近年来,“P-NMR(nuclear magnetic resonance)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31 P-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^-1HCI预提取,0.25mol·L^-1NaOH+0.05mol·L^-1 EDTA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,”P-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。
Solution 31 P-Nuclear Magnetic Resonance (NMR) is an analysis technology which has been an effective means for the analysis o{ 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 findthe most suitable sample preparation method for 31P-NMR analysis of the artificial wetland sediments, using different extractant (NaOH or 0.25 mol . L -1 NaOH-I-0. 05 mol . L -1 EDTA as main extractant, and 1M HC1 as pre-extractant or not), sample to extractant ratio (1 : 8 or 1 : 10), centrifugation conditions and scans time and so orL The results showed that the best 31P-NMR spectrum could be obtained with freeze-tied, ground and sieved sediments, 1 M HCI 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.