期刊论文

Optimization of the method for determination of 3-chloro-1,2-propanediol by adenine pre-column derivatization-HPLC-FLD

中文

中国油脂

1003-7969

2020

45

8

130-137

10.12166/j.zgyz.1003-7969/2020.08.026

湖北省粮食科技创新项目 大宗粮油精深加工教育部重点实验室(武汉轻工大学)开放课题(2018JYBQGDKFA02) 国家自然科学基金项目(31371783)。

本校为第一机构

3-氯-1,2-丙二醇（3-MCPD）经高碘酸钠溶液氧化裂解、腺嘌呤衍生化后的产物——1,N6-亚乙烯基腺嘌呤（ε-Ade）为强荧光物质,通过对其荧光光谱与重要影响因素进行研究与优化,结合测定体系背景干扰的抑制,对高效液相色谱-荧光法（HPLC-FLD）测定3-MCPD水溶液的条件进行了优化。得到优化条件为:使用耐碱性反相C18色谱柱进行测定,流动相中甲醇体积分数为20%,水相为pH 9.0的碳酸钠-碳酸氢钠缓冲液。食用油中3-MCPD的测定需以0.01 g/mL的NaCl溶液作为萃取水相,氧化裂解3-MCPD的高碘酸钠可采用等量的亚硫酸钠还原、1.1倍量的醋酸铅沉淀予以去除,从而抑制空白峰的干扰,将该方法应用于多种食用植物油样品...

The 3-chloro-1,2-propanediol(3-MCPD) was oxidatively cleaved with sodium periodate solution and then derivatized with adenine to produce a strong fluorescent substance of 1, N6-vinylidene adenine(ε-Ade). According to the study of the product’s fluorescence spectrum and the optimization of important influencing factors, the determination conditions of 3-MCPD by high performance liquid chromatography-fluorescence detection(HPLC-FLD) method was optimized after the suppression of the background interference of the measurement system. The optimal ...