水中常見藥物和個人護(hù)理品的分析方法改進(jìn)研究
發(fā)布時間：2018-07-17 17:28
【摘要】：近年來,藥物和個人護(hù)理品(PPCPs)在水中頻繁檢出,成為一類受到廣泛關(guān)注的新興污染物。準(zhǔn)確把握PPCPs的環(huán)境存在水平,是闡明其遷移轉(zhuǎn)化規(guī)律和評價其環(huán)境風(fēng)險的重要基礎(chǔ)。由于PPCPs種類繁多,各個國家/地區(qū)的生產(chǎn)和使用情況不同,因而其水環(huán)境中常見的主要PPCPs也會有很大差異。為此,必須開發(fā)針對性強(qiáng)、準(zhǔn)確靈敏而方便快捷的分析方法。本研究根據(jù)我國PPCPs的生產(chǎn)消費(fèi)特點(diǎn),建立了水中常見38種PPCPs的分析方法并開展了案例應(yīng)用;在此基礎(chǔ)上引入同位素內(nèi)標(biāo),進(jìn)一步開發(fā)了定量更準(zhǔn)確、穩(wěn)定性更好的PPCPs精準(zhǔn)測定方法。首先,以國際上主流的固相萃取液相色譜串聯(lián)質(zhì)譜分析方法為基礎(chǔ),通過對采水瓶材質(zhì)、固相萃取柱、液相色譜質(zhì)譜參數(shù)等的系統(tǒng)優(yōu)化,建立了針對我國水體中常見的38種PPCPs(包括16種人用和22種獸用PPCPs)的分析方法。篩選采用國產(chǎn)固相萃取柱Cleanert PEP-2來等效替代進(jìn)口柱Oasis HLB,大大降低了分析成本。將方法用于飲用水、河水、污水等實(shí)際水樣考察其適用性,結(jié)果表明:平行實(shí)驗(yàn)的相對標(biāo)準(zhǔn)偏差小于30%,空白實(shí)驗(yàn)中無高于方法定量限的本底存在,表明所建立的分析方法能夠很好的應(yīng)用于多種類型水體的監(jiān)測。接著,以清華大學(xué)校園內(nèi)的兩座中水站為對象,利用所建立的方法進(jìn)行了長達(dá)一個學(xué)期的跟蹤監(jiān)測。結(jié)果發(fā)現(xiàn):方法能夠很好地用于本案例的實(shí)際監(jiān)測;PPCPs在進(jìn)水中的濃度與學(xué)生學(xué)習(xí)、生活的活動規(guī)律具有較強(qiáng)的關(guān)聯(lián)性;兩座中水站對PPCPs的去除率均優(yōu)于普通市政污水處理廠,這得益于所采用的膜生物反應(yīng)器(MBR)工藝和全年保持室溫的穩(wěn)定運(yùn)行條件。最后,針對現(xiàn)有方法中內(nèi)標(biāo)物數(shù)量較少且與目標(biāo)物結(jié)構(gòu)和性質(zhì)差異較大,從而導(dǎo)致方法系統(tǒng)誤差較大的問題,開展了同位素內(nèi)標(biāo)方法的探索。結(jié)合最新的可獲得性情況,將方法中的提取內(nèi)標(biāo)從4種擴(kuò)展至31種,使絕大多數(shù)的目標(biāo)物可以按照同位素稀釋法原理進(jìn)行定量。結(jié)果表明:改進(jìn)方法的方法檢出限(MDL)總體上比常規(guī)內(nèi)標(biāo)法更低了一個數(shù)量級;同時在精密度和準(zhǔn)確度上也要優(yōu)于內(nèi)標(biāo)法。該方法為水中PPCPs的監(jiān)測提供了更為精準(zhǔn)的選擇,尤其適用于目標(biāo)物濃度極低或基質(zhì)復(fù)雜的監(jiān)測場合,以及對數(shù)據(jù)準(zhǔn)確度要求更高的科研目的。
[Abstract]:In recent years, drugs and personal care products (PPCPs) have been frequently detected in water, and have become a kind of emerging pollutants. Accurately grasping the environmental level of PPCPs is an important basis for clarifying the laws of their migration and transformation and evaluating their environmental risks. Due to the variety of PPCPs and the different production and use of PPCPs in different countries and regions, the main PPCPs in their water environment are also very different. Therefore, it is necessary to develop analytical methods with strong pertinence, accuracy, sensitivity and convenience. According to the characteristics of production and consumption of PPCPs in China, the analytical methods of 38 common PPCPs in water were established and the case application was carried out in this study, based on which the isotopic internal standard was introduced to further develop a more accurate quantitative method. A more stable and accurate method for the determination of PPCPs. First of all, based on the international mainstream solid-phase extraction liquid chromatography-tandem mass spectrometry (SPEC-MS) method, the material of the water bottle, the solid phase extraction column, the parameters of the liquid-phase chromatography-mass spectrometry were optimized. A method for the analysis of 38 species of PPCPs (including 16 human and 22 animal PPCPs) was established. The domestic solid phase extraction column (Cleanert PEP-2) was used to replace the imported column Oasis HLB.The analysis cost was greatly reduced. The method was used to investigate the applicability of the method in drinking water, river water, sewage and other real water samples. The results showed that the relative standard deviation of parallel experiments was less than 30, and there was no background above the quantitative limit of the method in the blank experiment. The results show that the proposed analytical method can be applied to the monitoring of many kinds of water bodies. Then, two middle water stations on the campus of Tsinghua University were used to track and monitor for a semester. The results show that the method can be used to monitor the concentration of PPCPs in the influent and the students' learning and living rules, and the removal rate of PPCPs by the two intermediate water stations is better than that of ordinary municipal wastewater treatment plants. This is due to the membrane bioreactor (MBR) process and stable operating conditions at room temperature throughout the year. Finally, aiming at the problem that the quantity of internal standard is small and the structure and property of the method are different from the target, which leads to the large systematic error of the method, the research of the isotope internal standard method is carried out. According to the latest available conditions, the extraction internal standard of the method is extended from 4 to 31, so that most of the target materials can be quantified according to the principle of isotope dilution method. The results show that the detection limit (MDL) of the improved method is lower by an order of magnitude than that of the conventional internal standard method, and the precision and accuracy of the improved method are also better than that of the internal standard method. This method provides a more accurate choice for the monitoring of PPCPs in water, especially for the monitoring situations where the concentration of the target material is very low or the matrix is complex, and for scientific research purposes which require higher accuracy of the data.
