离子色谱法测定生鲜牛奶中硫氰酸钠前处理方法的研究

Study on pretreatment methods of sodium thiocyanate in raw milk by ion chromatography

【目的】探寻低毒、安全的前处理试剂以及性价比高的固相萃取小柱,为优化检测生鲜牛奶中硫氰酸钠含量方法提供依据。【方法】以生鲜牛奶为原料,在《MRT/B 8-2016生乳中硫氰酸根的测定离子色谱法》基础上建立并采取不同的蛋白质沉淀剂及固相萃取小柱,对离子色谱法检测生鲜牛奶中硫氰酸钠含量的影响,从而优选出最佳的净化提取方法。【结果】采用有机溶剂法能快速沉淀生鲜牛奶中的蛋白质,乙醇在对比实验中净化效果好沉淀效果佳,回收率为96. 1%,且毒性低,试剂安全;HLB固相色谱小柱为最佳前处理净化小柱,回收率为93. 5%。【结论】采用乙醇作为蛋白质沉淀剂及HLB固相萃取小柱作为生鲜牛奶中测定硫氰酸钠的前处理方法,操作简单,性价比高,试剂安全低毒。

【Objective】 To study the low-toxicity, safe pre-treatment reagent and the high cost-effective solid-phase extraction column, and provide the basis for optimizing the method of detecting sodium thiocyanate in raw milk. 【Method】 Using fresh milk as raw material, the content of sodium thiocyanate in fresh/B 8-2016 by ion chromatography. And thus the best purification and extraction method is preferred. 【Result】The protein in fresh milk can be precipitated quickly by organic solvent method. Ethanol has good precipitation effect, the recovery is 96. 1%, and the toxicity is low and the reagent is safe. HLB solid phase chromatography column is the best pretreatment purification column, the recovery is 93. 5%. 【Conclusion】Ethanol is used as a protein precipitant and an HLB solid-phase extraction small column as a pretreatment method for the determination of sodium thiocyanate in raw milk. The method has the advantages of simple operation, high cost performance and low toxicity of the reagent.