本文關(guān)鍵詞： 羧基化納米碳球 固相萃取 全氟類化合物 液相色譜串聯(lián)質(zhì)譜儀　出處：《山東農(nóng)業(yè)大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：全氟化合物(Perfluorochemicals,PFCs)是一類持久存在于環(huán)境中的新型有機(jī)污染物。近年來,大量的研究顯示,全氟化合物已被發(fā)現(xiàn)在食品、土壤、水、空氣、接觸材料等介質(zhì)中。由于PFCs在環(huán)境的長久污染性和在生物體內(nèi)的積累性,使其越來越受到人們的關(guān)注。由于近幾年中國的氟化工行業(yè)的快速發(fā)展,在中國一些城市的飲用水污染現(xiàn)狀均高于其他國家。所以在食品安全領(lǐng)域?qū)λ泻哿咳惢衔锏姆治鰷y定一直是研究的熱點。在本研究中,使用了一種表面經(jīng)羧基修飾過的新型功能化納米碳球-羧基化納米碳球(CNSs-COOH),使之作為固相萃取(SPE)吸附劑,聯(lián)合液相色譜串聯(lián)質(zhì)譜儀(LC-MS/MS)建立了一種測定水中六種全氟類化合物的新方法,并對不同地方的實際水樣品基質(zhì)進(jìn)行了檢測分析,驗證了該方法的實用性。本研究主要結(jié)果如下:1.通過對萃取條件(萃取時間、pH值)、解吸條件(解吸溶劑種類、解吸溶劑體積)、水樣品的體積及羧基化納米碳球的用量進(jìn)行優(yōu)化等條件優(yōu)化,得到了最優(yōu)實驗條件為:400 mL pH=2的水樣品,流速為6 mL/min,解吸溶劑為pH=10的丙酮7 m L,羧基化納米碳球用量為300 mg。2.在最優(yōu)實驗參數(shù)下,建立的方法對于全氟癸酸(PFDA)、全氟壬酸(PFNA)、全氟辛酸(PFOA)、全氟庚酸(PFHpA)、全氟己烷磺酸(PFHxS)和全氟辛烷磺酸(PFOS)擁有0.01~1.20 ng L-1的低檢出限,在0.5~200 ng L-1的線性范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)(R2)為0.997~0.999,相對標(biāo)準(zhǔn)偏差介于3.70~8.80%。3.該方法被應(yīng)用于桶裝飲用水、自來水及池塘水樣品的分析檢測,在自來水樣品中有PFHxS被檢測出,在池塘水樣品中有PFHxS和PFOS被檢測出,而在桶裝飲用水中6種全氟類化合物均未被檢出。在100 ng L-1、50 ng L-1、10 ng L-1三個濃度下加標(biāo)試驗,回收率為82.2~109.7%。
[Abstract]:Perfluorochemical compounds (PFCs) are new organic pollutants that persist in the environment. In recent years, a large number of studies have shown that perfluorides have been found in food, soil, water, air, In contact materials and other mediums, PFCs has attracted more and more attention due to its long-term pollution in the environment and accumulation in organisms. Due to the rapid development of fluorine chemical industry in China in recent years, The status quo of drinking water pollution in some cities in China is higher than that in other countries. Therefore, the analysis and determination of trace perfluorides in water in the field of food safety has always been a hot topic. A new functionalized carbon nanospheres, CNSs-COOHN, modified by carboxyl group, was used as a solid phase extraction (SPE) adsorbent. A new method for the determination of six perfluorinated compounds in water was established by combined liquid chromatography tandem mass spectrometer (LC-MS / MS). The main results of this study are as follows: 1. The extraction conditions (extraction time and pH value), desorption conditions (kinds of desorption solvents) were determined. The desorption solvent volume, the volume of water sample and the amount of carboxylated carbon nanospheres were optimized. The optimal experimental conditions were obtained for water sample with 1: 400 mL pH=2. The flow rate is 6 mL / min, the desorption solvent is 7 mL of acetone of pH=10 and the amount of carboxylated carbon nanospheres is 300 mg 路2. Under the optimum experimental parameters, The established method has a low detection limit of 0.01 ~ 1.20 ng 路L ~ (-1) for PFDAA, PFNAA, PFOAA, PFHpAX, PFHxSand PFOS of perfluorooctanesulfonic acid, and a good linearity in the linear range of 0.5 ~ 200 ng 路L ~ (-1). The relative standard deviation was between 3.70 and 8.80. The method was applied to the analysis of bottled drinking water, tap water and pond water samples. PFHxS was detected in tap water samples and PFHxS and PFOS were detected in pond water samples. Six perfluorinated compounds were not detected in barrelled drinking water, and the recovery was 82.2% 109.7% at the concentration of 100 ng / L ~ (50) ng / L ~ (-1) and 10 ng / L ~ (10) ng 路L ~ (-1) ~ (-1).
【學(xué)位授予單位】：山東農(nóng)業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O658.2;X832

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