scholarly journals Phosphorus Speciation in Surface Waters by Ion Chromatography With High Resolution Mass Spectrometry Detection

Author(s):  
Vlastimil Packa

Phosphorus (P) containing compounds, depending on their origin, can enter freshwater systems in variety of forms. Utilization of bioavailable P, a key nutrient in living organisms, is a crucial factor in biological productivity in aquatic environment¹. An increase in the P concentration in water, resulting from both natural and anthropogenic processes, can lead to eutrophication and an excessive growth of vegetative biomass. Determination of organic and inorganic P species in ground, surface and waster is an important part of water quality control and monitoring². Analytical determination of P compounds, quantification, identification (Chapter 2) and P speciation process can be problematic due to P adsorption on storage containers, sulfate interference, presence of acid hydrolysable P species and colloidal matter, association of both inorganic and organic phosphates with iron, manganese and aluminum, biological uptake of P. Such processes have to be considered when designing an analytical procedure for analysis of P species. Analytical P compound separation by ion chromatography with mass spectrometry/Orbitrap technology for compound detection (Chapter 3) is a powerful technology with highly sensitive and selective properties capable of performing P speciation in one analytical run. Selectivity of the Orbitrap detector also allows for utilization of isotope dilution technique which can compensate for loss of P compounds during storage and transportation and thus increase accuracy of measurements and holding time of sample matrices. Analytical techniques used in the past were able to determine broad P-fractions, such as total P, total P or functional groups of inorganic and organic P compounds. Identification of variety of specific P-containing compounds of inorganic and organic origin by the methodology used in this thesis in combination with multivariate statistical analysis can be used to explain the large sets of intercorrelated analytical variables with a smaller set of independent variables (Chapter 4) and help in source identification in water pollution studies³.

2021 ◽  
Author(s):  
Vlastimil Packa

Phosphorus (P) containing compounds, depending on their origin, can enter freshwater systems in variety of forms. Utilization of bioavailable P, a key nutrient in living organisms, is a crucial factor in biological productivity in aquatic environment¹. An increase in the P concentration in water, resulting from both natural and anthropogenic processes, can lead to eutrophication and an excessive growth of vegetative biomass. Determination of organic and inorganic P species in ground, surface and waster is an important part of water quality control and monitoring². Analytical determination of P compounds, quantification, identification (Chapter 2) and P speciation process can be problematic due to P adsorption on storage containers, sulfate interference, presence of acid hydrolysable P species and colloidal matter, association of both inorganic and organic phosphates with iron, manganese and aluminum, biological uptake of P. Such processes have to be considered when designing an analytical procedure for analysis of P species. Analytical P compound separation by ion chromatography with mass spectrometry/Orbitrap technology for compound detection (Chapter 3) is a powerful technology with highly sensitive and selective properties capable of performing P speciation in one analytical run. Selectivity of the Orbitrap detector also allows for utilization of isotope dilution technique which can compensate for loss of P compounds during storage and transportation and thus increase accuracy of measurements and holding time of sample matrices. Analytical techniques used in the past were able to determine broad P-fractions, such as total P, total P or functional groups of inorganic and organic P compounds. Identification of variety of specific P-containing compounds of inorganic and organic origin by the methodology used in this thesis in combination with multivariate statistical analysis can be used to explain the large sets of intercorrelated analytical variables with a smaller set of independent variables (Chapter 4) and help in source identification in water pollution studies³.


2020 ◽  
Vol 86 (8) ◽  
pp. 23-31
Author(s):  
V. G. Amelin ◽  
D. S. Bolshakov

The goal of the study is developing a methodology for determination of the residual amounts of quaternary ammonium compounds (QAC) in food products by UHPLC/high-resolution mass spectrometry after water-acetonitrile extraction of the determined components from the analyzed samples. The identification and determination of QAC was carried out on an «UltiMate 3000» ultra-high-performance liquid chromatograph (Thermo Scientific, USA) equipped with a «maXis 4G» high-resolution quadrupole-time-of-flight mass spectrometric detector and an ion spray «ionBooster» source (Bruker Daltonics, Germany). Samples of milk, cheese (upper cortical layer), dumplings, pork, chicken skin and ground beef were used as working samples. Optimal conditions are specified for chromatographic separation of the mixture of five QAC, two of them being a mixture of homologues with a linear structure (including isomeric forms). The identification of QAC is carried out by the retention time, exact mass of the ions, and coincidence of the mSigma isotopic distribution. The limits for QAC detection are 0.1 – 0.5 ng/ml, the determination limits are 1 ng/ml for aqueous standard solutions. The determinable content of QAC in food products ranges within 1 – 100 ng/g. The results of analysis revealed the residual amount of QAC present in all samples, which confirms data of numerous sources of information about active use of QAC-based disinfectants in the meat and dairy industry. The correctness of the obtained results is verified by introduction of the additives in food products at a level of 10 ng/g for each QAC. The relative standard deviation of the analysis results does not exceed 0.18. The duration of the analysis is 30 – 40 min.


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