高效液相色谱-紫外法检测酱油中的3-氯-1,2-丙二醇
Quantitatively determining hazardous 3-chloro-1,2-propanediol in soy sauce with high performance liquid chromatography-ultraviolet method

建立了一种新的高效液相色谱-紫外法（HPLC-UV）测定酱油中的有害物质3-氯-1,2-丙二醇（3-chloro-1,2-propanediol,3-MCPD）含量的方法。首先将3-MCPD与叠氮化钠反应，所得到的叠氮化产物进一步和苯乙炔发生CuAAC 型点击反应，所得衍生物3-(4-苯基-1,2,3-三氮唑基)-1,2-丙二醇最后采用HPLC-UV进行分析检测。本检测方法对3-MCPD的检出限和定量限分别为0.1和0.3 μg/mL，且线性关系良好（r2=0.999）。对酱油样品进行加标回收实验，结果表明本方法的加标回收率为98.63%~100.17%，相对标准偏差（RSD值）为1.95%~4.74%。将本检测方法与国家标准检测方法GB 5009.191―2016进行对比检测，结果显示2种方法所得到的结果是一致的。
A novel high performance liquid chromatography-ultraviolet method (HPLC-UV) was developed for quantitatively determining the content of hazardous 3-chloro-1,2-propanediol (3-MCPD) in soy sauce.3-MCPD was first azidated with sodium azide,and the obtained azide product was further subjected to a CuAAC type click reaction with phenylacetylene,and the resulting derivative 3-(4-phenyl-1H-1,2,3 -triazol-1-yl) propane-1,2-diol (3-PTPD) was obtained and analyzed with HPLC-UV finally.The detection limits and quantitation limits of 3-MCPD were 0.1 and 0.3 μg/mL,respectively,and the linear relationship was good (r2=0.999).The results of spiked recovery test of soy sauce samples showed that the recoveries of the method were from 98.63% to 100.17%,and the relative standard deviation (RSD value) was from 1.95% to 4.74%.This method is compared with the national standard test method GB 5009.191―2016 as well,and the results obtained by the two methods are consistent.