scholarly journals A Novel LC–MS/MS-Based Method for the Diagnosis of ADA2 Deficiency from Dried Plasma Spot

Molecules ◽  
2021 ◽  
Vol 26 (18) ◽  
pp. 5707
Author(s):  
Alessia Cafaro ◽  
Federica Pigliasco ◽  
Sebastiano Barco ◽  
Federica Penco ◽  
Francesca Schena ◽  
...  
Keyword(s):  
Autoinflammatory Disease ◽  
Chromosome Region ◽  
Accurate Determination ◽  
Enzymatic Assay ◽  
Tandem Mass ◽  
Cat Eye Syndrome ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Adenosine Deaminase 2

Adenosine Deaminase 2 Deficiency (DADA2) (OMIM: 607575) is a monogenic, autoinflammatory disease caused by the loss of functional homozygous or heterozygous mutations in the ADA 2 gene (previously CECR1, Cat Eye Syndrome Chromosome Region 1). A timely diagnosis is crucial to start Anti-TNF therapies that are efficacious in controlling the disease. The confirmation of DADA2 is based on DNA sequencing and enzymatic assay. It is, thus, very important to have robust and reliable assays that can be rapidly utilized in specialized laboratories that can centralize samples from other centers. In this paper, we show a novel enzymatic assay based on liquid chromatography-tandem mass spectrometry that allows the accurate determination of the ADA2 enzyme activity starting from very small amounts of plasma spotted on filter paper (dried plasma spot). The method allows significantly distinguishing healthy controls from affected patients and carriers and could be of help in implementing the diagnostic workflow of DADA2.

Method Validation for Quantitative Analysis of Metribuzin in Wheat by Liquid Chromatography–Tandem Mass Spectrometry

2020 ◽  
Vol 59 (1) ◽  
pp. 47-54
Author(s):  
Dipak Kumar Hazra ◽  
Aloke Purkait ◽  
Durgesh Raghuwanshi ◽  
K Sri Rama Murthy
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the accurate determination of metribuzin levels in wheat. The widespread use of this herbicide in the production of wheat is of concern and could follow as well as the need for methodology, which required simple sample preparation being needed. Validation of method was done as per single laboratory validation approach. Samples were extracted through a modified quick, cheap, effective, rugged and safe technique. Sample preparation includes extraction by acetonitrile solvent and cleans up by C18, primary secondary amine and anhydrous MgSO4 for dispersive solid-phase extraction. LC–MS/MS was calibrated at 5 calibration levels with high correlation coefficients (r2) >0.995. Limit of detection and limit of quantitation of metribuzin were 0.01 and 0.03 μg/g, respectively. The mean recovery percentages lie in the range of 87–97 with standard deviation for repeatability (RSDa) <10% at three spiking levels (0.03, 0.15 and 0.30 μg/g). Combined uncertainty (U = 0.0017) and expanded uncertainty (2U = 0.0033) were fairly consequential. The method may successfully be applied to other cereals samples for determination of metribuzin.

scholarly journals Determination of glyphosate and glufosinate in human serum by monospin TiO extraction and liquid chromatography–tandem mass spectrometry

2020 ◽  
Vol 32 (1) ◽  
pp. 10-15
Author(s):  
Takeshi Saito ◽  
Akira Namera ◽  
Tomoatsu Tsuji ◽  
Wataru Noguchi ◽  
Sadaki Inokuchi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Serum ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Serum Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

We developed and validated an assay for determination of glyphosate (GLYP) and glufosinate (GLUF) in human serum. Serum samples were extracted by using a MonoSpin® TiO column and analyzed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). MonoSpin® TiO tends to specifically bind to phosphate groups. The assay was linear over a concentration range of 1–250 μg/mL. The recoveries for the 2 compounds were 1.6%–2.3%. The intra- and inter-day variations were <15%. Precision and accuracy were 5.6%–12.7% and 97.0%–103.9%, respectively. The validated method was applied to quantify the GLYP and GLUF content in the serum of GLYP and GLUF-poisoned patients. In conclusion, the method was successfully applied for accurate determination of GLYP and GLUF in serum obtained from patients with GLYP and GLUF poisoning.

Sign in / Sign up

Export Citation Format

Share Document