高效液相色谱-碰撞/反应池-电感耦合等离子体质谱测定贝类中砷形态化合物及健康风险评估
Accurate Determination of Arsenic Speciation in Shellfish by High Performance Liquid Chromatography Coupled with Collision/Reaction Cell Inductively Coupled Plasma Mass Spectrometry and Health Risk Assessment
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摘要: 本研究以九种青岛市售贝类样品为研究对象,并且通过高效液相色谱-碰撞/反应池-电感耦合等离子体质谱(HPLC-CRC-ICP-MS)测定总砷及砷形态化合物的含量,并对其食用安全性做出客观评价。样品采用超声提取(0.15 mol/L HNO3),优化后的色谱条件(50 mmol/L(NH4)2CO3,pH=9.5)进行色谱分离,并采用碰撞/反应池中O2反应模式进行检测。6种砷形态化合物的线性回归方程相关系数均在0.999以上,检出限为0.009~0.028 μg/L,相对标准偏差在3.6%~8.3%之间,加标回收率在91.2%~106.2%。实验表明,青岛市售贝类样品中的砷元素主要以无毒性的AsB的形式存在,无机砷含量符合国标限量要求。Abstract: This study aimed at developing an accurate method for determining the levels of total arsenic and arsenic species in edible species of shellfish using high performance liquid chromatography coupled with collision/reaction cell inductively coupled plasma mass spectrometry to assess the healthy risk objectively. The shellfish samples were extracted using ultrasonic bath extraction(0.15 mol/L HNO3),separated under the optimized chromatographic conditions(50 mmol/L(NH4)2CO3,pH=9.5)and determined with O2 mass-shift mode. Good linearities of six arsenic species were observed with correlation coefficients above 0.999.Limits of detection were between 0.009~0.028 μg/L. Relative standard deviation were within 3.6%~8.3% and recoveries were between 91.2%~106.2%. The results showed that AsB was the predominant as species in the shellfish samples of Qingdao City and inorganic arsenic contents meets the international limit.