ELECTROSPRAY IONIZATION MASS SPECTROMETRY FRAGMENTATION PATHWAYS OF SALTS OF SOME 1,2,4-TRIAZOLYLTHIOACETATE ACIDS, THE ACTIVE PHARMACEUTICAL INGREDIENTS

Objective: The goal of this research was to study fragmentation pathways of series salts of 1,2,4-triazolylthioacetate acids. Methods: The study was done in the Electrospray ionization source with single quadrupole mass spectrometer Agilent 6120 after elution through column Zorbax SB-C18, 30 mm × 4.6 mm, 1.8 μm at Agilent 1260 infinity high-performance liquid chromatography system. The series salts of 1,2,4-triazolylthioacetate acids were studied. These salts are active pharmaceutical ingredients of potential or registered pharmaceutical formulations. Results: The mass spectra of corresponding compounds have analyzed. The fragmentation patterns of these compounds decay have proposed. Conclusions: Studying the fragmentation of the indicated substances can be used for detecting the mentioned substances, as well as for confirming the structure of new compounds with the mass spectrum based on the patterns described above.

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Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

Revista de Chimie ◽

10.37358/rc.18.12.6799 ◽

2019 ◽

Vol 69 (12) ◽

pp. 3590-3592

Author(s):

Nela Bibire ◽

Romeo Iulian Olariu ◽

Luminita Agoroaei ◽

Madalina Vieriu ◽

Alina Diana Panainte ◽

...

Keyword(s):

High Performance ◽

Biological Fluids ◽

Gradient Elution ◽

High Performance Liquid Chromatographic ◽

Reversed Phase ◽

Assay Method ◽

Active Pharmaceutical Ingredients ◽

First Line ◽

Pharmaceutical Ingredients ◽

Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

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Analysis of Hydrolyzable Tannins and Other Phenolic Compounds in Emblic Leafflower (Phyllanthus emblica L.) Fruits by High Performance Liquid Chromatography–Electrospray Ionization Mass Spectrometry

Journal of Agricultural and Food Chemistry ◽

10.1021/jf302925v ◽

2012 ◽

Vol 60 (35) ◽

pp. 8672-8683 ◽

Cited By ~ 52

Author(s):

Baoru Yang ◽

Maaria Kortesniemi ◽

Pengzhan Liu ◽

Maarit Karonen ◽

Juha-Pekka Salminen

Keyword(s):

Mass Spectrometry ◽

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Phenolic Compounds ◽

Electrospray Ionization ◽

Electrospray Ionization Mass Spectrometry ◽

High Performance ◽

Ionization Mass ◽

Phyllanthus Emblica ◽

Hydrolyzable Tannins

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Diagnosis of Agglomeration and Crystallinity of Active Pharmaceutical Ingredients in Over the Counter Headache Medication by Electrospray Laser Desorption Ionization Mass Spectrometry Imaging

Molecules ◽

10.3390/molecules26030610 ◽

2021 ◽

Vol 26 (3) ◽

pp. 610

Author(s):

Mariann Inga Van Meter ◽

Salah M. Khan ◽

Brynne V. Taulbee-Cotton ◽

Nathan H. Dimmitt ◽

Nathan D. Hubbard ◽

...

Keyword(s):

Mass Spectrometry ◽

Mass Spectrometry Imaging ◽

Laser Desorption ◽

Ionization Mass Spectrometry ◽

Ionization Mass ◽

Active Pharmaceutical Ingredients ◽

Laser Desorption Ionization ◽

Over The Counter ◽

Pharmaceutical Ingredients ◽

Desorption Ionization

Agglomeration of active pharmaceutical ingredients (API) in tablets can lead to decreased bioavailability in some enabling formulations. In a previous study, we determined that crystalline APIs can be detected as agglomeration in tablets formulated with amorphous acetaminophen tablets. Multiple method advancements are presented to better resolve agglomeration caused by crystallinity in standard tablets. In this study, we also evaluate three “budget” over-the-counter headache medications (subsequently labeled as brands A, B, and C) for agglomeration of the three APIs in the formulation: Acetaminophen, aspirin, and caffeine. Electrospray laser desorption ionization mass spectrometry imaging (ELDI-MSI) was used to diagnose agglomeration in the tablets by creating molecular images and observing the spatial distributions of the APIs. Brand A had virtually no agglomeration or clustering of the active ingredients. Brand B had extensive clustering of aspirin and caffeine, but acetaminophen was observed in near equal abundance across the tablet. Brand C also had extensive clustering of aspirin and caffeine, and minor clustering of acetaminophen. These results show that agglomeration with active ingredients in over-the-counter tablets can be simultaneously detected using ELDI-MS imaging.

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Encapsulation of Active Pharmaceutical Ingredients in Lipid Micro/Nanoparticles for Oral Administration by Spray-Cooling

Pharmaceutics ◽

10.3390/pharmaceutics13081186 ◽

2021 ◽

Vol 13 (8) ◽

pp. 1186

Author(s):

Carmen S. Favaro-Trindade ◽

Fernando E. de Matos Junior ◽

Paula K. Okuro ◽

João Dias-Ferreira ◽

Amanda Cano ◽

...

Keyword(s):

Oral Administration ◽

Raw Materials ◽

Low Cost ◽

Pharmaceutical Formulations ◽

Spray Cooling ◽

Active Pharmaceutical Ingredients ◽

Pharmaceutical Ingredients ◽

Taste And Odor ◽

Cooling Technology ◽

Simple Technology

Nanoencapsulation via spray cooling (also known as spray chilling and spray congealing) has been used with the aim to improve the functionality, solubility, and protection of drugs; as well as to reduce hygroscopicity; to modify taste and odor to enable oral administration; and many times to achieve a controlled release profile. It is a relatively simple technology, it does not require the use of low-cost solvents (mostly associated to toxicological risk), and it can be applied for lipid raw materials as excipients of oral pharmaceutical formulations. The objective of this work was to revise and discuss the advances of spray cooling technology, with a greater emphasis on the development of lipid micro/nanoparticles to the load of active pharmaceutical ingredients for oral administration.

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