Hajslová J, Cuhra P, Kempný M, Poustka J, Holadová K, Kocourek V
Institute of Chemical Technology, Department of Food Chemistry and Analysis, Prague, Czech Republic.
J Chromatogr A. 1995 May 5;699(1-2):231-9. doi: 10.1016/0021-9673(95)00030-q.
Basic parameters associated with practical application of gas chromatography coupled with microwave-induced plasma atomic emission spectrometric detection GC-MIP-AED in the determination of seven "indicator" polychlorinated biphenyls (PCBs) in biotic matrices were evaluated. The detection limit for chlorine (Cl-479) was found to be 0.54 pg/s. Under the conditions used for sample analysis (1 microliters of purified extract injected into the GC-MIP-AED system represented 2.5 mg of original fat), this value corresponded approximately to 0.15 mg/kg of the respective congeners in fat. The detector response was linear within the tested range of 0.5-10 ng of each injected PCB. The relative standard deviation of repeated injections for the lowest concentration level of 0.5 ng of PCB per injection ranged between 10.5 and 34.4% depending on the chlorine content of the individual analytes. The results demonstrate a high selectivity of chlorine detection. Carbon (C-496) chromatograms recorded simultaneously demonstrated the efficiency of the clean-up step used. Quantitative results (analytes at levels of 0.1-1 mg/kg) obtained with the atomic emission detector did not differ significantly from those recorded with a conventional electron-capture detector.
评估了气相色谱-微波诱导等离子体原子发射光谱检测法(GC-MIP-AED)在生物基质中测定七种“指示性”多氯联苯(PCBs)实际应用中的基本参数。发现氯(Cl-479)的检测限为0.54 pg/s。在用于样品分析的条件下(注入GC-MIP-AED系统的1微升纯化提取物相当于2.5毫克原始脂肪),该值大致相当于脂肪中各同系物0.15毫克/千克。在所测试的每种注入PCB的0.5 - 10纳克范围内,检测器响应呈线性。每次注入0.5纳克PCB的最低浓度水平下,重复注入的相对标准偏差根据各分析物的氯含量在10.5%至34.4%之间。结果表明氯检测具有高选择性。同时记录的碳(C-496)色谱图证明了所用净化步骤的有效性。原子发射检测器获得的定量结果(分析物水平为0.1 - 1毫克/千克)与传统电子捕获检测器记录的结果无显著差异。