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Updated: Mar 5, 2026

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes
Published on: August 5, 2016
Determination of ammonia nitrogen in solid and liquid high-complex matrices using one-step gas-diffusion
Inês M Valente1, Hugo M Oliveira2, Carlos D Vaz3
1REQUIMTE/LAQV - ICBAS, Departamento de Clínicas Veterinárias, Instituto de Ciências Biomédicas Abel Salazar, Universidade do Porto, Rua de Jorge Viterbo Ferreira no. 228, 4050-313 Porto, Portugal; REQUIMTE/LAQV - Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre no. 687, 4169-007 Porto, Portugal.
A new method simplifies ammonia nitrogen (NH3) determination in complex agricultural samples using gas diffusion microextraction (GDME) and fluorimetric labeling. This technique offers a sensitive, reproducible, and versatile approach for analyzing volatile compounds in various matrices.
Area of Science:
- Analytical Chemistry
- Environmental Science
- Agricultural Science
Background:
- Accurate determination of ammonia nitrogen (NH3) is crucial in agricultural and livestock sectors.
- Analyzing NH3 in complex solid and liquid matrices presents significant challenges.
- Existing methods may lack the sensitivity or simplicity required for diverse sample types.
Purpose of the Study:
- To develop a novel, one-step method for quantifying NH3 in complex agricultural samples.
- To utilize gas diffusion microextraction (GDME) coupled with fluorimetric labeling for simultaneous extraction and detection.
- To optimize the method for high sensitivity, repeatability, and broad applicability.
Main Methods:
- Simultaneous extraction and fluorimetric labeling of NH3 using gas diffusion microextraction (GDME).
- Application of o-phthalaldehyde (OPA) as a fluorimetric labeling reagent.
- Optimization of reaction conditions and GDME parameters via full factorial experimental design.
- Quantification using a 96-well microplate fluorescence reader.
Main Results:
- The optimized method achieved NH3 quantification in the range of 0.38–6.27 mgL⁻¹.
- High repeatability (4.5% RSD) and reproducibility (9.5% RSD) were demonstrated.
- An adequate limit of detection (0.22 mgL⁻¹) was achieved with a 10-minute extraction at 25°C.
- Successful application in diverse complex matrices like silages, feces, and urine.
Conclusions:
- The developed GDME-based method provides a simple, sensitive, and versatile approach for NH3 determination.
- This methodology is suitable for analyzing volatile components in high-complexity environmental and biological samples.
- The technique holds promise for future advancements in analytical chemistry for agricultural and related fields.
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