液相色谱-原子荧光联用技术检测海产品中形态砷  

Detection of arsenic species in seafood using liquid chromatography-atomic fluorescence spectrometry

作　　者：方素珍[1,2] 林美霞 谢维平 陈林刚[1,2] 苏碧玲 汤炜涛[1,2] FANG Su-zhen;LIN Mei-xia;XIE Wei-ping;CHEN Lin-gang;SU Bi-ling;TANG Wei-tao(Department of Physics and Chemistry,Quanzhou Center for Disease Control and Prevention,Quanzhou,Fujian,362000,China;不详)

机构地区：[1]泉州市疾病预防控制中心理化科,福建泉州362000 [2]福建医科大学附属泉州疾病预防控制中心,福建泉州362000 [3]福建医科大学公共卫生学院

出　　处：《现代预防医学》2024年第23期4367-4372,共6页Modern Preventive Medicine

基　　金：泉州市科技项目(2023NS077)。

摘　　要：目的 建立液相色谱-原子荧光联用技术(LC-AFS)检测海产品中As(Ⅲ)、DMA、MMA、As(Ⅴ)四种形态砷的方法。方法 优化检测条件,包括载流的类型及浓度、硼氢化钾浓度、灯电流、负高压、流动相浓度及pH等,考察所建立检测方法的参数,包括线性范围、准确度、精密度、检出限等。结果 在5%盐酸、5 g/L氢氧化钠-20 g/L硼氢化钾、负高压270 V、灯主电流60 mA、流动相A为磷酸二氢铵(1 mmol/L,pH 8.5)、流动相B为磷酸二氢铵(25 mmol/L,pH 8.0)的条件下,As(Ⅲ)、DMA、MMA、As(Ⅴ)线性范围为0~100μg/L,相关系数均大于0.999;保留时间RSD为0.2%~1.2%,峰面积RSD为2.1%~4.4%;样品加标回收率为81.2%~111.6%。结论 方法灵敏度高、准确性好、精密度高,分析时间短,检测效率高,试剂用量少,结果满意。Objective To establish a method for detecting four arsenic species—As(III),DMA,MMA,and as(V)—in seafood using liquid chromatography-atomic fluorescence spectrometry(LC-AFS).Methods The detection conditions were optimized,including the type and concentration of the carrier liquid,concentration of potassium borohydride,lamp current,negative high voltage,mobile phase concentration,and pH.Parameters of the established detection method were evaluated,including linear range,accuracy,precision,and detection limit.Results Under the conditions of 5%hydrochloric acid,5 g/L sodium hydroxide-20 g/L potassium borohydride,a negative high voltage of 270 V,lamp main current of 60 mA,mobile phase A as ammonium dihydrogen phosphate(1 mmol/L,pH 8.5),and mobile phase B as ammonium dihydrogen phosphate(25 mmol/L,pH 8.0),the linear range for As(III),DMA,MMA,and As(V)was 0-100μg/L,with correlation coefficients exceeding 0.999.The relative standard deviation(RSD)for retention time ranged from 0.2%to 1.2%,while the RSD for peak area ranged from 2.1%to 4.4%.The recovery rate for spiked samples was between 81.2%and 111.6%.Conclusion The method demonstrates high sensitivity,accuracy,and precision,with a short analysis time and high detection efficiency,while requiring minimal reagent usage,yielding satisfactory results.

关 键 词：海产品 形态砷分析 液相色谱-原子荧光联用技术 

分 类 号：O657.72[理学—分析化学]