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为建立一种方便、快速、准确、安全的面制品中铝含量的检测方法,采用微波消化对面制品进行前处理,用分光光度法测定面制品中的铝含量,建立微波消解-分光光度法测定面制品中铝的方法。结果表明,微波消解条件为微波功率1 000 W,爬坡时间15 min,持续时间30 min,冷却时间10 min,赶酸温度150℃时,消解易控制,所有样品消解完全;反应体系最大吸收波长为636 nm,最适pH值为5.5,缓冲液加入量为8 mL,显色时间为25 min。该方法准确度和灵敏度高、精密度好,在0~6μg内,呈良好的线性关系,相关系数R为0.999 6,样品的平均加标回收率为94%,RSD为1.53%;分光光度法检测面粉和月饼所得结果分别较ICP-MS检测结果高8.8%和10.3%。微波消解法有效缩短了前处理时间、减少了强酸给人体带来的损害,适合面制品中铝的测定。
In order to establish a convenient, rapid, accurate and safe method for the determination of aluminum in flour products, the products were pretreated by microwave digestion, the aluminum content in the flour product was determined by spectrophotometry and the determination by microwave digestion - spectrophotometry Aluminum products in the pasta method. The results showed that the microwave digestion conditions were microwave power of 1 000 W, climbing time of 15 min, duration of 30 min, cooling time of 10 min and horsepower temperature of 150 ℃. The digestion was easy to control and all samples were completely digested. The maximum absorption wavelength 636 nm, the optimum pH was 5.5, the amount of buffer added was 8 mL, and the color development time was 25 min. The method has the advantages of high accuracy and sensitivity, good precision, good linearity within 0 ~ 6μg, correlation coefficient R of 0.999 6, average recoveries of samples of 94% and RSD of 1.53%. Spectrophotometry The results of the detection of flour and mooncake were 8.8% and 10.3% higher than those of ICP-MS respectively. Microwave digestion effectively shorten the pre-treatment time, reducing the damage caused by strong acids to the human body, suitable for the determination of aluminum in flour products.