mobile phase of methanol-10 mmol / L sodium phosphate dibasic solution (volume ratio 5:95, pH = 3.0 with perchloric acid) 0.8 m L / min, detection wavelength 210 nm. [Results] Cyanamid showed a good linearity in the range of 20-200 mg / kg with a detection limit of 8 mg / kg, a limit of quantification of 25 mg / kg and a linear correlation coefficient of 0.9985. kg in the range of 1 ~ 200 mg / kg, the detection limit was 0.1 mg / kg, the limit of quantification was 0.3 mg / kg, and the linear correlation coefficient was 0.9996. The detection limit 0.3 mg / kg, the limit of quantification was 0.9 mg / kg and the linear correlation coefficient was 0.9992. [Conclusion] The method is simple, sensitive and reproducible. It can be used for simultaneous determination of residual cyanamide and dicyandiamide in methyl cyanatomethyl ester.