【學(xué)位授予單位】：清華大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X832
本文編號：2130407
[Abstract]:In recent years, drugs and personal care products (PPCPs) have been frequently detected in water, and have become a kind of emerging pollutants. Accurately grasping the environmental level of PPCPs is an important basis for clarifying the laws of their migration and transformation and evaluating their environmental risks. Due to the variety of PPCPs and the different production and use of PPCPs in different countries and regions, the main PPCPs in their water environment are also very different. Therefore, it is necessary to develop analytical methods with strong pertinence, accuracy, sensitivity and convenience. According to the characteristics of production and consumption of PPCPs in China, the analytical methods of 38 common PPCPs in water were established and the case application was carried out in this study, based on which the isotopic internal standard was introduced to further develop a more accurate quantitative method. A more stable and accurate method for the determination of PPCPs. First of all, based on the international mainstream solid-phase extraction liquid chromatography-tandem mass spectrometry (SPEC-MS) method, the material of the water bottle, the solid phase extraction column, the parameters of the liquid-phase chromatography-mass spectrometry were optimized. A method for the analysis of 38 species of PPCPs (including 16 human and 22 animal PPCPs) was established. The domestic solid phase extraction column (Cleanert PEP-2) was used to replace the imported column Oasis HLB.The analysis cost was greatly reduced. The method was used to investigate the applicability of the method in drinking water, river water, sewage and other real water samples. The results showed that the relative standard deviation of parallel experiments was less than 30, and there was no background above the quantitative limit of the method in the blank experiment. The results show that the proposed analytical method can be applied to the monitoring of many kinds of water bodies. Then, two middle water stations on the campus of Tsinghua University were used to track and monitor for a semester. The results show that the method can be used to monitor the concentration of PPCPs in the influent and the students' learning and living rules, and the removal rate of PPCPs by the two intermediate water stations is better than that of ordinary municipal wastewater treatment plants. This is due to the membrane bioreactor (MBR) process and stable operating conditions at room temperature throughout the year. Finally, aiming at the problem that the quantity of internal standard is small and the structure and property of the method are different from the target, which leads to the large systematic error of the method, the research of the isotope internal standard method is carried out. According to the latest available conditions, the extraction internal standard of the method is extended from 4 to 31, so that most of the target materials can be quantified according to the principle of isotope dilution method. The results show that the detection limit (MDL) of the improved method is lower by an order of magnitude than that of the conventional internal standard method, and the precision and accuracy of the improved method are also better than that of the internal standard method. This method provides a more accurate choice for the monitoring of PPCPs in water, especially for the monitoring situations where the concentration of the target material is very low or the matrix is complex, and for scientific research purposes which require higher accuracy of the data.
【學(xué)位授予單位】：清華大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X832
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