食用植物油中溶剂残留测定方法研究

目的:在顶空气相色谱法测定食用植物油中残留溶剂的基础上,对影响残留溶剂测定的条件进行研究。方法:在恒定环境中,在不同的变量参数下,运用顶空气相色谱法依次进样分析,对色谱柱温度、进样口温度及载气流速进行研究和优化。结果:顶空气相分析的灵敏度与色谱柱温度、进样口温度、载气流速所决定的气相提取效率有关;在一定温度范围内组分的塔板数随载气流速的增加呈规律性递增,适当提高载气流速有利于提高检测的灵敏度;色谱柱温度和进样口温度的变化对检测效率影响显著,应选取最佳条件。结论:通过实验得到优化的气相分析参数,色谱柱温度为150℃、进样口温度为140℃、载气流速为5 mL·min^-1、回收率为98.2%~99.6%、精确度为3.04%~5.20%。

Study on the Determination Method of Solvent Residue in Edible Vegetable Oil

Objective:Based on the determination of residual solvents in edible vegetable oil by headspace gas chromatography,to study the conditions that affect the determination of residual solvents.Method:In a constant environment,under different variable parameters,headspace gas chromatography was used to inject samples sequentially to study and optimize the column temperature,inlet temperature and carrier gas flow rate.Results:The sensitivity of the headspace phase analysis is related to the gas phase extraction efficiency determined by the column temperature,inlet temperature,and carrier gas flow rate;within a certain temperature range,the number of trays of the components increases regularly with the increase of carrier gas flow rate,appropriately increasing the carrier gas flow rate is beneficial to improve the detection sensitivity;the change of the chromatographic column temperature and the temperature of the injection port has a significant impact on the detection efficiency,and the best conditions should be selected.Conclusion:The optimized gas analysis parameters are obtained through experiments.The column temperature is 150℃,the inlet temperature is 140℃,the carrier gas flow rate is 5 mL·min^-1,the recovery rate is 98.2%~99.6%,and the accuracy is 3.04%~5.20%.