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高冉, 饶竹, 郭晓辰, 等. 气相色谱-质谱法同时测定地下水中42种半挥发性有机污染物[J]. 分析测试学报, 2014,33(5):539-544.
Determination of 42 Semivolatile Organic Compounds in Groundwater by Gas Chromatography-Mass Spectrometry[J]. 2014,33(5):539-544.
建立了同时测定地下水中多环芳烃(PAHs)、多氯联苯(PCBs)、有机氯农药(OCPs)和有机磷农药(OPPs)等42种半挥发性有机污染物的分析方法,对固相萃取、液-液萃取、萃取溶剂和色谱柱等分析条件进行优化。最终采用乙酸乙酯-正己烷(1∶4)液液萃取,DB-5MS色谱柱分离,GC-MS/SIM测定,内标法定量。结果表明,42种目标物在0.5~1 000 μg/L范围内线性关系良好(r2>0.995);方法检出限为0.05~3.08 ng/L。在10、40、400 ng/L加标水平下,42种目标物的基体加标平均回收率为73.0%~107%,相对标准偏差(RSD,n=5)为1.4%~11.3%。将方法应用于石家庄周边地区水样检测,结果可靠。该方法灵敏、准确、简单易行,可显著提高地下水中主要有机污染物的分析效率。
A gas chromatography-mass spectrometric(GC-MS) method was established for the simultaneous determination of 42 semivolatile organic compounds,including polycyclic aromatic hydrocarbons(PAHs),polychlorinated biphenyls(PCBs),organochlorine pesticides(OCPs) and organophosphorus pesticides(OPPs)in groundwater.The preparation and analytical conditions,such as solid phase extraction(SPE),liquid-liquid extraction(LLE),extraction solvent and chromatographic column,were optimized.The 42 pollutants in groundwater were extracted by liquid-liquid extraction with ethyl acetate-hexane(1∶4),then determined by gas chromatography-mass spectrometry under selected ion monitoring(GC-MS/SIM) mode.Isotope labled acenaphthene-d10,phenanthrene-d10,chrysene-d12 and perylene-d12 were used as the internal standard for the quantitation analysis.Under the proposed conditions,the calibration curves of the compounds were linear in the range of 0.5-1 000 μg/L with correlation coefficients higher than 0.995.The method detection limits(MDL) were in the range of 0.05-3.08 ng/L.The accuracy and precision of the method were determined by analyzing water samples spiked with three concentration levels of 10,40,400 ng/L target compounds.The recoveries were in the range of 73.0%-107%,with RSDs(n=5) of 1.4%-11.3%.The method is sensitive,accurate and simple,which could significantly improve the efficiency in the analysis of main organic pollutants in groundwater.The method was successfully applied in the analysis of trace organic contaminants in groundwater samples collected from the surrounding area of Shijiazhuang,China.
气相色谱-质谱法(GC-MS)地下水多环芳烃(PAHs)多氯联苯(PCBs)有机氯农药(OCPs)有机磷农药(OPPs)
gas chromatography-mass spectrometry(GC-MS)groundwaterpolycyclic aromatic hydrocarbons(PAHs)polychlorinated biphenyls(PCBs)organochlorine pesticides(OCPs)organophosphorus pesticides(OPPs)
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