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本文将磁芯-硫脲壳聚糖作为固定相填充到自制的微柱中,采用流动注射在线分离富集与火焰原子吸收法联用对大米中痕量镉进行测定。pH=7.0的试液以3.9mL/min速率采样120s,以0.5mol/L HNO3-0.1mol/L硫脲作为洗脱液,用火焰原子吸收光谱法测定洗脱液中Cd2+,检测的线性范围为0.02~1.20μg/mL(r=0.9922),检出限(3σ)为2.5ng/mL,相对标准偏差(RSD)为0.79%(c=1.0μg/mL,n=7),加标回收率在96.0%~104.2%之间。
In this paper, the core-thiourea chitosan as a stationary phase was filled into a self-made microcolumn. The concentration of trace cadmium in rice was determined by flow injection on-line separation and enrichment combined with flame atomic absorption spectrometry. The solution of pH = 7.0 was sampled for 120s at a rate of 3.9mL / min and the concentration of Cd2 + in the eluate was determined by flame atomic absorption spectrometry with 0.5mol / L HNO3-0.1mol / L thiourea as the eluent. The linear range (RSD) was 0.79% (c = 1.0μg / mL, n = 7) with the detection limit (3σ) of 0.02 ng · mL-1.20 μg / Rates between 96.0% ~ 104.2%.