本文選題：季銨鹽　切入點(diǎn)：LC-MS　出處：《湖南大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：季銨化合物(QACs)是一類最主要的陽離子表面活性劑,被廣泛用于家庭,工業(yè),農(nóng)業(yè)及醫(yī)療應(yīng)用領(lǐng)域作為木材防腐劑,殺蟲劑,殺真菌劑,消毒劑和清潔劑。QACs普遍存在于全世界范圍內(nèi)的污水,工業(yè)廢水,污泥,地表水以及水體沉積物中,對(duì)生物處理系統(tǒng)及環(huán)境系統(tǒng)構(gòu)成威脅。現(xiàn)在,QACs的環(huán)境污染問題逐漸引起環(huán)境工作者的關(guān)注。因此,建立一種快捷、穩(wěn)定、可靠的環(huán)境樣品中QACs分析方法對(duì)環(huán)境中QACs的監(jiān)測(cè)具有十分重要的意義。本實(shí)驗(yàn)首先探討了經(jīng)TMSH衍生運(yùn)用GC-MS檢測(cè)十六烷基三甲基氯化銨(ATMAC-C16)的分析方法。從優(yōu)化衍生反應(yīng)條件、GC-MS分析條件出發(fā),研究了衍生劑用量對(duì)ATMAC-C16衍生產(chǎn)物檢測(cè)的影響。然而,由于GC-MS需要先對(duì)QACs進(jìn)行衍生化處理,較為復(fù)雜,本實(shí)驗(yàn)最終選定采用液相色譜質(zhì)譜聯(lián)用技術(shù)(LC-MS)結(jié)合正離子電噴霧電離(ESI+)方法檢測(cè)季銨鹽。首先,初步建立了LC-MS分析季銨鹽的儀器方法。在選定色譜柱為C18柱,流動(dòng)相為含有0.1%甲酸的甲醇/水(7:3)溶液的前提下,優(yōu)化了液相色譜的梯度洗脫程序,梯度洗脫開始時(shí)流動(dòng)相比例為30%A、70%B;0-4min時(shí)逐漸增加到100%B;4-6min時(shí)保持100%B;6-7min時(shí)又降低到30%A、70%B;7-8min時(shí)保持為30%A、70%B。該方法對(duì)十六烷基三甲基氯化銨(ATMAC-C16)、十八烷基芐基氯化銨(BAC-C18)、雙十二烷基二甲基溴化銨(DADMAC C12:C12)以及雙十八烷基二甲基溴化銨(DADMAC C18:C18)這四種季銨鹽的檢測(cè)限可達(dá)到5ng/m L;并建立了四種季銨鹽的線性方程分別為y=2494.9956x+49182.4711,y=4525.7995x+50788.1729,y=760.6959x+35908.5828,y=2711.0139x+14566.4124,相關(guān)系數(shù)均大于0.99;相對(duì)標(biāo)準(zhǔn)偏差小于10%,方法的精密度較好。本文還采用LC-MS方法對(duì)長(zhǎng)沙開福污水處理廠的進(jìn)出水和各處理單元的污泥樣品進(jìn)行檢測(cè),通過索氏萃取和固相萃取方法提取、富集及純化其中的季銨鹽。檢測(cè)結(jié)果表明進(jìn)水中含有ATMAC-C16、BAC-C18、DADMAC C12:C12、DADMAC C18:C18這四種季銨鹽,其中DADMAC C12:C12含量最高,為17.3093 ng/mL;其次是BAC-C18和DADMAC C18:C18,分別為15.5366 ng/mL和7.0409 ng/mL;ATMAC-C16含量最低,為5.2801 ng/mL。而出水樣中只檢測(cè)到ATMAC-C16,含量為1.0418 ng/mL;其它三種季銨鹽均低于檢測(cè)限,未被檢出。由此可算出該污水處理廠對(duì)四種季銨鹽的去除率均在80%以上。對(duì)該污水處理廠各處理單元的污泥樣品的檢測(cè)結(jié)果表明:所有污泥樣品中都含有這四種季銨鹽,但由于低于檢測(cè)限無法被定量。
[Abstract]:Quaternary ammonium compounds (quaternary ammonium compounds) are the most important cationic surfactants that are widely used as wood preservatives, insecticides and fungicides in household, industrial, agricultural and medical applications. Disinfectants and detergents. QACs are found worldwide in sewage, industrial wastewater, sludge, surface water and sediments. Threat to biological treatment systems and environmental systems. Now the problem of environmental pollution of QACs has gradually attracted the attention of environmental workers. Therefore, to establish a fast, stable, Reliable QACs analysis method in environmental samples is of great significance for the monitoring of QACs in the environment. In this experiment, the analytical method for the detection of cetyltrimethylammonium chloride ATMAC-C16 by TMSH derivation and GC-MS was first discussed. The reaction conditions were analyzed by GC-MS. The effect of the amount of derivatives on the detection of ATMAC-C16 derivatives was studied. However, because of the need of GC-MS for the first derivative treatment of QACs, it is more complicated. In this experiment, the liquid chromatography-mass spectrometry (LC-MS) combined with positive ion electrospray ionization ionization (ESI) method was used to detect quaternary ammonium salts. Firstly, an instrument for the determination of quaternary ammonium salts by LC-MS was established. The chromatographic column was selected as C18 column. With the mobile phase of methanol / water 7: 3 solution containing 0.1% formic acid, the gradient elution procedure of liquid chromatography was optimized. The mobile phase ratio at the beginning of gradient elution was 30A70BC16, 18 alkyl benzyl ammonium chloride BAC-C18, bis#number1# dialkyl methyl bromide, and then decreased to 30A70B7min, 30A70B7min and 30A70B at the beginning of the gradient elution. The method was applied to the determination of hexadecyltrimethylammonium chloride ATMAC-C16, 18 alkyl benzyl ammonium chloride BAC-C18, bis-#number1# dialkyl methyl bromide. The detection limits of the four quaternary ammonium salts (DADMAC C12: C12) and bis 18 alkyl dimethyl ammonium bromide (DADMAC C18: C18) can reach 5ng / mL, and the linear equations of the four quaternary ammonium salts are established respectively as yy 2494.9956x 49182.4711y4525.7995x 50788.1729ynium 760.69x 35908.5828yU 2711.139x 14566.4124124.The correlation coefficients are all greater than 0.990.The relative standard deviations are higher than 0.994.The linear equations of the four quaternary ammonium salts are as follows: YY 2494.9956x 49182.4711y4525.7995x 50788.1729yr 760.69x 35908.5828yr. Less than 10, the precision of the method is better. The LC-MS method is also used to detect the inlet and outlet water of Changsha Kaifu sewage treatment plant and the sludge samples from each treatment unit. The quaternary ammonium salt was enriched and purified by Soxhlet extraction and solid phase extraction. The results showed that there were four quaternary ammonium salts, ATMAC-C16, BAC-C18, DADMAC, C12: C12, DADMAC, C18C18, in which the content of DADMAC C12: C12 was the highest. BAC-C18 and DADMAC C18: C18 were 15.5366 ng/mL and 7.0409 ng / mL respectively, the lowest ATMAC-C16 content was 5.2801 ng / mL. however, only ATMAC-C16 was detected in water samples with a content of 1.0418 ng / mL; the other three quaternary ammonium salts were all below the detection limit. The removal rates of the four quaternary ammonium salts in the sewage treatment plant are all above 80%. The results of the sludge samples from each unit of the sewage treatment plant show that all the sludge samples contain these four quaternary ammonium salts. However, it can not be quantified because it is below the detection limit.
【學(xué)位授予單位】：湖南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：X703

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