Rapid determination of canagliflozin in rat plasma by UHPLC–MS/MS using negative ionization mode to avoid adduct-ions formation

Talanta ◽  
2015 ◽  
Vol 132 ◽  
pp. 29-36 ◽  
Author(s):  
Muzaffar Iqbal ◽  
Essam Ezzeldin ◽  
Khalid A. Al-Rashood ◽  
Yousif A. Asiri ◽  
Naser L. Rezk
Keyword(s):  
Rapid Determination ◽  
Rat Plasma ◽  
Negative Ionization Mode ◽  
Ionization Mode ◽  
Negative Ionization

Simultaneous Determination of 44 Pesticides in Tobacco by UPLC/MS/MS and a Modified QuEChERS Procedure

2013 ◽  
Vol 96 (2) ◽  
pp. 422-431 ◽  
Author(s):  
Xuyan Chen ◽  
Kongxiang Zhao ◽  
Baokun Ge ◽  
Qiyong Chen
Keyword(s):  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Modified Quechers ◽  
Negative Ionization Mode ◽  
Multiple Reaction Monitoring Mode ◽  
Primary Secondary Amine ◽  
Standard Calibration ◽  
Ionization Mode ◽  
Negative Ionization

Abstract A novel, simple, and rapid method for determination of the residues of 44 commonly used pesticides in tobacco was developed based on modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedures. The pesticides were extracted with acetonitrile and purified on a mixed sorbents column of primary secondary amine, C18, and graphitized carbon black. Quantitative determination of all pesticides was performed by ultra-performance LC/MS/MS in the positive or negative ionization mode by a single run due to the fast polarity switching capability of the mass spectrometer. Two precursor-product ion transitions were monitored for each compound in the multiple reaction monitoring mode. Quantification was carried out using matrix-matched standard calibration. The method has been validated by various tobacco cultivars, such as Burley, Oriental, and Virginia from different countries. Recoveries of the proposed method for spiked samples ranged from 71.1 to 109.8%, and RSD values were below 10%. The LOQ values were are all below the guidance residue levels proposed by the Agrochemical Advisory Committee of Cooperation Center for Scientific Research Relative to Tobacco. This method is valuable for measurement of pesticide residues in tobacco for QC and monitoring.

Simultaneous Determination of Nitrofuran Metabolites and Chloramphenicol in Shrimp with a Single Extraction and LC-MS/MS Analysis

2015 ◽  
Vol 98 (3) ◽  
pp. 595-601 ◽  
Author(s):  
Aref El-Demerdash ◽  
Fenhong Song ◽  
Robin K Reel ◽  
Judy Hillegas ◽  
Robert E Smith
Keyword(s):  
Extraction Procedure ◽  
Mode Switching ◽  
Selected Reaction Monitoring ◽  
Single Extraction ◽  
Ms Analysis ◽  
Negative Ionization Mode ◽  
Ionization Mode ◽  
Negative Ionization ◽  
Nitrofuran Metabolites

Abstract A method has been developed to quantify the nitrofuran metabolites 3-amino-5-morphorinomethyl-1,3-oxazolidinone, 3-amino-oxazolidinone, 1-aminohydantoin, and semicarbazide, as well as chloramphenicol in shrimp with a single extraction procedure followed by LC-MS/MS analysis. Dynamic selected reaction monitoring with positive and negative ionization mode switching was used. The method LODs were 0.5 ng/g for the nitrofuran metabolites and 0.3 ng/g for chloramphenicol.

scholarly journals Simultaneous Determination of 13 Constituents of Radix Polygoni Multiflori in Rat Plasma and Its Application in a Pharmacokinetic Study

2020 ◽  
Vol 2020 ◽  
pp. 1-10 ◽  
Author(s):  
Wenhao Cheng ◽  
Yinghui Li ◽  
Wei Yang ◽  
Siyang Wu ◽  
Mengmeng Wei ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Pharmacokinetic Study ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Limit Of Quantitation ◽  
Negative Ionization Mode ◽  
Negative Ionization

Radix Polygoni Multiflori (RPM) has been widely used to treat various diseases in Asian countries for many centuries. Although, stilbenes and anthraquinones, two major components of RPM, show various bioactive effects, it has been speculated that the idiosyncratic hepatotoxicity induced by RPM may be related to these constituents. However, information on the pharmacokinetics of stilbenes and anthraquinones at a subtoxic dose of RPM is limited. A simple and sensitive UPLC-MS/MS bioanalytical method for the simultaneous determination of 13 ingredients of RPM, including chrysophanol, emodin, aloe-emodin, rhein, physcion, questin, citreorosein, questinol, 2,3,5,4′-tetrahydroxystilbene-2-O-β-D-glucoside, torachrysone-8-O-glucoside, chrysophanol-8-O-β-D-glucoside, emodin-8-O-β-D-glucoside, and physcion-8-O-β-D-glucoside, in rat plasma was established. Acetonitrile was employed to precipitate the plasma with appropriate sensitivity and acceptable matrix effects. Chromatographic separation was performed using a waters HSS C18 column with a gradient elution using water and acetonitrile both containing 0.025% formic acid within a run time of 9 min. The constituents were detected in negative ionization mode using multiple reaction monitoring. The method was fully validated in terms of selectivity, linearity, accuracy, precision, recovery, matrix effects, and stability. The lower limit of quantitation of the analytes was 0.1–1 ng/mL. The intrabatch and interbatch accuracies were 87.1–109%, and the precision was within the acceptable limits. The method was applied to a pharmacokinetic study after oral administration of RPM extract to rats at a subtoxic dose of 36 g/kg.

