Determination of Polychlorinated Biphenyls in Water by Gas Chromatography-Mass Spectrometer Combined with Liquid-liquid Extraction
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摘要: 为准确、快速检测环境水体中多氯联苯(PCBs)，建立了液液萃取-气相色谱-质谱法同时测定18种PCBs的分析方法。通过对样品前处理流程、气相升温程序、载气流速、进样口温度等参数的优化，采用 HP- 5MS UI色谱柱 (30 m × 0.25 mm×0. 25μm)对目标物进行分离，在电子轰击电离源下以选择离子监测模式（SIM）进行检测。结果表明18 种PCBs在5 ~ 100μg/L范围内呈良好线性关系，线性相关系数R2均大于0.995。空白中低、中、高三个不同添加浓度下的样品平均加标回收率为78.1% ~ 101%，相对标准偏差(RSD，n=6)为0.272% ~ 3.28%，方法检出限(MDL)在0.44 ~ 0.96 ng/L之间。本方法选择性好、灵敏度高、重现性好，应用于实际样品检测的加标回收率在70.8% ~ 104%之间，能够满足环境水体样品中18种多氯联苯同时检测的分析要求。Abstract: In order to accurately and rapidly detect polychlorinated biphenyls (PCBs) in environmental water, a method was established for the simultaneous determination of eighteen kinds of PCBs by Gas Chromatography-Mass Spectrometer combined with liquid-liquid extraction. Through the optimization of parameters such as sample pretreatment process, gas temperature program, the flow rate of carrier gas, inlet temperature, etc., the gas chromatographic separation was carried out on HP-5MS UI chromatographic column (30 m × 0.25 mm × 0.25 μm), and selected ion monitoring mode (SIM) was used for detecting the targets under the electron ionization ion source. The results showed that the value of 18 kinds of PCBs linearly ranged from 5 to 100 mg/L, R2 value being over 0.995. Average recoveries of eighteen analytes in the blank water samples, which were spiked at three concentration levels, were between 78.1% and 101% with RSD (n=6) of 0.272%~3.28%. The MDL ranged from 0.44 to 0.96ng/L. This method was used in the detecting of practical samples, and the recoveries were between 70.8% and 104%. Thus, it can be seen that the method provides good selectivity, high sensitivity and good reproducibility, and it is suitable for the simultaneous determination of eighteen polychlorinated biphenyls in environmental water.
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Key words:
- liquid liquid extraction /
- gas chromatography-mass spectrometry /
- water body /
- PCBs
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