Hunter R T
J Assoc Off Anal Chem. 1986 May-Jun;69(3):493-5.
The method chosen for this collaborative study is a modification of the AOAC method for As residues, 41.009-41.012. The tissue is dry-ashed overnight at 500 degrees C, and then dissolved in dilute HCl. The solution is diluted and an aliquot is reacted with zinc metal to evolve arsine gas. The gas is trapped in AgDDC solution and As is quantitated at 540 nm. Nine collaborating laboratories performed single analyses on 4 blind duplicate pairs of bovine liver samples which were spiked at 0, 4.3, 10.8, or 21.6 mg As/kg liver. A National Bureau of Standards control (SRM 1566 Oyster Tissue, 13.4 +/- 1.9 mg As/kg) and a 1000 mg As/L standard were also submitted to the collaborators. Intralaboratory coefficients of variation ranged from 7.7 to 17.8%; interlaboratory coefficients of variation ranged from 10.9 to 19.0%. The method has been adopted official first action.
本次合作研究选用的方法是对AOAC测定砷残留量的方法(41.009 - 41.012)的改进。将组织在500摄氏度下干灰化过夜,然后溶解于稀盐酸中。将溶液稀释,取一份等分试样与锌金属反应以释放出砷化氢气体。该气体被捕获在二乙基二硫代氨基甲酸银(AgDDC)溶液中,并在540纳米处对砷进行定量。九个合作实验室对4对加标量分别为0、4.3、10.8或21.6毫克砷/千克肝脏的牛肝盲样重复样品进行了单次分析。还向合作实验室提交了国家标准局的对照品(标准参考物质1566牡蛎组织,13.4±1.9毫克砷/千克)和1000毫克砷/升的标准品。实验室内变异系数范围为7.7%至17.8%;实验室间变异系数范围为10.9%至19.0%。该方法已被正式首次采用。