Optimization of extraction and parameters for 31P-NMR analysis of organic phosphorus extracted from aquatic plants and algae
FENG Wei-ying1,2, ZHU Yuan-rong2, WU Feng-chang2, LIU Sha-sha1,2, ZHANG Chen2
1. College of Water Sciences, Beijing Normal University, Beijing 100875, China;
2. State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China
Characterization of organic phosphorus (Po) from aquatic plants and algae by solution 31P-Nuclear Magnetic Resonance (31P-NMR) is important to understand its biogeochemical cycling in lakes. Methods of extraction and selection of parameters for NMR characterization and quantification of Po critical. Various extractants and radio of sample to extractants were applied for 31P-NMR. A mixture of 0.5mol/L NaOH-25m mol/L EDTA with a ratio of sample to extractant of 1:60 was the optimal extraction of Po from aquatic plants and algae. When the extract was analyzed by use of 31P-NMR, the delay time (D1) and scanning time were set to 5s and 15h, respectively, which resulted in approximately 24,000 scans. Based on how Samples were extracted and results of 31P-NMR analysis, P in aquatic plants and algae included orthophosphates, orthophosphate monoesters, orthophosphate diesters and pyrophosphate, of which Po accounted for 34%~53% and 31%~73% respectively. Orthophosphate monoester was the predominant constituent of Po, which accounted for 92 and 83% of plants and algae, respectively. The proportion of orthophosphate diesters was small in aquatic plants and algae and accounted for only 0~6.65% of the TP. The content of pyrophosphate in algae was approximately 35-fold greater than that in aquatic plants.
Baldwin D S. Organic phosphorus in the aquatic environment[J]. Environmental Chemistry, 2013,10(6):439-454.
[2]
Zhu Y, Wu F, He Z, et al.Characterization of organic phosphorus in lake sediments by sequential fractionation and enzymatic hydrolysis[J]. Environ. Sci. Technol., 2013,47(14):7679-7687.
Reitzel K, Ahlgren J, Gogoll A, Rydin E.Effects of aluminum treatment on phosphorus, carbon, and nitrogen distribution in lake sediment:a 31P NMR study[J]. Water research, 2006,40(4):647-654.
Tao Y, Yuan Z, Fengchang W, Wei M. Six-Decade Change in Water Chemistry of Large Freshwater Lake Taihu, China[J]. Environmental Science and Technology, 2013,47(16):9093-9101.
Qu X, Xie L, Lin Y, et al. Quantitative and qualitative characteristics of dissolved organic matter from eight dominant aquatic macrophytes in Lake Dianchi, China[J]. Environmental Science and Pollution Research, 2013,20(10):7413-7423.
[12]
Da-Peng L, Yong H.Sedimentary phosphorus fractions and bioavailability as influenced by repeated sediment resuspension[J]. Ecological Engineering, 2010,36(7):958-962.
[13]
Monbet P, McKelvie I D, Worsfold P J. Dissolved organic phosphorus speciation in the waters of the Tamar estuary (SW England)[J]. Geochimica et Cosmochimica Acta, 2009,73(4):1027-1038.
[14]
Wang J, Pant H K. Identification of organic phosphorus compounds in the Bronx River bed sediments by phosphorus-31nuclear magnetic resonance spectroscopy[J]. Environmental Monitoring and Assessment, 2010,171(1-4):309-319.
[15]
Newman R, Tate K. Soil phosphorus characterisation by 31P nuclear magnetic resonance[J]. Communications in Soil Science and Plant Analysis, 1980,11(9):835-842.
[16]
Cade-Menun B J. Characterizing phosphorus in environmental and agricultural samples by 31P nuclear magnetic resonance spectroscopy[J]. Talanta, 2005,66(2):359-371.
[17]
Cade-Menun B J.Improved peak identification in 31P-NMR spectra of environmental samples with a standardized method and peak library[J]. Geoderma, 2015,257-258:102-114.
[18]
Zhu Y, Wu F, He Z, et al. Influence of Natural Organic Matter on the Bioavailability and Preservation of Organic Phosphorus in Lake Sediments[J]. Chemical Geology, 2015,397:51-60.
[19]
Ahlgren J, Reitzel K, Danielsson R, et al. Biogenic phosphorus in oligotrophic mountain lake sediments:Differences in composition measured with NMR spectroscopy[J]. Water Research, 2006, 40(20):3705-3712.
[20]
He Z, Olk D C, Cade-Menun B J. Forms and lability of phosphorus in humic acid fractions of Hord silt loam soil[J]. Soil Science Society of America Journal, 2011,75(5):1712-1722.
[21]
Bai X, Ding S, Fan C, et al. Organic phosphorus species in surface sediments of a large, shallow, eutrophic lake, Lake Taihu, China[J]. Environmental Pollution, 2009,157(8):2507-2513.
[22]
Otten T, Xu H, Qin B, et al. Spatiotemporal patterns and ecophysiology of toxigenic Microcystis blooms in Lake Taihu, China:implications for water quality management[J]. Environmental Science andTechnology, 2012,46(6):3480-3488.
[23]
Zhu Y, Zhang R, Wu F, et al. Phosphorus fractions and bioavailability in relation to particle size characteristics in sediments from Lake Hongfeng, Southwest China[J]. Environmental Earth Sciences, 2013,68(4):1041-1052.
Zhang W, Tang W, Zhang H, et al. Characterization of biogenic phosphorus in sediments from the multi-polluted Haihe River, China, using phosphorus fractionation and 31P-NMR[J]. Ecological Engineering, 2014,71:520-526.
[26]
He Z, Honeycutt C W, Griffin T S, et al. Phosphorus forms in conventional and organic dairy manure identified by solution and solid state P-31NMR spectroscopy[J]. Journal of Environmental Quality, 2009,38(5):1909-1918.
Read E K, Ivancic M, Hanson P, et al. Phosphorus speciation in a eutrophic lake by 31P NMR spectroscopy[J]. Water Research, 2014,62:229-240.
[30]
Giles C D, Lee L G, Cade-Menun B J, et al. Characterization of Organic Phosphorus Form and Bioavailability in Lake Sediments using P Nuclear Magnetic Resonance and Enzymatic Hydrolysis[J]. Journal of Environmental Quality, 2015,44(3):882-894.
[31]
Turner B L, Mahieu N, Condron L M. Phosphorus-31nuclear magnetic resonance spectral assignments of phosphorus compounds in soil NaOH-EDTA extracts[J]. Soil Science Society of America Journal, 2003,67(2):497-510.
[32]
Johnson N R, Hill J E. Phosphorus species composition of poultry manure-amended soil using high-throughput enzymatic hydrolysis[J]. Soil Science Society of America Journal, 2010, 74(5):1786-1791.
[33]
Pinchuk G E, Ammons C, Culley D E, et al. Utilization of DNA as a sole source of phosphorus, carbon, and energy by Shewanella spp.:ecological and physiological implications for dissimilatory metal reduction[J]. Applied and Environmental Microbiology, 2008,74(4):1198-1208.