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液相色谱-离子色谱联用体系同时测定环境基质中的6种硝基芳烃类化合物和3种阴离子OACSTPCD

Simultaneous determination of six nitroaromatic compounds and three anions in environmental matrices using a liquid chromatography-ion chromatography coupled system

中文摘要英文摘要

同时测定环境土壤和水基质中的硝基芳烃类化合物和阴离子对于选择合适的硝基芳烃类化合物降解方法和实现地表水水质监测具有重要意义.本文通过两个六通阀和一根富集柱将高效液相色谱和离子色谱连接,搭建了色谱联用体系.系统操作可分为 4 个阶段:(A)样品加载到定量环;(B)分离硝基芳烃类化合物和阴离子;(C)阴离子在AG20 柱中富集;(D)高效液相色谱和离子色谱分别测定硝基芳烃类化合物和阴离子.通过将液相色谱柱直接连接电导率检测器,确定阴离子流出液相色谱柱的时间,优化六通阀的切换时间,保证方法的准确性.在最优条件下,阴离子的检出限为 0.005~0.020 mg/L,硝基芳烃类化合物的检出限为0.043~0.150 mg/L.3 组不同加标浓度样品的平均回收率为 88.20%~105.38%,相对标准偏差为 2.0%~11.5%.该方法被用于检测 5 份地表水样品和 5 份土壤样品,硝基芳烃类化合物均未检出,3 种阴离子在地表水样品中的检出量为 0.41~55.3 mg/L,在土壤样品中的检出量为 0.56~30.2 mg/kg.经过方法学验证和实际样品检测,证明该色谱联用体系检测方法自动化程度高,操作简单,重复性好,准确度高,具有广泛的适用性和较高的灵敏度,适用于环境基质中硝基芳烃类有机物和亚硝酸根离子等阴离子含量的快速测定.

Nitroaromatic compounds are used extensively in various fields such as dyes,pesti-cides,spices,pharmaceuticals,and explosives.However,the residual raw materials of these compounds accumulate in the environment and pose serious risks to human health.Chronic ex-posure to low concentrations of nitroaromatic compounds can cause anemia,cancer,and organ damage.Currently,Fenton oxidation and natural bioremediation are the processes most often used to eliminate nitroaromatic compounds from environmental water and soil.According to previous research,the presence of inorganic anions such as chloride,nitrite,and nitrate ions in the environmental matrix exerts an inhibitory effect on the biodegradation of nitroaromatic com-pounds.Furthermore,high nitrate levels in drinking water can lead to the production of nitrosa-mine carcinogens,which affect ecological safety and human health,in water bodies.Thus,the simultaneous determination of nitroaromatic compounds and chloride,nitrite,and nitrate ions in environmental soil and water matrices is critical for selecting appropriate nitroaromatic compound degradation methods and monitoring surface water quality.Traditional detection methods require two sample pretreatment steps and two instrumental analytical techniques to determine nitroaromatic compounds and inorganic anions in environmental matrices;moreover,these methods are time consuming,labor intensive,and error prone.Therefore,in this study,a method that combines high performance liquid chromatography(HPLC)and ion chromatography(IC)was developed to simultaneously detect nitroaromatic compounds and anions in environmental matrices.In this method,sample enrichment was achieved through bulk injection and enrichment column collection,which greatly simplified the pretreatment process.The HPLC instrument was connected to the IC instrument using two six-way valves and an enrichment column.The system operation can be divided into four stages:(A)sample loading to the quantitative ring,(B)separation of nitroaromatic compounds and anions,(C)enrichment of anions in an AG20 column,and(D)simultaneous determination of nitroaromatic compounds and anions by HPLC and IC,respectively.The time of the anions flowing out of the C18 column was determined by directly connecting the C18 column to a conductivity detector.Based on the retention times of the anions,the switching time of the six-way valve was opti-mized to ensure that the anions completely entered the IC column,thereby ensuring the accura-cy of the method.During the chromatographic analysis stage,nitroaromatic compounds were separated and analyzed by HPLC system with a mobile phase composed of potassium phosphate buffer(pH 7.0)and acetonitrile(60∶40,v/v)at a flow rate of 1.0 mL/min;in the IC system,the anions were separated and analyzed using a 20 mmol/L sodium hydroxide aqueous solution as the mobile phase under a suppression current of 50 mA.Both anions and nitroaromatic com-pounds exhibited strong linear correlations within certain concentration ranges,with correlation coefficients greater than 0.993.The recoveries of the nitroaromatic compounds and anions ranged from 88.20%to 105.38%at three spiked levels,with relative standard deviations ran-ging from 2.0%to 11.5%.The contents of six nitroaromatic compounds and three anions in five surface water and five soil samples were determined using the developed method.Although no nitroaromatic compounds were detected in these samples,the three anions were detected at contents ranging from 0.41 to 55.3 mg/L in surface water samples,and 0.56 to 30.2 mg/kg in soil samples.Methodological validation and actual sample detection demonstrated that the pro-posed method has a high degree of automation,simple operation,good repeatability,high ac-curacy,wide applicability,and high sensitivity.Thus,this method is suitable for the rapid de-termination of chloride,nitrite,nitrate ions and nitroaromatic compounds in soil and water and can be extended to the simultaneous determination of inorganic ions and organic matters in oth-er samples.

雷佳诚;郑黄荣;刘璐;李巍霞

中国计量大学标准化学院,浙江 杭州 310018中国标准化协会,北京 100037

化学

离子色谱高效液相色谱硝基芳烃类化合物阴离子土壤环境水

ion chromatography(IC)high performance liquid chromatography(HPLC)ni-troaromatic compoundsanionssoilenvironmental water

《色谱》 2024 (001)

92-98 / 7

国家自然科学基金项目(22304167).National Natural Science Foundation of China(No.22304167).

10.3724/SP.J.1123.2023.10027

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