CAJ | 학술논문

近年来，31P-NMR（nuclearmagneticresonance）已成为研究环境有机磷的有力武器，然而此方法在湿地学研究中的应用却很少，关于湿地沉积物样品制备方法的研究更缺乏。本研究通过改变提取剂组成、提取剂比例、离心条件、检测扫描时间等因素设计实验，寻找最佳的湿地沉积物样品处理及检测方法，以期为31P-NMR技术在湿地沉积物样品有机磷研究中的应用提供科学依据。结果表明采用：1mol·L-1HCl预提取，0.25mol·L-1NaOH＋0.05mol·L-1EDTA主提取，沉积物与提取剂比例为1∶8的提取方法，可获得更好的提取效果。提取完成后，采用冷冻高速离心可更好地分离提取液、避免某些磷组分的水解。此外，NMR扫描分析时间设为14～16h（约扫描25000次）可获得更完整的图谱。相较于传统的化学分析法，31P-NMR法的样品前处理相对简单、分析时破坏性小且组分分辨完全，该技术的运用，有望获得湿地磷循环，特别是对有机磷认知的新突破。
근년래，31P-NMR（nuclearmagneticresonance）이성위연구배경유궤린적유력무기，연이차방법재습지학연구중적응용각흔소，관우습지침적물양품제비방법적연구경결핍。본연구통과개변제취제조성、제취제비례、리심조건、검측소묘시간등인소설계실험，심조최가적습지침적물양품처리급검측방법，이기위31P-NMR기술재습지침적물양품유궤린연구중적응용제공과학의거。결과표명채용：1mol·L-1HCl예제취，0.25mol·L-1NaOH＋0.05mol·L-1EDTA주제취，침적물여제취제비례위1∶8적제취방법，가획득경호적제취효과。제취완성후，채용냉동고속리심가경호지분리제취액、피면모사린조분적수해。차외，NMR소묘분석시간설위14～16h（약소묘25000차）가획득경완정적도보。상교우전통적화학분석법，31P-NMR법적양품전처리상대간단、분석시파배성소차조분분변완전，해기술적운용，유망획득습지린순배，특별시대유궤린인지적신돌파。
Solution 31 P-Nuclear Magnetic Resonance (NMR) is an analysis technology which has been an effective means for the analysis of environmental organic phosphorus .However ,the method is rarely applied in the study of wetlands so that the corre-sponding researches about wetland sediment sample preparation method also very deficient .The present study was aimed to find the most suitable sample preparation method for 31 P-NMR analysis of the artificial wetland sediments ,using different extractant (NaOH or 0.25 mol · L -1 NaOH+0.05 mol · L -1 EDTA as main extractant ,and 1 M HCl as pre-extractant or not) ,sample to extractant ratio (1∶8 or 1∶10) ,centrifugation conditions and scans time and so on .The results showed that the best 31 P-NMR spectrum could be obtained with freeze-ried ,ground and sieved sediments ,1 M HCl as pre-extractant for 16 h ,NaOH+0.05 mol · L -1 EDTA as main extractant for 16 h ,extraction ratio of 1∶8 ,and low temperature and high-speed centrifugation (4 ℃ ,10 000 r · min-1 for 30min) for avoiding hydrolysis of certain components .Besides ,choosing much longer NMR scan time ,as 14~16 h (scans about 25 000 times) ,could get more complete spectral signals spectrum .And finally ,four kinds of P-compounds (orthophosphate ,orthophosphate monoesters ,orthophosphate diesters and pyrophosphate ) were detected in the NMR spec-trum .But neither polyphosphate nor phosphonates was not found in all these experiments ,which need further study .Compared with the traditional chemical analysis method ,31 P-NMR method of sample preparation is relatively simple .Then it is less de-structive with components distinguished completely .Using 31 P-NMR technology ,the cognition of wetland phosphorus cycle ,es-pecially organophosphate ,will be expected to get new breakthrough .