中国乳业 ›› 2023, Vol. 0 ›› Issue (11): 60-68.doi: 10.12377/1671-4393.23.11.12

• 质量安全 • 上一篇    下一篇

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

毕成名1, 卢智华1, 李艳红1,*, 齐琦1, 秦晓婷1, 王英南1, 李洪梅1, 王斌1, 白晓玲2, 伊德润2   

  1. 1 蒙牛乳业（唐山）有限责任公司,河北唐山 064000;
    2 蒙牛乳业常温事业部,内蒙古呼和浩特 011500
  • 出版日期:2023-11-25 发布日期:2023-12-12
  • 通讯作者: *李艳红（1984-）,女,内蒙古赤峰人,本科,初级工程师,研究方向为食品检验。
  • 作者简介:毕成名（1998-）,男,河北秦皇岛人,硕士,研究方向为食品加工与安全;卢智华（1983-）,女,内蒙古赤峰人,硕士,中级工程师,研究方向为食品检验;齐 琦（1999-）,女,河北唐山人,本科,研究方向为食品检验;秦晓婷（1984-）,女,河北唐山人,本科,初级工程师,研究方向为食品检验;王英南（1990-）,男,河北唐山人,本科,研究方向为食品加工与安全;李洪梅（1982-）,女,内蒙古赤峰人,本科,研究方向为食品检验;王 斌（1982-）,男,陕西榆林人,本科,研究方向为食品加工与安全;白晓玲（1984-）,女,内蒙古扎兰屯人,研究生在读,食品药品工程中级工程师,研究方向为食品检验;伊德润（1977-）,男,内蒙古兴安盟人,本科,检乳品检测助理工程师,研究方向为食品检验。

Microwave digestion-atomic fluorescence for thedetermination of arsenic and mercury in liquid milk and its application

BI Chengming1, LU Zhihua1, LI Yanhong1,*, QI Qi1, QIN Xiaoting1, WANG Yingnan1, LI Hongmei1, WANG Bin1, BAI Xiaoling2, YI Derun2   

  1. 1Mengniu Dairy (Tangshan) Limited Liability Company,Tangshan Hebei 064000;
    2Mengniu Dairy Room Temperature Division,Hohhot Neimenggu 011500
  • Online:2023-11-25 Published:2023-12-12

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摘要： 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。

关键词: 原子荧光, 微波消解, 牛奶, 重金属元素

Abstract: 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.

Key words: atomic fluorescence, microwave digestion, milk, heavy metal elements

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