为准确检测牛奶中重金属含量,采用微波消解-原子荧光法检测牛奶中的重金属元素砷和汞,通过单因素和正交实验,以加标回收率为指标优化其检测方法,并对方法进行验证和应用。[结果]表明,砷和汞的最佳检测条件为还原剂硫脲的浓度为50 g/L、硼氢化钾-氢氧化钾的浓度15 g/L,氨基磺酸的添加量为2.5 mL,硝酸的添加量为5 mL、微波消解温度为195℃。砷和汞的检出限分别为0.01 mg/kg、0.003 mg/kg;标准曲线方程线性范围分别为0~10 ng/mL、0~1 ng/mL,相关系数分别为0.997、0.992;砷和汞的加标回收和质控样本的检测数据重现性RSD分别为0.11、0.18、3.82、4.29,精密度分别为0.59、0.56、3.28、4.32;一个季度砷、汞加标回收率和质控样本共检测48次,回收率分别为98.84%、99.23%,RSD为1.01、1.91。质控样本检测值偏差符合实验要求,RSD为2.79~3.80。回收率和质控值偏差均符合国家标准要求。成功建立同时检测砷和汞的便捷、准确灵敏的原子荧光检测方法,为监管食品受重金属污染奠定基础。
毕成名, 卢智华, 李艳红, 齐琦, 秦晓婷, 王英南, 李洪梅, 王斌, 白晓玲, 伊德润
. 微波消解-原子荧光法检测液奶中砷和汞样品前处理方法探究及应用[J]. 中国乳业, 2023
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DOI: 10.12377/1671-4393.23.11.12
In order toaccurately detect heavy metals in milk,microwave digestion-atomic fluorescence method was used to detect heavy metal elements arsenic and mercury in milk,and its detection method was optimized by one-way and orthogonal experiments with spiked recovery as the index.The method was also validated and applied. The results showed that the optimal conditions for the determination of arsenic and mercury were 50 g/L for thiourea,15 g/L for potassium borohydride-potassium hydroxide,2.5 mL of sulfamic acid,5 mL of nitric acid, and 195 ℃ for microwave digestion.The detection limits of arsenic and mercury were 0.01 mg/kg and 0.003 mg/kg,respectively;the linear ranges of the standard curve equations were 0-10 ng/mL and 0-1 ng/mL,with the correlation coefficients of 0.997 and 0.992,respectively;the RSDs of the spiked recoveries of arsenic and mercury and the reproducibility of the detection data of the quality control samples were 0.11,0.18,3.82 and 4.29,respectively.Precision was 0.59,0.56,3.28,4.32,respectively;a quarter of arsenic and mercury spiked recovery and quality control samples were tested 48 times,the recovery rate was 98.84%,99.23%,RSD was 1.01,1.91,respectively.the deviation of the detection value of the quality control samples complied with the experimental requirements,and the RSD was 2.79-3.80.the recovery rate and the deviation of the quality control value were in accordance with the national standards.Requirements.A convenient,accurate and sensitive atomic fluorescence detection method for the simultaneous detection of arsenic and mercury has been successfully established,which lays the foundation for the supervision of food contamination by heavy metals.
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