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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。
A new method and system for on-line automated solid-phase extraction enrichment UV spectrophotometry by flow injection are presented. Influencing factors such as acidity of melamine solution, UV absorption spectrum of melamine, column elution-sampling time, sample loop volume, system flow, current-carrying type, precipitating agent, centrifugal speed and coexisting ion interference The optimum conditions were as follows: the melamine content of various dairy products was determined successfully under the optimum conditions, the recoveries ranged from 94.2% to 105.4%; the range of analysis was 0.1-3.0 mg / L (r = 0.9983) , The relative standard deviation is less than 3.6%, the detection limit is 0.1 mg / L, 15 samples can be processed automatically per hour. Without the need for high performance liquid chromatography, sample extraction, enrichment, impurity cleaning, separation, sample elution, sample injection, and auto-complete of the measurement process are achieved.