水样中铅和镉磁性固相萃取测定法

职业与健康 ›› 2023, Vol. 39 ›› Issue (15): 2026-2029.

水样中铅和镉磁性固相萃取测定法

王露, 吴珺玮, 宋鑫, 冯晓青, 杨鹏飞, 张敏会

淮安市疾病预防控制中心检验科,江苏淮安 223001

收稿日期:2023-01-19 修回日期:2023-02-20 发布日期:2026-03-24
通信作者: 张敏会,副主任技师,E-mail：511247939@qq.com
作者简介:王露,女,高级工程师,主要从事卫生检验工作。
基金资助:
淮安市科技计划（指导性）项目（HABZ201732）; 淮安市突发公共卫生事件应急检测重点实验室（HAP201906）; 淮安市“天医星”医学检验重点实验室（HAP202004）; 淮安市突发公共卫生事件应急检测重点实验室培优课题项目（ETPHI-P-14）

Determination of lead and cadmium in water samples by magnetic solid-phase extraction

WANG Lu, WU Junwei, SONG Xin, FENG Xiaoqing, YANG Pengfei, ZHANG Minhui

Laboratory Department,Huaian Center for Disease Control and Prevention,Huaian Jiangsu 223001,China

Received:2023-01-19 Revised:2023-02-20 Published:2026-03-24
Contact: ZHANG Minhui,Deputy chief technician,E-mail：511247939@qq.com

摘要/Abstract

摘要： 目的以乙二胺四乙酸（ethylene diamine tetraacetic acid,EDTA）修饰的β-环糊精（cyclodextrin,CD）-壳聚糖（chitosan,CS）/四氧化三铁Fe₃O₄（CDCS/Fe₃O₄-EDTA）为磁性固相萃取吸附剂,建立了磁性固相萃取-电感耦合等离子体质谱法（inductively coupled plasma mass spectrometry,ICP-MS）同时测定水样中铅和镉的分析方法。方法样品pH值、萃取时间、吸附剂用量和洗脱剂等对能影响固相萃取效率的条件逐一进行优化。结果在最佳实验条件下,磁性壳聚糖对铅和镉的最大吸附容量分别为57.2 和43.7 mg/g,在12 min内达到吸附饱和状态。铅和镉在 0.2~10.0 μg/L范围内线性关系良好,相关系数分别为0.999 9和0.999 9,检出限分别为0.02和0.05 μg/L。结论 CDCS/Fe₃O₄-EDTA已成功萃取富集环境水样中的铅和镉。

关键词: 磁性壳聚糖, β-环糊精, 铅, 镉, 电感耦合等离子体质谱

Abstract: Objective To take the ethylene diamine tetraacetic acid（EDTA） modified β-cyclodextrin-（CD） chitosan（CS）/Fe₃O₄（CDCS/Fe₃O₄-EDTA） as magnetic solid-phase extraction adsorbent,develop a method for the simultaneous determination of lead and cadmium in water samples by magnetic solid phase extraction-inductively coupled plasma mass spectrometry（ICP-MS）. Methods The conditions that affect the efficiency of solid-phase extraction,such as pH,extraction time,adsorbent dosage and eluent,were optimized. Results Under the optimal conditions,the maximum adsorption capacities of magnetic chitosan were 57.2 mg/g for lead and 43.7 mg/g for cadmium. The adsorptions reached saturation state within 12 min. There was a good linear relationship for lead and cadmium within the range of 0.2-10.0 μg/L,the correlation coefficient was 0.999 9 and 0.999 9 respectively,and the detection limit was 0.02 and 0.05 μg/L respectively. Conclusion The CDCS/Fe₃O₄-EDTA has successfully extracted and enriched lead and cadmium in environmental water samples.

Key words: Magnetic chitosan, β-cyclodextrin, Lead, Cadmium, Inductively coupled plasma mass spectrometry

中图分类号:

R115

王露, 吴珺玮, 宋鑫, 冯晓青, 杨鹏飞, 张敏会. 水样中铅和镉磁性固相萃取测定法. [J]职业与健康, 2023, 39(15): 2026-2029.

WANG Lu, WU Junwei, SONG Xin, FENG Xiaoqing, YANG Pengfei, ZHANG Minhui. Determination of lead and cadmium in water samples by magnetic solid-phase extraction. [J]OCCUPATION AND HEALTH, 2023, 39(15): 2026-2029.

