Quantification of a New Antifungal Drug Based on 1,3,4-Thiadiazole by HPLC-ESI/MS: Method Development, Validation and Pharmacokinetic Application

Drug Research ◽  
2021 ◽  
Author(s):  
Nadezhda Yur'evna Sipkina ◽  
Denis Igorevich Sipkin ◽  
Igor Pavlovich Yakovlev
Keyword(s):  
Method Development ◽  
Matrix Effects ◽  
Reversed Phase ◽  
Antifungal Drug ◽  
Absolute Calibration ◽  
Pharmacokinetic Parameters ◽  
Selected Ion Monitoring ◽  
Esi Ms ◽  
T Distribution

AbstractThe high sensitive HPLC-ESI/MS method for quantitative determination of a new antifungal drug – 2-[(1Z)-1-(3,5-diphenyl-1,3,4-thiadiazol-2(3Н)-ylidene)methyl]-3,5-diphenyl-1,3,4-thiadiazol-3-ium chloride (TDZ) – was developed and fully validated. TDZ was separated from plasma and urine samples by acetonitrile deproteinization and extraction without time-consuming sample preparation. The reversed-phase high-performance liquid chromatography on Kromasil 100–3.5 C8 column of TDZ in isocratic elution mode using 0.03% trifluoroacetic acid : acetonitrile (65:35, v/v) at a flow rate of 0.2 mL min−1 was performed. Determination of TDZ was carried out by a positive electrospray ionization in a selected ion monitoring mode for [M+]=489 m/z. The method of absolute calibration was used for quantification of TDZ in two concentrations ranges: 100–2500 pg mL−1 and 2500–30 000 pg mL−1. The established method showed a good linearity (R=0.999 for both ranges), the limits of determination and quantification were 50 and 100 pg mL−1, respectively. The Intra- and Inter-day precision values were measured by t-Distribution and Fisher′s Exact Test and were in accordance with the regulatory guidance. Low matrix effects and good recovery were found for TDZ. The present method was successfully applied to determine the pharmacokinetic parameters of TDZ by means of intravenous and oral administrations to rats at 5.0 mg kg−1 and 10.0 mg kg−1, respectively.

Determination of Glutamate and GABA Released by Mouse Embryonic Stem Cells Using HILIC-ESI-MS/MS

2020 ◽  
Vol 10 (2) ◽  
pp. 122-129
Author(s):  
Haoyu Lv ◽  
Yabin Tang ◽  
Fan Sun ◽  
Shimin An ◽  
Xinjie Yang ◽  
...  
Keyword(s):  
Stem Cells ◽  
Embryonic Stem Cells ◽  
Embryonic Stem ◽  
Mouse Embryonic Stem Cells ◽  
Reversed Phase ◽  
Water Soluble ◽  
Substitution Matrix ◽  
Neural Cells ◽  
Esi Ms

Background:In recent years, more and more researches have shown that neurotransmitters can also be synthesized and released by peripheral non-neural cells. However, specificity and high sensitivity detection means were required for confirming ESCs autocrine glutamate and γ - aminobutyric acid (GABA). Glutamate and GABA are water-soluble and polar compounds which cannot be retained on a reversed phase C18 column, and their contents are often at a trace level. On the other hand, the biological matrix such as cell culture fluid contains a large number of amino acids, vitamins, carbohydrates, inorganic ions and other substances. Therefore, the main problem is the selection of the chromatographic column to avoid matrix interference.Objective:To establish a rapid and reliable method for the simultaneous determination of glutamate and GABA released from embryonic stem cells based on analytical chemistry.Methods:Glutamate and GABA released from mouse embryonic stem cells were determined on the basis of hydrophilic interaction chromatography coupled with electrospray ionization tandem Mass Spectrometry (HILIC- ESI- MS/MS), using isotope internal standards and substitution matrix method.Results:Undifferentiated embryonic stem cells autocrine glutamate and GABA and will reach releasing- reuptacking dynamic equilibriums at different time points. In contrast, neither glutamate nor GABA releasing could be detected from the MEFs, indicating the specificity release of the mESCs in the applied analytic method.Conclusion:A novel, simple, sensitive, selective and quantitative method was developed for determination of the glutamate and GABA from mouse embryonic stem cells.

scholarly journals Application of Bar Adsorptive Microextraction for the Determination of Levels of Tricyclic Antidepressants in Urine Samples

