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作 者:马莹莹[1] 沈幸[1] 龚慧娟[2] 张进琪[3] 鲜啟鸣[1] 邹惠仙[1]
机构地区:[1]污染控制与资源化研究国家重点实验室,南京大学环境学院,南京210093 [2]南京大学现代分析中心,南京210093 [3]南京大学化学化工学院,南京210093
出 处:《南京大学学报(自然科学版)》2007年第4期365-371,共7页Journal of Nanjing University(Natural Science)
基 金:国家自然科学基金(20477015)
摘 要:在深入研究饮用水中强致突变物MX的过程中,发现了一个前人从未研究过的氯化消毒副产物.在实验室模拟氯化,经分离、提纯制备得到了该新副产物的纯化合物,通过GC/MS、IR、1HNMR和13CNMR和四圆X单晶衍射等多种现代仪器的分析表征,确定了该新副产物的结构,并将其命名为2,2,4-三氯-5-甲氧基环戊-4-烯-1,3-二酮(TCMCD).接着在实验室自行设计合成了TCMCD的标样,同时也用全合成的方法再次确认了TCMCD结构的正确性.研究建立了饮用水中TCMCD富集分离、定性定量的分析方法,并对一些水厂的水样进行了检测,最高浓度可达80.1ng/L.采用Ames实验对TCMCD的毒性进行了初步研究,结果表明其具有一定的致突变性.Disinfection by-products (DBPs) in drinking water continue to be an area of great interest in environmental science due to their potential adverse heath effects in humans. A new DBP was firstly found when we studied the Mutagen in drinking water. We have chlorinated under the best reaction condition for many times. The chlorination products were extracted by ethyl ether and isolated further through times of silica column chromatography. Finally a few of the pure DBP was got through recrystallization from n-hexane. It was identified as 2,2, 4-trichloro-5-methoxy-cyclopenta-4-ene-1. 3-dione (TCMCD) through GC/MS. IR ^1 HNMR and ^13C NMR spectra and single-crystal x-ray diffraction method. Then we designed the synthetical route of TCMCD and synthesized it from heptachlor propane in the laboratory. The overall yield is 13% and the purity of the product is above 98%. At the same time, we reconfirm the structure we previously proposed is correct. We study the analytic method of TCMCD with solid-phase extraction. The experiment by the way of XAD-2 resin adsorption, acetic ether elution, qualitative and quantitative determination with GC/MS. The average recovery at high concentration is 66. 9% and its degree of precision is 1.49%. And we determinate the concentration level of TCMCD in drinking water at high cancer rate area of Jiangsu Province. The result found that the concentration can reach 80.1 ng/L in YCDF drinking water we collected, which is higher than MX in the same place. Ames test was conducted to study the mutagen city of TCMCD. TA100 and TA98 strains were chosen as tester strains. The result revealed that the number of revert ant increased obviously when the dosage of TCMCD changed from 10-100 μg/plate by using tests strain TA100. Thus conclusion could be made that TCMCD was mutagenic.
关 键 词:饮用水 氯化 TCMCD 结构表征 合成 分析检测
分 类 号:X131.2[环境科学与工程—环境科学]
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