本文選題：蜂蜜　切入點：全氟烷基化合物　出處：《山東農(nóng)業(yè)大學》2017年碩士論文　論文類型：學位論文

【摘要】：全氟烷基化合物(Perfluorinated alkyl substances,PFASs)是人工合成的一類新型持久性有機污染物,由親水基末端和不同長度的疏水烷基碳鏈組成的,疏水烷基碳鏈上的氫原子全部被氟原子替代,形成含有極高化學能的C-F鍵(約為110 kcal/mol),其穩(wěn)定性極強,具有化學惰性和耐熱性等優(yōu)良性能。在20世紀50年代就廣泛被用作殺蟲劑、表面活性劑、潤滑劑、催化劑、以及合成藥物、氟橡膠、樹脂的中間體。PFASs難以被新陳代謝、水解、光解、生物降解,在生物體內(nèi)隨著時間的推移可不斷富集,PFASs在生物體內(nèi)的蓄積濃度遠高于已知的二VA英和有機氯等持久性環(huán)境污染物。大量研究發(fā)現(xiàn),全氟辛酸(PFOA)與全氟辛烷磺酸(PFOS)具有生殖毒性、心血管毒性、肝臟毒性、甲狀腺毒性和神經(jīng)毒性。目前,國內(nèi)外學者相繼在水產(chǎn)品、動物肝臟、蛋、奶、母乳中檢測出了PFASs,而通過膳食攝入PFASs已成為人體內(nèi)PFASs的來源之一。本文采用高效液相色譜-串聯(lián)質(zhì)譜技術(shù)結(jié)合QuEChERS方法對蜂蜜中的PFASs殘留檢測方法進行了研究。主要研究內(nèi)容如下:采用高效液相色譜-串聯(lián)質(zhì)譜(HPLC-MS/MS)技術(shù)結(jié)合改進QuEChERS預處理方法建立了同時蜂蜜中20種全氟烷基化合物(全氟丁酸、全氟戊酸、全氟丁烷磺酸、全氟己酸、全氟戊烷磺酸鈉、全氟庚酸、全氟己烷磺酸、全氟庚烷磺酸鈉、全氟辛酸、全氟辛烷磺酸鈉、全氟壬酸、全氟壬烷磺酸鈉、全氟癸酸、全氟癸烷磺酸鈉、全氟十一烷酸、全氟十二烷酸、全氟十三烷酸、全氟十四烷酸、全氟十六烷酸、全氟十八烷酸)的殘留檢測方法。稱取5.0 g蜂蜜樣品于50 mL聚丙烯(PP)離心管中,加入5μL 2μg/mL混合內(nèi)標標準溶液和5 m L水,然后加入10 mL含1.5%甲酸(v/v)的乙腈,漩渦1 min后,加入1 g氯化鈉和4 g無水硫酸鎂,振搖10 min后,以10000 r/min離心10 min。取上層乙腈7 mL轉(zhuǎn)移到裝有40 mg PSA、80 mg C18和900mg無水MgSO4的15 mL離心管中,振搖10 min后,以10000 r/min離心10 min,最后取4 m L(相當于2 g試樣提取液)上清液于玻璃氮吹管中,40℃水浴氮吹至干,以1 mL甲醇定容后,過0.22μm濾膜,HPLC-MS/MS分析。Atlantis T3 C18色譜柱分離,以含5 mmol/L乙酸銨的甲醇溶液和5 mmol/L乙酸銨溶液溶液為流動相進行梯度洗脫。電噴霧離子(ESI)源負離子模式下以多反應監(jiān)測(MRM)掃描,采用同位素內(nèi)標法進行定量分析。實驗結(jié)果表明,20種PFASs在0.2~10μg/L濃度范圍內(nèi)線性相關(guān)系數(shù)均大于0.995;檢出限范圍為0.04~0.1μg/kg;定量限范圍為0.1~0.2μg/kg。在0.1、0.5、1和2μg/kg添加濃度下(n=6),20種PFASs加標回收率范圍為72.56%~112.98%,相對標準偏差(RSD)范圍為0.73%~15.73%。結(jié)果表明,該方法快速、高效、準確,適用于蜂蜜樣品中20種PFASs的同時分析檢測。
[Abstract]:Perfluorinated alkyl substrates (PFASs) are a new class of synthetic persistent organic pollutants, which are composed of hydrophilic end groups and hydrophobic alkyl carbon chains of different lengths. All hydrogen atoms in hydrophobic alkyl carbon chains are replaced by fluorine atoms. Forming C-F bonds with extremely high chemical energy (about 110kcal / mol / mol) with excellent stability, chemical inertia and heat resistance. In 1950s, C-F bonds were widely used as insecticides, surfactants, lubricants, catalysts, etc. And the intermediates of synthetic drugs, fluorocarbons, resins. PFASs are difficult to metabolize, hydrolyze, photolysis, biodegrade, The accumulation of PFASs in organisms over time is much higher than that of known persistent environmental pollutants such as diVA and organochlorine. Perfluorooctanoic acid (PFOAA) and perfluorooctane sulfonate (PFOS) have reproductive toxicity, cardiovascular toxicity, liver toxicity, thyroid toxicity and neurotoxicity. PFASs were detected in breast milk, and dietary PFASs intake has become one of the sources of PFASs in human body. In this paper, the detection of PFASs residues in honey by high performance liquid chromatography-tandem mass spectrometry (HPLC / MS) combined with QuEChERS method was studied. The main contents are as follows: 20 perfluoroalkyl compounds (perfluorobutyric acid, perfluorobutyric acid, perfluorobutyric acid, perfluorobutyric acid, perfluorobutyric acid, perfluorobutyric acid, perfluorobutyric acid) in simultaneous honey were. Perfluoropentanoic acid, perfluorobutane sulfonic acid, perfluorohexanoic acid, perfluoropentane sulfonate, perfluoroheptanesulfonate, perfluorooctanesulfonate, perfluorooctanesulfonate, perfluorononane sulfonate, perfluorovaleric acid, perfluorononane sulfonate, perfluorodecanoic acid, perfluoroheptanesulfonate, perfluorooctanesulfonate. Perfluorodecane sulfonate, perfluorodecanoic acid, perfluorohexadecanoic acid, perfluorohexadecanoic acid, perfluorinated 13 alkanoic acid, perfluorinated 14 alkanoic acid, perfluorohexadecanoic acid, Determination of perfluoroalkanoic acid in 50 mL PP centrifuge tube with 5.0 g honey, 5 渭 L 2 渭 g / mL mixed internal standard solution and 5 mL water was added, then 10 mL acetonitrile containing 1.5% formic acid v / v) was added for 1 min. Adding 1 g sodium chloride and 4 g anhydrous magnesium sulfate, shaking for 10 min, centrifuging for 10 mins at 10000 r / min. The upper layer acetonitrile was transferred to 15 mL centrifuge tube containing 40 mg PSA-80 mg C18 and 900mg anhydrous MgSO4 for 10 min, and the upper acetonitrile was transferred to 15 mL centrifuge tube containing 40 mg PSA-80 mg C18 and 900mg anhydrous MgSO4. The supernatant of 4 mL (equivalent to 2 g sample extract) was centrifuged at 10000 r / min for 10 min. The supernatant was blown to dry in the glass nitrogen blowing tube at 40 鈩，

本文編號：1561580