超声酸提取-液相色谱-原子荧光联用同时测定水生动植物中甲基汞和乙基汞  

Determination levels of methylmercury and ethyl mercury in aquatic animals and plants by ultrasonic acid extraction liquid chromatography-atomic fluorescence morphometry

作　　者：丁宇[1] 周睿[1] 敬海泉[2] 孙澄颖 凌志毅 DING Yu;ZHOU Rui;JING Haiquan;SUN Chengying;LING Zhiyi(Huangpu district center for the disease control&prevention,Shanghai 200023,China;Pudong district center for the disease control,Shanghai 200120,China)

机构地区：[1]上海市黄浦区疾病预防控制中心,上海200023 [2]上海市浦东新区疾病预防控制中心,上海200120

出　　处：《预防医学情报杂志》2023年第10期1220-1224,1229,共6页Journal of Preventive Medicine Information

基　　金：上海市黄浦区科委项目(项目编号:HLM202224)。

摘　　要：目的建立水生动植物食品中有机汞的液相色谱原子荧光联用检测方法(LC-AFS),以适于普通实验室对相关项目的检测。方法将水生动植物样品粉碎均匀,加入盐酸溶液,超声水浴提取。提取液高速低温离心,吸取上清液,调节pH值至3~7。加入L-半胱氨酸溶液作为络合剂,滤膜过滤,滤液进LC-AFS检测,标准曲线法定量。结果在1.0μg/L~50.0μg/L的范围内,甲基汞和乙基汞线性良好,相关系数分别为0.9997和0.9996,方法检出限(LOD)分别为7.43μg/kg和6.95μg/kg,方法定量限(LOQ)分别为24.51μg/kg和22.94μg/kg。以莲藕和草鱼基质进行加标实验,回收率在87.7%~97.8%之间。结论该方法线性范围宽,准确,可靠,适合于水生动植物食品中有机汞的检测。Objective To establish a method for determination levels of organic mercury in aquatic animal and plant food by using liquid chromatography atomic fluorescence(LC-AFS)to be suitable for the detection of related items in ordinary laboratories.Methods Samples of aquatic animals and plants were crushed evenly,and extracted by the hydrochloric acid solution and ultrasonic water bath.The extract was centrifuged at high speed and low temperature.Then,the supernatant was absorbed,and the pH value was adjusted to 3-7.Next,L-cysteine solution was added as the complexing agent.After filtrated by membrane,the filtrate was detected by LC-AFS,and quantified by using the standard curve method.Results The linear relationship of this method was good in the range of 1.0μg/L~50.0μg/L,and the correlation coefficients of methyl mercury and ethyl mercury were 0.9997 and 0.9996.The limits of detection(LOD)were7.43μg/kg and 6.95μg/kg,respectively.The limits of quantification(LOQ)were 24.51μg/kg and 22.94μg/kg,respectively.The recovery rate ranged from 87.7%to 97.8%.Conclusions The method has a wide linear range.It is accurate,reliable,and suitable for the determination of organic mercury in aquatic animal and plant foods.

关 键 词：超声酸提取 液相色谱-原子荧光联用 水生动植物 甲基汞 乙基汞 

分 类 号：R155.5[医药卫生—营养与食品卫生学]