色谱

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应用搅拌棒吸附萃取-热脱附-气相色谱/质谱法快速测定滇池水系中的16种多环芳烃

杨蕾1,2,王保兴1,2,侯英1,杨燕1

  

  1. 1.Yunnan Reascend Tobacco Technology (Group) Co., Ltd., Kunming 650106, China; 2.Yunnan Normal University, Kunming 650092, China

  • 收稿日期:2007-03-20 修回日期:2007-05-24 出版日期:2007-09-30 发布日期:1985-03-25
  • 通讯作者: 杨蕾

Determination of Polycyclic Aromatic Hydrocarbons in Dianchi Lake Using Stir Bar Sorptive Extraction-Thermal Desorption-Gas Chromatography/Mass Spectrometry

YANG Lei1,2, WANG Baoxing1,2, HOU Ying1, YANG Yan1

  

  1. 1.Yunnan Reascend Tobacco Technology (Group) Co., Ltd., Kunming 650106, China; 2.Yunnan Normal University, Kunming 650092, China

  • Received:2007-03-20 Revised:2007-05-24 Online:2007-09-30 Published:1985-03-25

摘要:

应用搅拌棒吸附萃取(SBSE)-热脱附(TDS)-气相色谱/质谱联用(GC/MS)方法测定了滇池水系(滇池和盘龙江上、中、下游)中16种多环芳烃(PAHs)的含量。方法快速简便,无有机溶剂污染,PAHs的最低检出限为1.0~468.8 pg,理论回收率在90%以上,加标回收率为83.1%~109.4%,相对标准偏差小于10%。测定结果表明,这16种多环芳烃在滇池水样中的含量为89.16 ng/L,在盘龙江上游水样中的含量为65.41 ng/L,在盘龙江中游水样中的含量为339.22 ng/L,而在盘龙江下游水样中的含量为62.25 ng/L,说明滇池水系已经受到一定的PAHs污染,加强对滇池、盘龙江中PAHs有机污染的控制势在必行。

关键词: 滇池, 多环芳烃, 搅拌棒吸附萃取, 盘龙江 , 气相色谱, 热脱附, 质谱

Abstract:

A fast method for determination of polycyclic aromatic hydrocarbons (PAHs) in water samples was established. The samples from the Dianchi Lake and Panlong River were analyzed directly using stir bar sorptive extraction-thermal desorption system-gas chromatography/mass spectrometry (SBSE-TDS-GC/MS). Polydimethylsiloxane (PDMS) was used as the extraction phase. The samples were extracted with stir bars at 1100 r/min for 60 min at ambient temperature (25 ℃). Desorption was carried out at 300 ℃ for 5 min under a helium flow of 50 mL/min in the splitless mode while maintaining a cryofocusing temperature of 0 ℃ in the programmed-temperature vaporization (PTV) injector of the GC/MS system. The limits of detection of PAHs ranged from 1.0 pg to 468.8 pg. The theoretical recoveries of PAHs were greater than 90% (except that naphthalene was 64.90%), and the recoveries of 16 PAHs from water samples ranged from 83.1% to 109.4%, and the relative standard deviations (RSDs) ranged from 1.2% to 9.3% (n=6). PAHs in Dianchi Lake and Panlong River samples were quantified rapidly by this method. The results show that, the total content of these 16 PAHs is 89.16 ng/L in Dianchi Lake, 65.41 ng/L in the up-stream of Panlong River, 339.22 ng/L in the middle-stream of Panlong River and 62.25 ng/L in the down-stream of Panlong River. It is demonstrated that the Dianchi Lake and Panlong River were polluted by PAHs to some degree.

Key words: Dianchi Lake, gas chromatography (GC), mass spectrometry (MS), Panlong River , polycyclic aromatic hydrocarbons, thermal desorption, stir bar sorptive extraction (SBSE)