超高压高效液相色谱串联质谱法测定土壤中的5种硝基酚类化合物  

Determination of 5 Nitrophenols in Soil Samples by Ultra High Pressure High Perfor⁃mance Liquid Chromatography-Mass Spectrometry

作　　者：贾以律 高媛媛 任子威 郑志豪 Jia Yi-lv;Gao Yuan-yuan;Ren Zi-wei;Zheng Zhi-hao(Zhejiang Huakun Geological Development Co.,Ltd,Wenzhou,Zhejiang 325000,China)

机构地区：[1]浙江华坤地质发展有限公司,浙江温州325000

出　　处：《福建分析测试》2023年第4期1-4,10,共5页Fujian Analysis & Testing

摘　　要：建立了超高压高效液相色谱串联质谱法测定土壤中的5种硝基酚类化合物的分析方法。土样由二氯甲烷-正己烷(2:1,v/v)混合溶液快速溶剂萃取,萃取物经SPE柱净化去除大部分干扰物,采用Thermo acquity UPLC BEH C18柱(50mm×2.1mm,1.7μm)分离,以0.01mol/L甲酸铵-甲酸水溶液(pH 4.0)为流动相进行梯度洗脱,流速0.4mL/min,柱温30℃,进样5μL,电喷雾负离子电离(ESI-)模式、多反应监测(MRM)模式进行检测,外标法定量。5种硝基酚类化合物的峰面积与其质量浓度在一定浓度范围内均呈良好的线性关系(r^(2)≥0.997),方法检出限为0.002~0.008μg/kg。测定低、中、高加标浓度的样品,5种硝基酚类化合物的相对标准偏差为0.8%~5.8%(n=6)。此方法灵敏度高,干扰小,分析速度快,可适用于环境土壤中5种硝基酚类污染物的同时分析。A method for the determination of 5 nitrophenols in soil by ultra high pressure high performance liquid chromatog⁃raphy tandem mass spectrometry was established.10g soil samples were extracted by dichloromethane-n-hexane(2:1,v/v)mixed solution.Most of the interferences were removed by SPE.The samples were separated by thermoequity UPLC BEH C18 column(50 mm×2.1 mm,1.7μm).The gradient elution was carried out with 0.01 mol/L ammonium formate-Formic acid aqueous solution(pH 4.0)as mobile phase,with a flow rate of 0.4 ml/min,column temperature of 30℃,and sample in⁃jection of 5μL,electrospray ionization(ESI-)mode and multiple reaction monitoring(MRM)mode were used to detect and quantified by external standard method.There was a good linear relationship between the peak area of 5 nitrophenols and their mass concentration in a certain range(R^(2)≥0.997).The detection limit of the method was 0.002-0.008μg/kg.The relative standard deviation of 5 nitrophenols was 0.8%-5.8%(n=6)for the samples with low,medium and high stan⁃dard concentration.This method has the advantages of high sensitivity,small interference and fast analysis speed,which can be applied to the simultaneous analysis of five nitrophenols in environmental soil.

关 键 词：硝基酚 超高压液相串联质谱 快速溶剂萃取 土壤 

分 类 号：O657.72[理学—分析化学]