摘要
建立了加速溶剂萃取／气相色谱-质谱法（ASE／GC—MS）同时测定海洋沉积物中28种多氯联苯（PCBs）、16种多环芳烃（PAHs）和21种有机氯农药（OCPs）的分析方法。结果表明，ASE的最佳萃取温度为100℃，最佳静态时间为5min。GC—MS同时分析65种化合物时，PAHs的线性范围为0．05～5．00mg／L，线性系数（r^2）为0．991～0．999；PCBs和OCPs的线性范围为5．0～500．0μg／L，r^2不低于0．996。PCBs、PAHs和OCPs的检出限分别为0．03～0．11、0．04～0．73、0．06～0．48μg/kg，定量下限分别为0．11～0．35、0．12～2．42、0．18～1．61μg/kg，平均加标回收率为70％～146％，方法的相对标准偏差（n=6）为1．2％-17．3％。经海洋沉积物标准参考物质验证，该方法高效、准确，适合海洋沉积物中65种化合物的同时定量分析。
A gas chromatography - mass spectrometry （ GC - MS） coupled with accelerated solvent extraction（ASE） method was developed for the simultaneous determination of 28 polychlorinated biphenyls, 16 polycyclic aromatic hydrocarbons and 21 organochlorine pesticides in marine sediments. The results indicated that the best simultaneous extraction temperature and time were 100 ℃ and 5 min, respectively. Under the optimal conditions, the analysis of 65 compounds were carried out with GC - MS. The calibration curves were linear in the range of 0.05 - 5.00 mg/L for PAHs with correlation coefficients（ r^2） of 0. 991 -0. 999 and 5.0 -500. 0 μg/L for PCBs and OCPs with r^2 no less than 0. 996. The limits of detection of PCBs, PAHs and OCPs were in the range of 0. 03 - 0. 11, 0. 04 - 0. 73, 0. 06 - 0. 48μg/kg, and the limits of quantitation were in the range of 0. 11 - 0. 35, 0. 12 -2.42, 0. 1g - 1.61 μg/kg, respectively. The spiked recoveries ranged from 70% to 146% with RSDs（n =6） of 1.2% - 17.3% for all the compounds. Through marine sediments standard reference materials, the method was proved to be effective and accurate, and could be applied in the simultaneous determination of 65 compounds in marine sediments.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第2期152-160,共9页
Journal of Instrumental Analysis
基金
国土资源部海洋油气资源与环境地质重点实验室基金资助项目(RME200918)
关键词
海洋沉积物
多氯联苯
多环芳烃
有机氯农药
同时测定
marine sediments
polychlorinated biphenyls
polycyclic aromatic hydrocarbons
organochlorine pesticides
simuhaneous determination
