Glycan reducing end dual isotopic labeling (GREDIL) for mass spectrometry-based quantitative N-glycomics

2015 ◽  
Vol 51 (71) ◽  
pp. 13603-13606 ◽  
Author(s):  
Weiqian Cao ◽  
Wei Zhang ◽  
Jiangming Huang ◽  
Biyun Jiang ◽  
Lijuan Zhang ◽  
...  

GREDIL for quantitative N-glycomics largely improves the stability of N-glycan 18O-labeling and greatly decreases the interference of isotopic cluster overlap.

Metabolites ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 277
Author(s):  
Sabrina Krautbauer ◽  
Raquel Blazquez ◽  
Gerhard Liebisch ◽  
Marcus Hoering ◽  
Philip Neubert ◽  
...  

Lipids are a ubiquitous class of structurally complex molecules involved in various biological processes. In the fast-growing field of lipidomics, preanalytical issues are frequently neglected. Here, we investigated the stability of lipid profiles of murine liver, brain, lung, heart, and spleen homogenates by quantitative flow injection analysis using tandem mass spectrometry and high-resolution mass spectrometry. Storage of tissue homogenates at room temperature showed substantial alterations of the lipid profiles reflecting lipolytic action. Therefore, ratios of ceramide to sphingomyelin, lysophosphatidylethanolamine to phosphatidylethanolamine, lysophosphatidylcholine to phosphatidylcholine, and diglyceride to triglyceride were applied to monitor sample stability and the effect of sodium dodecyl sulfate (SDS) as a potential stabilizing agent. The addition of SDS led to a concentration-dependent stabilization of lipid profiles in liver, brain, and heart homogenates, while in lung and spleen homogenates, in particular, the lysophosphatidylethanolamine to phosphatidylethanolamine ratio increased upon addition of SDS. In conclusion, we demonstrated that lipid class ratios reflecting lipolytic activity could be applied to evaluate both the stability of samples and the influence of stabilizers.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Priyanka Verma ◽  
Atul Bajaj ◽  
R. M. Tripathi ◽  
Sudhir K. Shukla ◽  
Suman Nagpal

Abstract Background Recent advances in the diversified anti-diabetic drugs have appeared in the startling increase in the count of poisoning cases. The epidemics of diabetes mellitus are increasing; hence, the no. of anti-diabetic drug users raised by 42.9%. The use of glimepiride raised to 24%. As the toxicity and drug cases are also escalating with increasing epidemics of diabetes mellitus, a novel gas chromatography-mass spectrometry (GC-MS) method for detecting glimepiride in biological matrices is developed. Results Liquid-liquid extraction method was employed by using 1-butanol: hexane (50:50, v/v) under an alkaline medium, and then back extraction was done via acetic acid. Distinct derivatization techniques were employed for the sample preparation for GC-MS analysis, i.e., silylation and acylation. Derivatization approaches were optimized under different parameters, i.e., reaction temperature and reaction time. N-Methyl-N-(trimethylsilyl) trifluoroacetamide [MSTFA] was found to be the best sound derivatization reagent for the GC-MS analysis of glimepiride. Total ion current (TIC) mode was selected for the monitoring of ions of trimethylsilyl (TMS) derivative of glimepiride with an m/z ratio of 256. Distinct parameters like specificity, carryover, stability, precision, and accuracy were evaluated for validating the identification method. The GC-MS method is found to be linear and illustrated within the range 500 to 2500 ng/ml with the value of R2 (coefficient of determination) at 0.9924. The stability of the extracted and derivatized glimepiride was accessed with regard to processed/extracted sample conditions and autosampler conditions, respectively. Accuracy at each concentration level was within the + 15% of the nominal concentration. Precision (%) for the interday and intraday analysis was found to be in the respectable spectrum. Conclusion Henceforth, the proposed GC-MS method can be employed for the determination of glimepiride in biological matrices.


2020 ◽  
Author(s):  
Mathieu Tiquet ◽  
Raphaël La Rocca ◽  
Daan van Kruining ◽  
Pilar Martinez-Martinez ◽  
Gauthier Eppe ◽  
...  

<p><i>MALDI mass spectrometry imaging (MSI) is a powerful analytical method giving access to the 2D localizations of compounds in a thin section of a sample. To properly discern isobaric compounds in complex biological samples, dynamically harmonized ICR cell (ParaCell©) has been introduce to achieve extreme spectral resolution. However, high resolution MS images realized on a 9.4T FTICR High resolution instrument with recommended parameters suffered from an abnormal shifting of m/z ratios pixel to pixel. Resulting datasets show poor mass accuracy measurements and resolutions under estimations. By following the behavior of the Total Ion Current in function of the number of laser shots, the abnormal mass shifting phenomenon has been linked to the stability of the Total Ion Current (TIC) during images acquisitions. An optimization of laser parameters is proposed in order to limit the observed mass shift to retain machine specifications during MSI analyses. It is also shown that the method has been successfully employed to realize quality MS images with resolution above 1,000,000 in the lipid mass range across the whole image.</i></p>


Processes ◽  
2019 ◽  
Vol 7 (12) ◽  
pp. 954 ◽  
Author(s):  
Daria Bożejewicz ◽  
Katarzyna Witt ◽  
Małgorzata A. Kaczorowska ◽  
Borys Ośmiałowski

A new compound 2,6-bis(4-methoxybenzoyl)-diaminopyridine (L) was used as an extractant for copper(II) ion recovery in a solvent extraction conducted at a temperature of 25 °C. The best results (99% recovery of copper(II) ions) were obtained when the aqueous phase contained 0.001 mol/dm3 Cu(II) and 0.2 mol/dm3 NH3 (pH~5.8), while the organic phase was a 0.001 mol/dm3 chloroform solution of 2,6-bis(4-methoxybenzoyl)-diaminopyridine. Spectrophotometry studies were used to determine the dissociation constant of the tested compound and determine the stability constant of the complex of subjected compound with copper(II) ions. The high-resolution mass spectrometry (HRMS) and higher energy collisional dissociation tandem mass spectrometry (HCD MS/MS) methods have been applied for the confirmation of the structure of 2,6-bis(4-methoxybenzoyl)-diaminopyridine and to determine its complexation with Cu(II) in solution.


Biochemistry ◽  
2002 ◽  
Vol 41 (25) ◽  
pp. 8013-8018 ◽  
Author(s):  
A. P. M. de Brouwer ◽  
C. Versluis ◽  
J. Westerman ◽  
B. Roelofsen ◽  
A. J. R. Heck ◽  
...  

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