参考文献

[1] WEN T,WANG J,YU S J,et al.Magnetic porous Carbonaceous material produced from tea waste for efficient removal of As(V),Cr(VI),humic acid,and dyes[J].ACS Sustain Chem Eng.2017,5(5):4371-4379.
[2] 张哲辉. 水环境重金属污染现状及其评价[J].皮革制作与环保科技,2022,3(11):94-96.
[3] 张世霞. 水环境重金属污染的现状及其评价[J].中国科技信息, 2009(13):32-33.
[4] LIU M,WANG Z,ZONG S,et al.SERS detection and removal of mercury(Ⅱ)/Silver(Ⅰ) using oligonucleotide-functionalized core/shell magnetic silica sphere@Au nanoparticles[J].Acs Appl Mater Inter,2014,6(10):7371-7379.
[5] 黄芸,袁洪,黄志军,等.环境重金属暴露对人群健康危害研究进展[J].中国公共卫生,2016,32(8):1113-1116.
[6] 朱建龙,徐伟杰,郭硕铖,等.水体重金属污染危害及治理技术[J].现代农业科技,2022(6):129-132.
[7] 徐鲁翔. 我国食品中重金属危害现状及检测技术分析[J].中国食品,2022(7):111-113.
[8] 董学畅,王美香,郝南明,等.8-氨基喹哪啶固相萃取光度法测定水中痕量铁(Ⅲ)的研究[J].分析测试学报,2005,24(5):95-97.
[9] DABRPWSKI A,HUBICKI Z.Selective removal of the heavy metal ions from waters and industrial wastewaters by ion-exchange method[J].Chemosphere,2004,56(2):91-106.
[10] FF A,QI W.Removal of heavy metal ions from wastewaters:A review-Science Direct[J].J Environ Manage,2011,92(3):407-418.
[11] CAI G B,ZHAO G X,WANG X K,et al.Synthesis of polyacrylic acid stabilized amorphous calcium carbonate nanoparticles and their application for removal of toxic heavy metal ions in water[J].J Phys Chem C,2010,114(30):12948-12954.
[12] 刘景龙,韩倩,杨超,等.浊点萃取技术在重金属分析中的应用与进展[J].广州化学,2022,47(3):29-37.
[13] 袁玉兵,邓浩辉,何慧清.微波萃取-ICP-AES测定纺织品中的重金属元素[J].印染,2022,48(1):71-74.
[14] BACCAR R,BOUZID J,FEKI M,et al.Preparation of activated carbon from tunisian olive-waste cakes and its application for adsorption of heavy metal ions[J].J Hazard Mater,2009,162(2-3):1522-1529.
[15] 陈晓琴,黄晶,张蕾.固相萃取-电感耦合等离子体原子发射光谱(ICP-AES)法测定地下水中三种重金属[J].中国无机分析化学,2022,12(5):7-12.
[16] 王琛,李跃.磁性固相萃取剂Fe₃O₄/PDA/PAMAM的制备及其在Pb²+和Cd²+检测中的应用[J].材料科学与工程学报,2021,39(3):477-482.
[17] 邱素艳,俞熙仁,董一帆,等.基于聚乙烯吡咯烷酮功能化磁性氧化石墨烯固相萃取鸡饲料中Cu(Ⅱ)、Zn(Ⅱ)、Cr(Ⅲ)、Cd(Ⅱ)和Pb(Ⅱ)离子[J].分析测试学报,2022,41(2):242-248.
[18] GUIBAL E.Metal ion interactions with chitosan-a review[J].Sep Purif Technol,2004,38(1):43-50.
[19] FAN L L,ZHANG Y,LUO C N,et al.Synthesis and characterization of magnetic β-cyclodextrin-chitosan nanoparticles as nano-adsorbents for removal of methyl blue[J].Int J Biol Macromol,2012,50(2):444-451.
[20] 刘义,张淑琴,任大军,等.不同官能团改性壳聚糖吸附重金属的研究进展[J].化学试剂,2022,44(4):495-503.
[21] QIN R,LI F,CHEN M,et al.Preparation of chitosan-ethylene diaminetetra acetate-enwrapped magnetic CoFe₂O₄ nanoparticles via zero-length emulsion crosslinking method[J].Appl Surf Sci,2009,256(1):27-32.
[22] YANG L,LI Y,WANG L,et al.Preparation and adsorption performance of a novel bipolar PS-EDTA resin in aqueous phase[J].J Hazard Mater,2010,180(1-3):98-105.
[23] REPO E,WARCHOL J K,KURNIAWAN T A,et al.Adsorption of Co(Ⅱ) and Ni(Ⅱ) by EDTA-and/or DTPA-modifified chitosan:Kinetic and equilibrium modeling[J].Chem Eng J,2010,161:73-82.
[24] HUANG.Fabrication of water-compatible molecularly imprinted polymer based on beta-cyclodextrin modified magnetic chitosan and its application for selective removal of bisphenol A from aqueous solution[J].J Taiwan Inst Chem E,2017,77:113-121.
[25] YANG W,LU W,TIAN T,et al.Automated solid-phase extraction hyphenated to voltammetry for the determination of quercetin using magnetic nanoparticles and sequential injection lab-on-valve approach[J].Analyst,2012,137(10):2400-2405.