scholarly journals Development of an UPLC-MS/MS Method for the Analysis of Mycotoxins in Rumen Fluid with and without Maize Silage Emphasizes the Importance of Using Matrix-Matched Calibration

Toxins ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 519 ◽  
Author(s):  
Sandra Debevere ◽  
Siegrid De Baere ◽  
Geert Haesaert ◽  
Michael Rychlik ◽  
Veerle Fievez ◽  
...  
Keyword(s):  
Analytical Method ◽  
Western Europe ◽  
Matrix Effects ◽  
Rumen Fluid ◽  
Ultra Performance Liquid Chromatography ◽  
Potential Interaction ◽  
Maize Silage ◽  
Rumen Microbiota ◽  
Mycotoxin Degradation ◽  
Liquid Chromatography Tandem Mass

Ruminants are less susceptible to the effects of mycotoxins than monogastric animals as their rumen microbiota are claimed to degrade and/or deactivate at least some of these toxic compounds. However, the mycotoxin degradation is not well-known yet. For this, a sensitive, specific, and accurate analytical method is needed to determine mycotoxins in the rumen fluid. This study aims to develop and thoroughly validate an ultra-performance liquid chromatography tandem mass spectrometry method for the quantitative determination in the rumen fluid of some of the most relevant mycotoxins found in maize silage in Western Europe: deoxynivalenol (DON), nivalenol (NIV), zearalenone (ZEN), mycophenolic acid (MPA), roquefortine C (ROQ-C) and enniatin B (ENN B), as well as their metabolites deepoxy-deoxynivalenol (DOM-1), α-zearalenol (α-ZEL), β-zearalenol (β-ZEL), zearalanone (ZAN), α-zearalanol (α-ZAL) and β-zearalanol (β-ZAL). As feed is often present in the rumen fluid samples, the potential interaction of feed particles with the mycotoxin extraction and analysis was investigated. Extraction recovery and matrix effects were determined in the rumen fluid with and without maize silage. Differences in those parameters between rumen fluid alone and rumen fluid with maize silage highlight the importance of using matrix-matched calibration curves for the quantification of mycotoxins in rumen fluid samples. A cross-validation of the method with rumen fluid and maize silage demonstrates that this analytical method can be applied in research on rumen fluid samples to investigate the degradation of the reported mycotoxins by rumen microbiota if matrix-matched calibration is performed.

Determination of 12 Carbamate Insecticides in Typical Vegetables and Fruits by Rapid Multi-Plug Filtration Cleanup and Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry Detection

2019 ◽  
Vol 58 (2) ◽  
pp. 109-116
Author(s):  
Lili Ma ◽  
Liuwei Zhao ◽  
Jiaqi Wang ◽  
Canping Pan ◽  
Cong Liu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Matrix Effects ◽  
Solid Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Vegetables And Fruits

Abstract A multiresidue method for determining 12 carbamate pesticides in purple cabbage, orange, watermelon, cucumber, cowpea and Lactuca sativa L. employing multi-plug filtration cleanup (m-PFC) and ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was developed. M-PFC was carried out by cleanup at dispersive solid phase extraction (d-SPE), one m-PFC tip-filtration, two m-PFC tip-filtration and other methods (1–3 m-PFC cleanups). Results demonstrated that filtration simplified the cleanup method compared with d-SPE and other m-PFC methods (1–3 m-PFC cleanups). The method validation results showed that the method was linear, selective and accurate. The limits of quantification (LOQs) were 0.05–5.0 μg/kg, and the recoveries were in the range of 70.1–119.9% in different matrices. Although matrix effects were observed, they were successfully compensated using matrix-matched calibration. Finally, the developed method was successfully applied to detect pesticides in real samples.

Determination of Residues of Seven Carbamate Pesticides in Milk Using Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry and QuEChERS Methods

2013 ◽  
Vol 96 (3) ◽  
pp. 657-662 ◽  
Author(s):  
Shao-Ying Liu ◽  
Quan Jin ◽  
Xi-Hui Huang ◽  
Guo-Nian Zhu
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Analytical Method ◽  
Multiple Reaction Monitoring ◽  
High Sensitivity ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Modified Quechers ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode

Abstract An improved analytical method was developed for simultaneous quantification of seven carbamates in milk by ultra-performance LC combined with electrospray ionization triple quadrupole tandem mass spectrometry in the multiple reaction monitoring mode. Samples were extracted and purified using a modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. The LOQs ranged from 0.033 to 0.23 μg/kg; reasonable recoveries (85.4 to 110.9%) of the seven carbamates in milk were demonstrated at different spike levels. The developed analytical method would be appropriate for the routine, high throughput, high sensitivity quantification of the seven carbamates using modified QuEChERS pretreatment.

An UPLC-MS/MS Method for Routine Quantification of Insulin Degludec in Plasma

2020 ◽  
Vol 16 (6) ◽  
pp. 792-799
Author(s):  
Yudong Zhang ◽  
Yue Jiang ◽  
Ya Wang ◽  
Ling Wang ◽  
Weijie Han ◽  
...  
Keyword(s):  
Formic Acid ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Subcutaneous Administration ◽  
Ultra Performance Liquid Chromatography ◽  
Insulin Degludec ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Acquity Uplc

Background: Chromatographic methods for determination of insulin degludec in rabbit plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry were developed. Methods: Analytes were eluted from Waters ACQUITY UPLC® Peptide BEH C18 (2.1×50mm, 300Å) column with a mobile phase of water containing 0.1% formic acid (A) and acetonitrile containing 0.1% formic acid (B). Quantitation of insulin degludec was performed using 1222.06 > 641.24 m/z on Multiple- Reaction Monitoring (MRM) mode. Results: Good linearity was observed in the concentration range of 500-50000 ng/mL (r >0.99), and the lower limit of quantification was 500ng/mL. The within-run and between-run precision (expressed as relative standard deviation, RSD) of insulin degludec were ≤ 14.16% and ≤ 13.64% respectively, and the accuracy was within 94.37-96.35%. The recovery and matrix effects were both within acceptable limits. Conclusion: This method was successfully applied for the pharmacokinetic study of insulin degludec in rabbit after subcutaneous administration.

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