用于乳制品中三聚氰胺含量测定的固相萃取富集流动注射紫外光度法  

A flow-injection solid phase extraction-separation ultraviolet photometry for automatic determination of melamine content in dairy products

作　　者：侯彦秋[1] 李永生[1] 

机构地区：[1]四川大学化学工程学院,成都610065

出　　处：《分析试验室》2013年第8期98-102,共5页Chinese Journal of Analysis Laboratory

摘　　要：给出了一种新的流动注射在线自动固相萃取富集紫外光度分析方法和系统。对该系统相关的各种影响因素,如三聚氰胺溶液酸度、三聚氰胺紫外吸收光谱、柱洗脱-采样时间、样品定量环体积、系统流量、载流种类、沉淀剂、离心转速、共存离子干扰等影响因素进行了优选和考察;在最优条件下,成功测定了多种乳制品中的三聚氰胺含量,回收率在94.2%～105.4%范围内;分析范围为0.1～3.0 mg/L(r=0.9983),相对标准偏差小于3.6%,检出限为0.1 mg/L,每小时可自动处理15个样品左右。无需与高效液相色谱联用,实现了样品萃取、富集、杂质清洗、分离、样品洗脱、样品定量注入及测定过程的自动完成。The paper proposed a flow-injection solid phase extraction-separation ultraviolet photometry（FI-SPESUV） and a system.In the research,various effecting factors on the FI-SPES-UV system were optimized and investigated,including the acidity and absorption spectrum of melamine,elution and sampling times of the extraction column,volume of the sampling loop,flow rate of the system,kinds of the carriers,precipitation agents and centrifugal speed for the sample,interference of coexist ions,etc.Under the optimized conditions,the contents of melamine in varied dairy products have been determined successfully,and the obtained recoveries were 96.4% ～ 104.8%.The determination range of the system is 0.5 ～ 15 mg / L（r = 0.9989）,the relative standard deviation is less than 3.6%,and the detection limit is 0.1 mg / L;it can be analyzed automatically about 15 samples per hour.Merits of the FI-SPES-UV system are that the extracting,cleaning,separating and eluting,injecting and determining of the samples can be realized automatically without coupling with high performance liquid chromatographic analyzer.

关 键 词：流动注射 三聚氰胺 固相萃取 紫外光度法 乳制品 

分 类 号：O657.3[理学—分析化学]