HPLC method for the analysis of the urease inhibitor N-(n-butyl)thiophosphoric triamide and its metabolites

Douglass, E.A.; Hendrickson, L. L.

doi:10.1021/jf00012a045

Cited by 10 publications

(8 citation statements)

References 7 publications

(9 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…NBPT and NBPTo are polar residues and can be retained on reverse-phase HPLC systems. Douglass and Hendrickson [116] reported an early method that allowed the simultaneous analysis of NBPT and NBPTo using a C 18 separation and post-column derivatization with fluorescence detection (Figure 3). Following separation, the analytes were sequentially hydrolyzed to n-butylamine with nitric acid at 155 • C and then converted to fluorescent derivatives using o-phthaladehyde (OPA).…”

Section: Analytical Methods For the Detection Of Inhibitors In Complex Milk And Environmental Matricesmentioning

confidence: 99%

Urease and Nitrification Inhibitors—As Mitigation Tools for Greenhouse Gas Emissions in Sustainable Dairy Systems: A Review

et al. 2020

View full text Add to dashboard Cite

Currently, nitrogen fertilizers are utilized to meet 48% of the total global food demand. The demand for nitrogen fertilizers is expected to grow as global populations continue to rise. The use of nitrogen fertilizers is associated with many negative environmental impacts and is a key source of greenhouse and harmful gas emissions. In recent years, urease and nitrification inhibitors have emerged as mitigation tools that are presently utilized in agriculture to prevent nitrogen losses and reduce greenhouse and harmful gas emissions that are associated with the use of nitrogen-based fertilizers. Both classes of inhibitor work by different mechanisms and have different physiochemical properties. Consequently, each class must be evaluated on its own merits. Although there are many benefits associated with the use of these inhibitors, little is known about their potential to enter the food chain, an event that may pose challenges to food safety. This phenomenon was highlighted when the nitrification inhibitor dicyandiamide was found as a residual contaminant in milk products in 2013. This comprehensive review aims to discuss the uses of inhibitor technologies in agriculture and their possible impacts on dairy product safety and quality, highlighting areas of concern with regards to the introduction of these inhibitor technologies into the dairy supply chain. Furthermore, this review discusses the benefits and challenges of inhibitor usage with a focus on EU regulations, as well as associated health concerns, chemical behavior, and analytical detection methods for these compounds within milk and environmental matrices.

show abstract

Section: Analytical Methods For the Detection Of Inhibitors In Complex Milk And Environmental Matricesmentioning

confidence: 99%

Urease and Nitrification Inhibitors—As Mitigation Tools for Greenhouse Gas Emissions in Sustainable Dairy Systems: A Review

et al. 2020

View full text Add to dashboard Cite

show abstract

“…To investigate the possibility that ingested NBPT is transferred to milk or meat in cattle or other livestock populations, development and validation of a sensitive analytical method to detect NBPT residues in livestock tissues and milk is critically needed. A high-performance liquid chromatography (HPLC) method has been published for NBPT and its metabolites in soil samples ( Douglass and Hendrickson, 1991 ); however, an analytical method for NBPT in animal milk and tissues was not identified. For this reason, a liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated to meet the study objective, ensuring sufficient sensitivity to detect low concentrations of NBPT residue in milk products (milk, skim milk, and cream) and selected tissues of cattle.…”

Section: Introductionmentioning

confidence: 99%

Nondetectable or minimal detectable residue levels of N-(n-butyl) thiophosphoric triamide in bovine tissues and milk from a 28-d NBPT dosing study

