scholarly journals Accurate Determination of Amino Acids in Serum Samples by Liquid Chromatography–Tandem Mass Spectrometry Using a Stable Isotope Labeling Strategy

2015 ◽  
Vol 53 (9) ◽  
pp. 1536-1541 ◽  
Author(s):  
Cuihua Song ◽  
Shijuan Zhang ◽  
Zhongyin Ji ◽  
Yipeng Li ◽  
Jinmao You
Keyword(s):  
Mass Spectrometry ◽  
Amino Acids ◽  
Liquid Chromatography ◽  
Isotope Labeling ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Serum Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

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.

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) &gt;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) &lt;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 A Novel Method for the Determination of Vancomycin in Serum by High-Performance Liquid Chromatography-Tandem Mass Spectrometry and Its Application in Patients with Diabetic Foot Infections

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2939 ◽  
Author(s):  
Min Liu ◽  
Zhi-Hui Yang ◽  
Guo-Hui Li
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Diabetic Foot ◽  
High Performance ◽  
Tandem Mass ◽  
Serum Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

A novel, precise, and accurate high-performance liquid chromatography-tandem mass spectrometry (Q-trap-MS) method was developed, optimized, and validated for determination of vancomycin in human serum using norvancomycin as an internal standard. Effect of different parameters on the analysis was evaluated. ZORBAX SB-C18 column (150 × 4.6 mm, 5 μm) using water (containing 0.1% formic acid, v/v)–acetonitrile (containing 0.1% formic acid, v/v) as a mobile phase was chosen. The calibration curve was linear over the concentration ranges of 1 to 2000 ng/mL for vancomycin. The limit of detection (LOD) and limit of quantification (LOQ) for vancomycin were 0.3 and 1.0 ng/mL. Recoveries were between 87.2 and 102.3%, which gave satisfactory precision. A total of 100 serum samples (from 50 patients with diabetic foot proven Gram-positive infection and 50 nondiabetic patients with pneumonia requiring hospitalization and antibiotic therapy) were analyzed by this method. The trough vancomycin concentrations of diabetic foot infection (DFI) patients and nondiabetic patients were 8.20 ± 2.83 μg/mL (range: 4.80–14.2 μg/mL) and 15.80 ± 5.43 μg/mL (range: 8.60–19.5 μg/mL), respectively. The method is sensitive, precise, and reproducible, it could be applied for routine laboratory analysis of vancomycin in serum samples.

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