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

作　　者：吴倩 江洪[1] 马济美[1] 曾贞[1] WU Qian;JIANG Hong;MA Jimei;ZENG Zhen(College of Science,Huazhong Agricultural University,Wuhan 430070,China)

机构地区：[1]华中农业大学理学院,武汉430070

出　　处：《华中农业大学学报》2019年第3期97-103,共7页Journal of Huazhong Agricultural University

基　　金：国家自然科学基金项目(21502058)

摘　　要：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0.3μg/mL,且线性关系良好(r^2=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 0.3μg/mL,respectively,and the linear relationship was good(r^2=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.

关 键 词：酱油 3-氯-1 2-丙二醇 叠氮化 点击反应 高效液相色谱-紫外法 

分 类 号：TS212.7[轻工技术与工程—粮食、油脂及植物蛋白工程]