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目的建立超声辅助溶剂萃取——直接测汞法测定海产品中甲基汞的检测方法,应用此方法检测黄鱼、鳕鱼、金枪鱼、扇贝、杂色蛤等海产品中甲基汞的含量。方法选择盐酸为萃取溶剂,通过优化萃取溶剂的浓度和提取条件,选择5 mol/L盐酸作为溶剂,超声1 h,以二氯甲烷分两次萃取,再以水反萃取,应用测汞仪直接测定水相中甲基汞的含量。结果甲基汞标准曲线的线性相关系数大于0.997,检出限为0.75 ng/g。不同类型生物标准参考物质实际测定值与标准参考值相符,测定值的相对标准偏差小于4%。结论该方法操作简便、快速、准确,适用于鱼、贝类海产品中甲基汞的快速萃取分离和测定。不同种类样品中甲基汞污染程度不同,实验选取的样品中甲基汞的含量均未超过卫生限量,鳕鱼、金枪鱼中甲基汞含量较高。
OBJECTIVE To establish a method for the determination of methylmercury in seafood by ultrasonic assisted solvent extraction - direct mercury determination. The method was used to detect methylmercury in seafood such as yellow croaker, cod, tuna, scallop and variegated clams. Methods Hydrochloric acid was selected as the extraction solvent. The optimal extraction solvent concentration and extraction conditions were selected by using 5 mol / L hydrochloric acid as the solvent, sonicated for 1 h, extracted twice with dichloromethane, and then extracted by water. Determination of methylmercury content in aqueous phase. Results The linear correlation coefficient of methylmercury standard curve was greater than 0.997 with a detection limit of 0.75 ng / g. The actual measured values of different types of biological reference materials are in accordance with the standard reference values, and the relative standard deviations of the measured values are less than 4%. Conclusion The method is simple, rapid and accurate and is suitable for the rapid extraction, separation and determination of methylmercury in fish and shellfish products. Different levels of methylmercury contaminants in different samples, the experiment selected samples of methylmercury content did not exceed the health limit, cod, tuna higher methylmercury content.