Ligt

Borghoff

Yoon

et al. 2019

Translational Animal Science

View full text Add to dashboard Cite

N-(n-butyl) thiophosphoric triamide (NBPT) (Figure 1) is an active ingredient in nitrogen stabilizer (urease inhibitor), which temporarily inhibits the action of the urease enzyme to improve the efficiency of urea-containing fertilizers. Given the potential for NBPT residues to be present in milk and tissues of dairy cattle, due diligence is needed to demonstrate the safety of NBPT in urea-based fertilizers used on forages and crops intended for consumption by Holstein dairy cows. This study used controlled dosing of NBPT in capsule form to dairy cattle for 28 d, followed by a 14-d depuration phase to assess the potential for residues to exist in milk and tissues of dairy cattle at exaggerated use levels. Fourteen lactating cows were selected for the dosing and depuration phases of the study, based on health, body weight (BW), and milk production. There were four treatment groups: 0 mg NBPT/kg BW (Control) (n = 2 cows), 1 mg NBPT/kg BW (1×) (n = 3 cows), 3 mg NBPT/kg BW (3×) (n = 3 cows), and 10 mg NBPT/kg/BW (10×) (n = 6 cows); levels were based on maximum tolerable amount of urea that a cow can ingest on a daily basis (1×) and the maximum concentration of NBPT commercially used when treating urea (0.1 wt% NBPT in urea). At the end of the 28-d dosing phase, cows were randomly selected for the 14-d depuration phase of the study (one control and three 10× cows). The results showed no NBPT residue is detectable at all dose levels, except that a residue level was above the lower limit of quantitation in a single milk and subcutaneous fat sample in the highest (10×) treatment group, which represents the level of NBPT that would be theoretically present in 10× the lethal dosing of daily consumable urea to a cow. Overall, the study demonstrated that it is unlikely for NBPT residues to be present in cattle milk or edible tissues or to cause negative effects on animal health under good agricultural practice.

show abstract

“…The purpose of this work was to develop a new simple analytical method to determine simultaneously NBPT and DCD in urea formulation by LC–MS/MS. To achieve good separation of NBPT and DCD in urea matrix, different columns reported in the literature were tried such as Zorbax‐Rx C‐8 column , RRHD C18 , Hypersil 5 Phenomenex, C18 . Also, various mobile phase compositions consisting of acidified water with formic acid or Phosphoric acid or ammonium acetate buffer with water and acetonitrile in an isocratic mode were tried.…”

Section: Resultsmentioning

confidence: 99%

“…It is important to have single analytical method to monitor them in final product for quality control purpose and also to understand the stability of inhibitors under different environmental storage conditions, which aid in developing efficient formulation of urea containing inhibitors for crop applications. From the prior art analysis, it was found that various researchers have reported HPLC or HPLC‐MS methods to quantify NBPT and DCD individually in various matrices such as urea, other fertilizers, soils, water and in food applications. However, there is no single method reported in literature for simultaneous estimation of NBPT and DCD in urea or any other matrix.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous quantification of N‐butylthiophosphoric triamide and dicyandiamide in urea formulation by liquid chromatography with tandem mass spectrometry

Yogesha¹,

Kumar²,

Shetty³

et al. 2018

J of Separation Science

View full text Add to dashboard Cite

A new liquid chromatography with tandem mass spectrometry method employing a mixed‐mode zwitterionic stationary phase was developed for simultaneous determination of urease inhibitor (N‐butylthiophosphoric triamide) and nitrification inhibitor (dicyandiamide) in urea fertilizer. Molecular modeling based on density functional theory calculations was employed to provide an insight into the interaction mechanism of urea, dicyandiamide, and N‐butylthiophosphoric triamide with zwitterionic stationary phase in chromatographic separation system. The detection of analytes was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode using positive electrospray ionization. The ion transitions monitored were m/z 85→68 for dicyandiamide and m/z 168.2→74 for N‐butylthiophosphoric triamide, respectively. The standard calibration curves of dicyandiamide and N‐butylthiophosphoric triamide were linear over the range of 1.0 ̶ 15 ppm (coefficient of determination = 0.9984), 0.05 ̶ 1 ppm (coefficient of determination = 0.9995), with limit of detection of 25 and 5 ppb, respectively. The recoveries of low, middle, and high concentrations were from 96.7 to 105.8% for N‐butylthiophosphoric triamide and 94.4 to 105.8% for dicyandiamide with accuracy (relative error %) of ≤5.8% and ≤5.8%, the precision (coefficients of variation) was ≤2.0% and ≤2.9%, respectively. The validated method was successfully applied on real urea samples to determine N‐butylthiophosphoric triamide and dicyandiamide simultaneously.

show abstract

HPLC method for the analysis of the urease inhibitor N-(n-butyl)thiophosphoric triamide and its metabolites

Cited by 10 publications

References 7 publications

Urease and Nitrification Inhibitors—As Mitigation Tools for Greenhouse Gas Emissions in Sustainable Dairy Systems: A Review

Urease and Nitrification Inhibitors—As Mitigation Tools for Greenhouse Gas Emissions in Sustainable Dairy Systems: A Review

Nondetectable or minimal detectable residue levels of N-(n-butyl) thiophosphoric triamide in bovine tissues and milk from a 28-d NBPT dosing study

Simultaneous quantification of N‐butylthiophosphoric triamide and dicyandiamide in urea formulation by liquid chromatography with tandem mass spectrometry

Contact Info

Product

Resources

About