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首页> 外文期刊>Analytical Sciences >Development of a Screening Method for the Determination of PCBs in Water Using QuEChERS Extraction and Gas Chromatography–Triple Quadrupole Mass Spectrometry
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Development of a Screening Method for the Determination of PCBs in Water Using QuEChERS Extraction and Gas Chromatography–Triple Quadrupole Mass Spectrometry

机译：QuEChERS萃取和气相色谱-三重四极杆质谱法测定水中多氯联苯的筛选方法的开发

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摘要

A new method has been developed and validated for the simultaneous analysis of 11 polychlorinated biphenyls (PCBs), in water samples at trace levels by gas chromatography coupled to triple quadrupole mass spectrometry (GC-QqQ-MS/MS). Water samples were extracted by the QuEChERS (Quick Easy Cheap Effective Rugged and Safe) method. The QqQ analyzer acquired data in multiple reactions monitoring (MRM), permitting both quantification and confirmation in a single injection with a running time reduced up to 11.0 min. The effect of matrix interferences in extracts on analyte quantification and the identification of PCBs in water samples was deeply studied. The results showed that PCBs were prone to strong matrix interactions in water samples, and the quantification and identification of PCBs were highly affected by a matrix enhancement effect. To evaluate the performance of the method, validation experiments were carried out on water samples at three spiking levels (1.6, 8.0, 40.0 μg L~(?1)). Recovery was in the range of 95 – 109% at 1.6 μg L~(?1), 90 – 95% at 8.0 μg L~(?1) and 97 – 102% at 40.0 μg L~(?1), respectively. Precision values expressed as relative standard deviation (RSD) were lower than 15%. Linearity in the range of 0.5 – 50.0 μg L~(?1) provided determination coefficients (R ~(2)) higher than 0.999 for all compounds. The limits of detection (LODs) for PCBs were ≤0.1 μg L~(?1) and the limits of quantification (LOQs) ranged from 0.04 to 0.3 μg L~(?1). The applicability of the proposed method to detect and quantify PCBs has been demonstrated in analyse of 15 real samples.
机译：通过气相色谱-三重四极杆质谱联用（GC-QqQ-MS / MS），开发了一种新方法，该方法可同时分析痕量水样中的11种多氯联苯（PCB）。水样通过QuEChERS（快速，简单，便宜，有效，坚固，安全）方法提取。 QqQ分析仪在多反应监测（MRM）中获取数据，可在单次进样中同时进行定量和确认，而运行时间最多可缩短11.0分钟。深入研究了萃取物中基质干扰对水样中分析物定量和PCBs鉴定的影响。结果表明，多氯联苯在水样中易于发生强烈的基质相互作用，而基质增强作用对多氯联苯的定量和鉴定影响很大。为了评估该方法的性能，在三个加标水平（1.6、8.0、40.0μgL〜（？1））上对水样品进行了验证实验。 1.6 µg L〜（？1）时的回收率分别为95 – 109％，8.0 µg L〜（？1）时为90 – 95％和40.0 µg L〜（？1）时为97 – 102％。表示为相对标准偏差（RSD）的精度值低于15％。线性范围在0.5 – 50.0μgL〜（？1）内，所有化合物的测定系数（i R〜（2））均高于0.999。多氯联苯的检出限（LOD）≤0.1μgL〜（？1），定量限（LOQ）在0.04至0.3μgL〜（？1）的范围内。在分析15个真实样品中已证明了所提出方法检测和定量PCB的适用性。

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