食品中总砷测定的3种前处理方法比较  

Comparison of three pretreatment methods for arsenic determination in food

作　　者：李慧[1] 洪全[1] 

机构地区：[1]宿迁市疾病预防控制中心,江苏宿迁223800

出　　处：《中国卫生检验杂志》2017年第24期3532-3533,3536,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的比较食品中总砷测定的3种前处理方法,为选择总砷测定样品前处理方法提供参考依据。方法采用微波消解、硝酸-高氯酸-硫酸消化法和干消化法分别处理芹菜、胡萝卜、黄豆、大米、鸡肉、紫菜、鱼粉、牡蛎8种标准物质,然后采用氢化物发生-原子荧光光度法测定。结果对于紫菜、鱼粉、牡蛎,用干消化法消解后检测得到满意结果,用微波消解和湿法消化测定的结果明显偏低。对于芹菜、胡萝卜、黄豆、大米、鸡肉等标准物质,用3种前处理方法消解样品测定的结果均在标准值范围内。其中微波消解法平行样结果误差最小,回收率最高(91.3%~98.2%),操作简单,消化时间短。结论干消化法消解过程中虽然有所损失,回收率低,平行样误差大,但用于含有大量有机砷的样品消解,其结果较满意。其他2种前处理方法处理后的样品结果明显偏低,因此不可用。Objective To provide reference for correctly selecting scientific pretreatment methods of total arsenic determination in different samples by comparison of three different pretreatment methods. Methods Using three pretreatment methods,including microwave digestion method,nitric acid-perchloric acid-sulfuric acid digestion method and dry digestion method,the standard materials including celery,carrot,soybean,rice,chicken,laver,fish meal and oyster were pretreated. And the total arsenic in sample solution was analyzed by hydride generation-atomic fluorescence spectrometry. Results The test values were satisfactory when dry digestion method was used to digest laver,fish meal and oyster samples. It is obvious that the test values were lower when micro-wave digestion method and wet digestion method were used to digest these samples. And the test values were all in the range of standard value by using the above-mentioned three pretreatment methods to digest celery,carrot,soybean,rice and chicken samples. Among the three pretreatment methods,the relative standard deviation（ RSD） of micro-wave digestion method was the least with the highest recovery rate of 91. 3%-98. 2%. Besides,the operation was simple and digestion time was also short. Conclusion There are some disadvantages of lower recovery rate and big parallel sample value tolerance in the dry digestion method,but when it was used for testing the sample materials with mass organic arsenic,the testing result will be satisfactory. If using the other two pretreatment methods to test the samples,the result value is obviously lower,so they are not capable.

关 键 词：微波消解法 湿消化法 干消化法 有机态砷 无机态砷 

分 类 号：R155.5[医药卫生—营养与食品卫生学]