摘要
建立了快速溶剂萃取(ASE)-气相色谱-串联质谱(GC-MS/MS)分析海洋沉积物中16种多环芳烃(PAHs)的分析方法。样品由正己烷-丙酮(1∶1,v/v)溶液萃取,经无水硫酸钠脱水、氮吹浓缩后,采用硅胶固相萃取小柱进行净化,然后经HP-5MS色谱柱(30 m×0.25 mm×0.25μm)分离,在电子轰击电离源下以多反应监测(MRM)模式进行检测,内标法定量。分析结果表明,16种PAHs在0.01~1.00 mg/L范围内线性关系良好,相关系数(R)大于0.997;目标物的加标回收率为75.8%~97.8%;日内与日间精密度(RSD)均小于10%。当取样量为20.0 g时,16种PAHs的方法检出限为0.048~0.234μg/kg。该法快速、准确、稳定,能够满足海洋沉积物中痕量PAHs的测定。
A method based on gas chromatography-tandem mass spectrometry(GC-MS/MS)with accelerated solvent extraction(ASE)was developed for the determination of 16 polycyclic aromatic hydrocarbons(PAHs) in marine sediments. The sediment samples were extracted with hexane-acetone(1 ∶1,v/v). The extracts were dehydrated with anhydrous sodium sulfate,and concentrated with a termovap sample concentrator. The concentrated solutions were further cleaned up with Si SPE columns. The purified solutions were then isolated by HP-5 MS column(30 m × 0. 25 mm × 0. 25 μm). The analytes were detected using electron impact source under multiple reaction monitoring(MRM)mode. The results showed that the 16 PAHs had good linearities in the range of 0. 01-1. 00 mg/L with the correlation coefficients(R)greater than 0. 997. The spiked recoveries of the 16 PAHs were in the range of 75. 8%-97. 8%,and the relative standard deviations(RSDs)were less than 10%. The method detection limits(MDLs)of the 16 PAHs ranged from 0. 048-0. 234 μg/kg with 20. 0 g sampling weight. This method is suitable for the determination of trace PAHs in marine sediments.
出处
《色谱》
CAS
CSCD
北大核心
2018年第1期51-58,共8页
Chinese Journal of Chromatography
关键词
气相色谱-串联质谱
快速溶剂萃取
多环芳烃
海洋沉积物
gas chromatography-tandem mass spectrometry(GC-MS/MS)
accelerated solvent extraction(ASE)
polycyclic aromatic hydrocarbons(PAHs)
marine sediments
