高效液相色谱-电感耦合等离子体质谱联用技术测定畜禽肉制品中八种砷形态化合物

Determination of Eight Arsenic Species Compounds in Livestock and Poultry Meat Products by HPLC-ICP-MS

  • 摘要: 建立了畜禽肉制品中三价砷As(Ⅲ)、一甲基砷(MMA)、二甲基砷(DMA)、五价砷As(Ⅴ)、阿散酸(p-ASA)、 洛克沙砷(ROX)、4-羟基苯砷酸(4-HPAA)和4-硝基苯砷酸(4-NPAA)等砷形态化合物的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。以甲醇-水(1∶1,V/V)作为提取剂,采用超声水浴对样品进行前处理,选取Dionex IonPac AS14 阴离子交换柱作为分析柱,50 mmol/L (NH4)2HPO4(pH 7.3)为流动相,对畜禽肉制品中的砷形态化合物进行分析测定。结果表明,8种砷形态化合物的线性范围为1~300 μg/L,相关系数(R2)均大于0.999,检出限为0.1~0.5 μg/L。以精密度考察方法重现性,相对标准偏差(RSD)均小于5%,方法加标回收率在80.8%~105.7%之间。通过对实际样品的分析测定,发现在畜禽肉制品中的有机砷制剂主要为三价砷阿散酸和洛克沙砷,另外还有一种未知的砷化合物,有待进一步研究确认。

     

    Abstract: As (Ⅲ), MMA, DMA, As (Ⅴ), p-ASA, ROX, 4-HPAA and 4-NPAA in livestock and poultry meat products were determined by high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS). Ultrasonic water bath was used to pretreat the samples with methanolwater (1∶1, V/V) as extraction agent. Dionex IonPac AS14 anion exchange column was used as analytical column, 50 mmol/L (NH4)2HPO4 (pH 7.3) was used as mobile phase, and the method was used to detect arsenic species compounds in livestock and poultry meat products. The results show that the linear range of eight arsenic compounds is 1 300 μg/L, the correlation coefficient (R2) is greater than 0.999, the detection limit is 0.1-0.5 μg/L. The reproducibility of this method was inspected by precision, RSD is less than 5%, the recovery is between 80.8% and 105.7%. Through the analysis of actual samples, As (Ⅲ), p-ASA and ROX are checked out in livestock and poultry meat products, and an unknown arsenic compounds is also checked out.

     

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