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3101
Author(s):  
Mariana N. Oliveira ◽  
Oriana C. Gonçalves ◽  
Samir M. Ahmad ◽  
Jaderson K. Schneider ◽  
Laiza C. Krause ◽  
...  
Keyword(s):  
Tricyclic Antidepressants ◽  
Matrix Effects ◽  
Activated Carbons ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Experimental Conditions ◽  
Analytical Methodology ◽  
Low Efficiency

This work entailed the development, optimization, validation, and application of a novel analytical approach, using the bar adsorptive microextraction technique (BAμE), for the determination of the six most common tricyclic antidepressants (TCAs; amitriptyline, mianserin, trimipramine, imipramine, mirtazapine and dosulepin) in urine matrices. To achieve this goal, we employed, for the first time, new generation microextraction devices coated with convenient sorbent phases, polymers and novel activated carbons prepared from biomaterial waste, in combination with large-volume-injection gas chromatography-mass spectrometry operating in selected-ion monitoring mode (LVI-GC-MS(SIM)). Preliminary assays on sorbent coatings, showed that the polymeric phases present a much more effective performance, as the tested biosorbents exhibited low efficiency for application in microextraction techniques. By using BAμE coated with C18 polymer, under optimized experimental conditions, the detection limits achieved for the six TCAs ranged from 0.2 to 1.6 μg L−1 and, weighted linear regressions resulted in remarkable linearity (r2 > 0.9960) between 10.0 and 1000.0 μg L−1. The developed analytical methodology (BAμE(C18)/LVI-GC-MS(SIM)) provided suitable matrix effects (90.2–112.9%, RSD ≤ 13.9%), high recovery yields (92.3–111.5%, RSD ≤ 12.3%) and a remarkable overall process efficiency (ranging from 84.9% to 124.3%, RSD ≤ 13.9%). The developed and validated methodology was successfully applied for screening the six TCAs in real urine matrices. The proposed analytical methodology proved to be an eco-user-friendly approach to monitor trace levels of TCAs in complex urine matrices and an outstanding analytical alternative in comparison with other microextraction-based techniques.

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.

Specific and Sensitive RP-HPLC Method Development and Validation for the Determination of Aripiprazole: Application in Preformulation Screening of Nanoemulsion

2020 ◽  
Vol 10 (1) ◽  
pp. 76-86 ◽  
Author(s):  
Santosh A. Kumbhar ◽  
Chandrakant R. Kokare ◽  
Birendra Shrivastava ◽  
Hira Choudhury
Keyword(s):  
Quantitative Determination ◽  
Method Development ◽  
Developmental Stages ◽  
Reversed Phase ◽  
Hplc Method ◽  
Least Square ◽  
Formulation Development ◽  
Linear Calibration ◽  
Rp Hplc

Background: It has been hypothesized that delivery of aripiprazole through nanoemulsion formulation would better deliver the drug into the central nervous system to treat major depressive conditions in psychological patients. Due course of formulation development, to determine solubility of the drug in different matrices and nanoemulsion is an important step. Materials & Methods: Therefore, a simple, rapid and selective reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the determination of aripiprazole as per International Conference of Harmonization (ICH) guidelines. Satisfactory analysis method was employed for the quantitative determination of aripiprazole during pre-formulation development. Results and Discussion: The separation technique was achieved using the mobile phases of methanol-acetonitrile, 80:20 (v/v) delivered at 1.0 mL.min-1 flow rate through HIQ SIL C18 250x4.6 mm (5 μm particle size) column and detected at 218 nm wavelength. The method depicted linear calibration plots within the range of 5 to 50 µg.mL-1 with a determination coefficient (r2) of 0.9991 calculated by least square regression method. The validated method was sensitive with LOD of 10.0 ng.mL-1 and 30.0 ng.mL-1 of LOQ. The intra-day and inter-day precision values were ranged between 0.37-0.89 and 0.63-1.11 respectively, with accuracy ranging from 98.24 to 100.88 and 97.03 to 100.88, respectively. This developed and validated method was found to be sensitive for the determination of aripiprazole for the first time from various oils, surfactants, co-surfactants, and nanoemulsion formulation. Conclusion: This RP-HPLC method was successfully implemented for the quantitative determination of aripiprazole at developmental stages of nanoemulsion formulation.

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