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首页> 外文期刊>Journal of mass spectrometry: JMS >Determination of polychlorinated biphenyls by liquid chromatography-atmospheric pressure photoionization-mass spectrometry
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Determination of polychlorinated biphenyls by liquid chromatography-atmospheric pressure photoionization-mass spectrometry

机译：液相色谱-大气压光电离质谱法测定多氯联苯

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This study presents the atmospheric pressure photoionization (APPI) of high-chlorinated (five or more chlorine atoms) polychlorinated biphenyls (PCBs) using toluene as dopant, after liquid chromatographic separation. Mass spectra of PCB 101, 118, 138, 153, 180, 199, 206 and 209 were recorded by using liquid chromatography-APPI-tandem mass spectrometry (LC-APPI-MS/MS) in negative ion full scan mode. Intense peaks appeared at m/z that correspond to [M-Cl +O]~- ions, where M is the analyte molecule. Furthermore, a detailed strategy, which includes designs of experiments, for the development and optimization of LC-APPI-MS/MS methods is described. Following this strategy, a sensitive and accurate method with low instrumental limits of detection, ranging from 0.29 pg for PCB 209 to 8.3 pg for PCB 101 on column, was developed. For the separation of the analytes, a Waters XSELECT HSS T3 (100mm× 2.1 mm, 2.5 μm) column was used with methanol/water as elution system. This method was applied for the determination of the above PCBs in water samples (surface water, tap water and treated wastewater). For the extraction of PCBs from water samples, a simple liquid-liquid extraction with dichloromethane was used. Method limits of quantification, ranged from 4.8 ngl~(-1), for PCB 199, to 9.4 ngl~(-1), for PCB 180, and the recoveries ranged from 73%, for PCB 101, to 96%, for PCB 199. The estimated analytical figures were appropriate for trace analysis of high-chlorinated PCBs in real samples.
机译：这项研究提出了液相色谱分离后，使用甲苯作为掺杂剂的高氯（五个或五个以上氯原子）多氯联苯（PCB）的大气压光电离（APPI）。通过在负离子全扫描模式下使用液相色谱-APPI串联质谱（LC-APPI-MS / MS）记录PCB 101、118、138、153、180、199、206和209的质谱图。强烈的峰出现在m / z处，对应于[M-Cl + O]-离子，其中M是分析物分子。此外，还介绍了用于开发和优化LC-APPI-MS / MS方法的详细策略，其中包括实验设计。按照这种策略，开发了一种灵敏而准确的方法，其检测限较低，从柱上PCB 209的0.29 pg到PCB 101的8.3 pg不等。为了分离分析物，使用了Waters XSELECT HSS T3（100mm×2.1 mm，2.5μm）色谱柱，并用甲醇/水作为洗脱系统。该方法用于测定水样（地表水，自来水和处理后的废水）中的上述多氯联苯。为了从水样中提取多氯联苯，使用了一种简单的用二氯甲烷进行液-液提取的方法。方法的定量限从PCB 199的4.8 ngl〜（-1）到PCB 180的9.4 ngl〜（-1）不等，回收率从PCB 101的73％到PCB的96％不等199.估计的分析数字适用于痕量分析实际样品中的高氯多氯联苯。

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