气相色谱/三重四极杆串联质谱法检测土壤中氯代多环芳烃和溴代多环芳烃

采用气相色谱-三重串联四极杆质谱联用仪（GC-QQQ-MS/MS）建立了同时检测土壤样品中19种氯代多环芳烃（Cl-PAHs）和8种溴代多环芳烃（Br-PAHs）的方法。采用正己烷-二氯甲烷（1：1,V/V）混合溶剂提取样品中的待测组分,经中性硅胶柱、双层碳可逆管柱净化后,采用GC-QQQ-MS/MS在多反应监测（MRM）模式下进行内标法定量。仪器分析条件：EI模式,多反应监测（MRM）,电离电压70eV;DB-5MS毛细管柱（60m×0.25mmi.d.,0.25μm）;进样口、离子源、四极杆和传输线温度分别为：280,230,150和300℃;碰撞流量1.5mL/min,淬火流量2.25m...

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Bibliographic Details
Published in分析化学 Vol. 41; no. 12; pp. 1825 - 1830
Main Author 莫李桂 马盛韬 李会茹 于志强 盛国英 傅家谟
Format Journal Article
LanguageChinese
Published 中国科学院广州地球化学研究所有机国家重点实验室,广州510640 2013
中国科学院研究生院,北京100039%中国科学院广州地球化学研究所有机国家重点实验室,广州,510640
Subjects
土壤
气相色谱-三重四极杆串联质谱
氯代多环芳烃
溴代多环芳烃
Chlorinated-polycyclic aromatic hydrocarbon
Brominated polycyclic aromatic hydrocarbon
Soil
Gas chromatography-triple quadrupole mass spectrometry
氯代多环芳烃
溴代多环芳烃
气相色谱-三重四极杆串联质谱
土壤
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ISSN0253-3820
DOI10.3724/SP.J.1096.2013.20434

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Summary:采用气相色谱-三重串联四极杆质谱联用仪（GC-QQQ-MS/MS）建立了同时检测土壤样品中19种氯代多环芳烃（Cl-PAHs）和8种溴代多环芳烃（Br-PAHs）的方法。采用正己烷-二氯甲烷（1：1,V/V）混合溶剂提取样品中的待测组分,经中性硅胶柱、双层碳可逆管柱净化后,采用GC-QQQ-MS/MS在多反应监测（MRM）模式下进行内标法定量。仪器分析条件：EI模式,多反应监测（MRM）,电离电压70eV;DB-5MS毛细管柱（60m×0.25mmi.d.,0.25μm）;进样口、离子源、四极杆和传输线温度分别为：280,230,150和300℃;碰撞流量1.5mL/min,淬火流量2.25mL/min;载气,He（1.0mL/min）。结果表明：d-PAHs,Cl-PAHs和Br-PAHs回收率在70%～118%之间,相对标准偏差（RSD）≤12%,仪器检出限在0.4～5.0pg之间。将该方法应用于我国某地区土壤样品的分析,移Cl-PAHs和移Br-PAHs浓度分别在725～1012pg/g和3532～5924pg/g之间。
Bibliography:In this study, simultaneous determination of C1-PAHs and Br-PAHs was developed by gas chromatography coupled to triple quadrupole mass spectrometry （GC-QQQ-MS/MS）. Soil samples were exacted and cleaned through silica gel column, dual-layer carbon reversible column respectively, after that, 19 congeners of C1-PAHs and 8 congeners of Br-PAHs were quantified. The GC-QQQ-MS/MS analysis condition was： EI and Multi-reaction monitoring （MRM） model, the electron emission energy was 70 eV; DB-5 MS fused silica capillary column （60 m × 0.25mm, 0.25 μm） ; the temperatures of injection, ion source, quadrupole and transfer line were 280, 230, 150 and 300 ℃, respectively. The collision and quenching flow were 1. 5 and 2. 25 mL/min, respectively. The carrier gas was Helium with the flow 1.0 mL/min. The results showed that the relative standard deviation （RSD） of parallel standard reference sample were ~〈 12.0%, and the recoveries of d-PAHs, C1-PAHs and Br-PAHs were between 70% -118%. The instrument detection limits of Cl-PA
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2013.20434