Mass spectrometric detection in narrow-bore (0.10 mm i.d.) capillary chromatography fast, sensitive and selective analysis of polychlorinated biphenyls.
Mass spectrometric detection in narrow-bore (0.10 mm i.d.) capillary chromatography fast, sensitive and selective analysis of polychlorinated biphenyls.
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窄孔（内径 0.10 毫米）毛细管色谱法中的质谱检测对多氯联苯进行快速、灵敏和选择性分析。
DOI：
10.1016/s0021-9673(01)01001-9
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发表时间：
2001
影响因子：
4.1
通讯作者：
Paul Schepens
中科院分区：
文献类型：
--
作者：
A. Covaci;Paul Schepens
研究了窄孔毛细管气相色谱-台式四极杆质谱联用检测多氯联苯的方法。通过几种分析（PCB标准和人乳提取物）说明了该系统的定性和定量性能。比较了不同内径（分别为0.10、0.18和0.22 mm）的毛细管柱对PCB同系物的分离能力和分析时间。较短的运行时间（小于7分钟）足以在0.10 mm内径（I.D.）毛细管柱上完全分离PCB同源物，而与0.22 mm内径柱相比，没有任何分辨率损失。在运行时间为8 min时，四极杆质谱仪可以获得良好的定性和定量数据，但当运行时间减少到3-4 min时，观察到峰读数不完整。选择离子监测和停留时间10 ms是必要的，以获得单个PCB同源物的检测限低至0.4 pg μl−1标准溶液和0.2 ng g−1脂肪牛奶提取物。采用冷无劈裂进样方法，窄孔毛细血管的进样量较大（1 μl），且无峰值畸变。
The combination of narrow-bore capillary gas chromatography with bench-top quadrupole mass spectrometric detection was evaluated for the determination of polychlorinated biphenyls (PCBs). The qualitative and quantitative performances of the system are illustrated by several analyses (PCB standards and human milk extracts). Capillary columns with different internal diameters (0.10, 0.18 and 0.22 mm, respectively) were compared for their ability to separate PCB congeners and the analysis time. Short run times (less than 7 min) were sufficient for complete separation of PCB congeners on a 0.10-mm internal diameter (I.D.) capillary column without any loss of resolution when compared with a 0.22 mm I.D. column. Good qualitative and quantitative data acquisition was possible with quadrupole mass spectrometer for run times of 8 min, but incomplete peak reading was observed when run times were reduced to 3–4 min. Selected ion monitoring and dwell times of 10 ms are necessary to obtain detection limits for individual PCB congeners as low as 0.4 pg μl−1for standard solutions and 0.2 ng g−1fat for milk extracts. By using cold splitless injection, relatively high volumes (1 μl) for narrow-bore capillaries could be injected without any peak distortion.