scholarly journals Determination of Ten Corticosteroids in Illegal Cosmetic Products by a Simple, Rapid, and High-Performance LC-MS/MS Method

2017 ◽  
Vol 2017 ◽  
pp. 1-12 ◽  
Author(s):  
Vita Giaccone ◽  
Giuseppe Polizzotto ◽  
Andrea Macaluso ◽  
Gaetano Cammilleri ◽  
Vincenzo Ferrantelli
Keyword(s):  
High Performance ◽  
Skin Diseases ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Cosmetic Products ◽  
Chromatography Method ◽  
Esi Ms ◽  
Negative Ionization Mode ◽  
Negative Ionization

The aim of our present work was the development of a rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) for the determination of several corticosteroids in cosmetic products. Corticosteroids are suspected to be illegally added in cosmetic preparations in order to enhance the curative effect against some skin diseases. Sample preparation step consists in a single extraction with acetonitrile followed by centrifugation and filtration. The compounds were separated by reversed-phase chromatography with water and acetonitrile (both with 0.1% formic acid) gradient elution and detected by ESI-MS positive and negative ionization mode. The method was validated at the validation level of 0.1 mg kg−1. Linearity was studied in the 5–250 μg L−1 range and linear coefficients (r2) were all over 0.99. The accuracy and precision of the method were satisfactory. The LOD ranged from 0.085 to 0.109 mg kg−1 and the LOQ from 0.102 to 0.121 mg kg−1. Mean recoveries for all the analytes were within the range 91.9–99.2%. The developed method is sensitive and useful for detection, quantification, and confirmation of these corticosteroids in cosmetic preparations and can be applied in the analysis of the suspected samples under investigation.

scholarly journals Improved Small Molecule Identification through Learning Combinations of Kernel Regression Models

Metabolites ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 160 ◽  
Author(s):  
Céline Brouard ◽  
Antoine Bassé ◽  
Florence d’Alché-Buc ◽  
Juho Rousu
Keyword(s):  
Small Molecule ◽  
Kernel Regression ◽  
Feature Space ◽  
Molecular Structures ◽  
Subgradient Optimization ◽  
Hinge Loss ◽  
Fast Training ◽  
Negative Ionization Mode ◽  
Ionization Mode ◽  
Negative Ionization

In small molecule identification from tandem mass (MS/MS) spectra, input–output kernel regression (IOKR) currently provides the state-of-the-art combination of fast training and prediction and high identification rates. The IOKR approach can be simply understood as predicting a fingerprint vector from the MS/MS spectrum of the unknown molecule, and solving a pre-image problem to find the molecule with the most similar fingerprint. In this paper, we bring forward the following improvements to the IOKR framework: firstly, we formulate the IOKRreverse model that can be understood as mapping molecular structures into the MS/MS feature space and solving a pre-image problem to find the molecule whose predicted spectrum is the closest to the input MS/MS spectrum. Secondly, we introduce an approach to combine several IOKR and IOKRreverse models computed from different input and output kernels, called IOKRfusion. The method is based on minimizing structured Hinge loss of the combined model using a mini-batch stochastic subgradient optimization. Our experiments show a consistent improvement of top-k accuracy both in positive and negative ionization mode data.

scholarly journals Rapid Determination of Isomeric Benzoylpaeoniflorin and Benzoylalbiflorin in Rat Plasma by LC-MS/MS Method

2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Chuanqi Zhou ◽  
Xiaoke Wang
Keyword(s):  
Linear Response ◽  
Therapeutic Agent ◽  
Rapid Determination ◽  
Rat Plasma ◽  
Mass Spectrometric ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Bioanalytical Application ◽  
Tandem Mass Spectrometric

Benzoylpaeoniflorin (BP) is a potential therapeutic agent against oxidative stress related Alzheimer’s disease. In this study, a more rapid, selective, and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed to determine BP in rat plasma distinguishing with a monoterpene isomer, benzoylalbiflorin (BA). The method showed a linear response from 1 to 1000 ng/mL (r>0.9950). The precision of the interday and intraday ranged from 2.03 to 12.48% and the accuracy values ranged from −8.00 to 10.33%. Each running of the method could be finished in 4 minutes. The LC-MS/MS method was validated for specificity, linearity, precision, accuracy, recovery, and stability and was found to be acceptable for bioanalytical application. Finally, this fully validated method was successfully applied to a pharmacokinetic study in rats following oral administration.

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