气相色谱法测定香兰素衍生物VND中的残留溶剂

目的用毛细管气相色谱法建立VND中4种残留溶剂的测定方法。方法采用DB-Wax(30m×0.45mm,0.85μm)毛细管柱,载气为氮气,FID检测器。程序升温,柱温:起始温度为35℃,保持17min,然后以30℃/min的速率升至200℃,保持8min。进样口温度:200℃,检测器温度:250℃。分流直接进样,二甲基亚砜为溶剂,正丁醇为内标物,内标法测定残留溶剂的含量。结果在考察范围内呈良好的线性关系(甲醇r=0.9996,异丙醇r=0.9996,乙醇r=0.9995,N,N-二甲基甲酰胺r=0.9995),平均回收率为96%～103%,理论塔板数大于10000,相邻峰分离度均大于1.5,精密度、重复性的RSD均小于3%。结论本法简单、结果准确、重复性好,可同时检测VND中甲醇、异丙醇、乙醇、N,N-二甲基甲酰胺4种残留溶剂。

Determination of Residual Solvents in Vanillin Derivatives VND by Gas Chromatography

Objective A method for determining the four kinds of residual solvents in VND by capillary gas chromatography is established.Methods The capillary column was DB-Wax(30m×0.45mm,0.85μm)with an FID detector and nitrogen as carrier gas.The injector temperature and the detector temperature were controlled at 200°C,250°C,respectively.The column temperature program was initially 35°C(hold 17min) and was increased at the rate of 30°C/min to 200°C(hold 8min),the sample was dissolved in dimethylsulfoxide and N-butanol was used as the internal standard.The assay of residual solvents was calculated by internal standard method.Results A good linearity was observed at the experimental concentration(r= 0.9995~0.9996).The rate of recovery was in the range of 96%~103%.The number of theoretical plates exceeded 10000 and the resolutions between the adjacent peaks were more than 1.5.The RSD of precision and accuracy was less than 3%.Conclusion The method is simple,sensitive,accurate,and can be used for detection of four residual solvents in Vanillin derivatives.