首页|气相色谱-三重四极杆串联质谱法测定土壤中16种多环芳烃及衰减规律的研究

气相色谱-三重四极杆串联质谱法测定土壤中16种多环芳烃及衰减规律的研究

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建立了一种土壤中16种多环芳烃多反应监测(MRM)气相色谱-三重四极杆串联质谱(GC-MS/MS)的检测方法.本文使用加速溶剂萃取,以正己烷-丙酮(体积比1∶1)为萃取溶剂,在温度100 ℃、压力10 Mpa条件下萃取5 min,循环萃取两次;经快速滤过型净化柱净化,氮吹浓缩后采用多反应监测模式气相色谱-三重四极杆串联质谱法测定.优化方法条件下,所得标准曲线相关系数R2≥0.9991,空白加标回收率77.5%~112.2%,相对标准偏差0.7%~14.0%;实际样品加标回收率79.9%~119.4%,方法检出限0.01~0.05 μg/kg.研究了土壤中高、低两种浓度的多环芳烃在室温、冷藏、冷冻3种保存条件下,150天的衰减规律.结果显示,室温条件衰减速度>冷藏>冷冻,低浓度衰减速度略大于高浓度.
Study on the Determination of 16 Polycyclic Aromatic Hydrocarbons in Soil by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry and Their Attenuation Patterns
In this work,a method for detecting 16 types of polycyclic aromatic hydrocarbons in soil was developed using multiple reaction monitoring via Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry(GC-MS/MS).The procedure entailed twice accelerated solvent extraction with n-hexane∶acetone(1∶1,V/V)as the solvent under the conditions of 100℃ and 10 Mpa for 5 minutes.After post-extraction,samples were purified using a rapid filter purification column and concentrated under nitrogen before GC-MS/MS analysis in MRM mode.Spike recoveries in blank matrix ranged from 77.5%to 112.2%,with relative standard deviations between 0.7%and 14.0%;and spike recoveries in actual samples varied from 79.9%to 119.4%.The detection limits of the method were between 0.01 and 0.05 μg/kg.The study also investigated the degradation patterns of high and low concentrations of polycyclic aromatic hydrocarbons in soil under various storage conditions—room temperature,refrigerated,and frozen-over a period of 150 days.The findings indicated that degradation was the fastest at room temperature,followed by refrigeration,and slowest under frozen,with lower concentrations degrading slightly faster than higher concentrations.

Polycyclic aromatic hydrocarbonsGas chromatography-triple quadrupole tandem mass spectrometryMultiple reaction monitoringMPFC-QuEChERSAttenuation pattern

张兰、王敏捷、曹立峰、范文耀、张南、李丹、木春红

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河南省地质局地质灾害防治中心,河南郑州 454000

河南省第三地质勘查院有限公司,河南郑州 451464

多环芳烃 气相色谱-三重四极杆串联质谱法 多反应监测 快速滤过型净化柱 衰减规律

2024

分析科学学报
武汉大学,北京大学,南京大学

分析科学学报

CSTPCD北大核心
影响因子:0.717
ISSN:1006-6144
年,卷(期):2024.40(6)