中文摘要：

以高磷污染河流沉积物为研究对象，利用液相31P核磁共振（^31P-NMR）技术研究了沉积物中有机磷提取剂的选择和提取过程.结果表明：前提取以BD和EDTA效果最佳，TP和Po的提取量分别为（322.87±13.81）和（119.76±16.00）mg·kg^-1、（24.91±15.25）和（20.90±2.58）mg·kg^-1，2种提取剂均促进了NaOH的提取效率，前提取后NaOH提取液中TP和Po的提取量分别达到（2271.20±75.63）和（2477.40±112.71）mg·kg^-1、（152.04±1.55）和（186.93±20.53）mg·kg^-1；对顺磁性离子Fe和Mn而言，利用BD和EDTA＋Na2S2O4作为前提取剂可以提取更多的Fe离子，提取液中的浓度分别为（5116.57±24.32）和（10677±215.61）mg·kg^-1；EDTA和EDTA＋Na2S2O4提取剂对Mn的去除效量较高，提取液中浓度分别为（243.02 ±2.80）和（266.61±1.61）mg·kg^-1.液相31P-NMR图谱显示，上述提取剂处理后均可得到正磷酸盐、焦磷酸、磷酸单酯、磷脂和DNA 5种磷形态，其中EDTA可提高沉积物中正磷酸盐、焦磷酸盐、磷脂和DNA的含量.综合考虑：利用EDTA和NaOH两步提取可实现较高的Po提取量和较低的顺磁性离子干扰，并得到理想的核磁共振图谱，从而保证沉积物中有机磷液相31P-NMR分析的科学性和有效性.

英文摘要：

A two-step extraction using different extractants was studied on the phosphorus （P） pollution river sediments by solution 31P-NMR. Pro-extraction using BD or EDTA all increased TP and Po extraction amounts in NaOH post-extraction, which were （2271.20±75.63） and （2477.40±112.71） mg·kg^-1 for TP, and （152.04±1.55） and （186.93±20.53） mg·kg^-1 for Po. Moreover, the extractants （BD or EDTA＋Na2S2O4） increased Fe extraction amounts in pro-extraction, reaching （5116.57±24.32） and （10677±215.61） mg·kg^-1, respectively, while EDTA or EDTA＋Na2S2O4 increased Mn extraction amounts in pro-extraction, reaching （243.02±2.80） and （266.61±1.61） mg·kg^-1, respectively. Five P species, including orthophosphate （ortho-P）, pyrophosphate （pyro-P）, orthophosphate monoesters （mono-P）, phospholipids （lipids-P） and deoxyribonucleic acids （DNA-P）, were all detected in different extractions, and the EDTA pro-extraction could increase the concentrations of ortho-P, pyro-P, lipids-P and DNA-P. The results showed that the two-step extraction using EDTA and NaOH could increase TP and Po extraction amounts in post-extract and Fe and Mn extraction amounts in pro-extract, which optimized 31P-NMR spectroscopy for Po analysis.