微波消解-FAAS测定虾肉中钙的质量分数
Determination of calcium content in prawn meat using microwave digestion-flame atomic absorption spectrometry
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摘要: 采用微波消解-火焰原子吸收光谱法(flame atomic absorption spectrometry, FAAS)测定虾肉中钙(Ca)元素的质量分数, 对微波消解前处理的条件进行了研究。试验结果显示, 最佳的微波消解体系为取样量0.500 g, 以硝酸(HNO3)作为消解溶剂, 用量5.0 mL, 最适微波消解程序为多步消解程序D, 包含3个步骤: 1)功率400 W, 比例100%, 升温5 min, 消解温度120 ℃, 保持5 min; 2)功率800 W, 比例100%, 升温5 min, 消解温度150 ℃, 保持10 min; 3)功率800 W, 比例100%, 升温10 min, 消解温度180 ℃, 保持10 min。样品消解液在常温或冷藏条件下保存48 h之内的稳定性良好。经微波消解前处理后虾肉样品中w(Ca)的相对标准偏差(relative standard deviation, RSD)为5.284%, 加标回收率为91%~98%。微波消解-FAAS测定虾肉中的w(Ca)具有样品处理时间短、试剂用量少、结果准确和安全性高等优点。Abstract: The calcium content in prawn meat was determined by using microwave digestion-flame atomic absorption spectrometry (FAAS), and the optimal conditions of microwave digestion and FAAS program were studied. The results show that the optimal amount of digestion reagent HNO3 is 5.0 mL when the sampling amount of prawn meat is 0.500 g. The optimal microwave digestion program for calcium determination in prawn meat is multistep digestion process D, which includes 3 steps: 1) power 400 W, ratio 100%, heat-up time 5 min, digestion temperature 120 ℃ for 5 min; 2) power 800 W, ratio 100%, heat-up time 5 min, digestion temperature 150 ℃ for 10 min; 3) power 800 W, ratio 100%, heat-up time 10 min, and digestion temperature 180 ℃ for 10 min. The calcium content in microwave-digested solution remains stable within 48 h. Under those conditions, the relative standard deviation (RSD) of determination is 5.284%, and the recovery of calcium is 91%~98%. The microwave digestion-FAAS method is rapid, accurate, economical and safe in determining the calcium content in prawn meat.