scholarly journals Electrochemical Degradation of Carbamazepine: A Case Study of Quantification of “10, 11 Dihydro-10 Hydroxy Carbamazepine And 10, 11-Epoxycarbamazepine” As The Main By-Products Using LC-TOF/MS.

Author(s):  
Zainab Haider Mussa ◽  
Fouad Fadhil Al-Qaim

Abstract Carbamazepine (CBZ) is one of the most widely used antiepileptic drugs in Malaysia, so, it was detected in wastewater frequently. The electrochemical treatment process has been applied for the degradation of CBZ using graphite-PVC as an anode. However, two main by-products, namely, 10,11-dihydro10-hydroxy carbamazepine (HDX-CBZ) and 10,11-epoxycarbamazepine (EPX-CBZ) have been analysed and quantified using liquid chromatography-time of flight/mass spectrometry (LC-TOF/MS). HDX-CBZ and EPX-CBZ were analysed in positive ionisation mode and were separated chromatographically using 5 mm, 2 mm´150 mm C18 column at a flow rate of 0.3 mL/min. To improve sensitivity and detectability, SPE was applied as a pre-concentration step for the treated carbamazepine samples to extract and pre-concentrate HDX-CBZ and EPX-CBZ. However, three different solvents, namely, methyl tertiary butyl ether, acetone and methanol, have been optimized to enhance the recovery. The recovery was 85% and 92% for HDX-CBZ and EPX-CBZ, respectively, in the presence of methanol. The limit of quantification (LOQ) was 0.588 and 0.109 µg/L for both by-products, respectively. The concentration of HDX-CBZ and EPX-CBZ was 343 and 144 μg/L, respectively, after 20 min of treatment, then, it was decreased to 17.2 and 9.8 μg/L at 40 min. Finally, both by-products were eliminated after 60 min.

Catalysts ◽  
2018 ◽  
Vol 8 (11) ◽  
pp. 540
Author(s):  
Zainab Mussa ◽  
Fouad Al-Qaim ◽  
Ali Yuzir ◽  
Hirofumi Hara ◽  
Shamila Azman ◽  
...  

This paper describes an electrochemical treatment process of hydrochlorothiazide (HDZ) under different conditions such as initial concentration, sodium chloride and applied voltage. In this present study, HDZ was treated by electrochemical oxidation process using graphite-PVC composite electrode as anode and Platinum (Pt) as cathode. All results were analyzed using liquid chromatography-time of flight/mass spectrometry (LC-TOF/MS). It was found that at high applied voltages, and high amounts of NaCl, the electrochemical treatment process was more efficient. The removal% of HDZ was 92% at 5 V after 60 min. From the obtained results, the electrochemical oxidation process of HDZ followed pseudo first order with rate constant values ranged between 0.0009 and 0.0502 min−1, depending on the experimental conditions. Energy consumption was also considered in this study, it was ranged between 0.9058 and 5.56 Wh/mg using 0.5, 0.3 and 0.1 g NaCl within interval times of (10, 20, 30, 40, 50, 60, 70, and 80 min). Five chlorinated and one non-chlorinated by-products were formed and analyzed in negative ionization (NI) mode during the electrochemical process. Due to the strong oxidizing potential of the chlorine (Cl2) and hypochlorite ion (ClO−), HDZ and its by-products were removed after 140 min. Furthermore, a novel synthesis of chlorothiaizde as one of the new by-products was reported in this present study. Toxicity was impacted by the formation of the by-products, especially at 20 min. The inhibition percentage (I%) of E. coli bacteria was decreased to be the lowest value after 140 min.


2021 ◽  
Vol 68 (4) ◽  
pp. 811-820
Author(s):  
Zainab H. Mussa ◽  
Fouad F. Al-Qaim ◽  
Zahraa H. Alqaim ◽  
Jalifah Latip

This study reports electrochemical treatment of different therapeutic classes of pharmaceuticals (caffeine, prazosin, enalapril, carbamazepine, nifedipine, levonorgestrel, and simvastatin) in a mixture. The electrochemical process was investigated using graphite-PVC anode at different applied voltages (3, 5, and 12 V), initial concentrations of studied pharmaceuticals in aqueous solution (5 and 10 mg/L), and concentrations of sodium chloride (1 and 2 g/L). The % removal of pharmaceuticals increased with the applied voltage, and was found higher than 98% after 50 min of electrolysis at 5 V. Energy consumption ranged between 0.760 and 3.300 Wh/mg using 12 V being the highest value compared to 3 and 5 V. The formation of chlorinated by-products from four selected pharmaceuticals, simvastatin (C11H13Cl3O5, and C10H12 Cl4O3), prazosin (C13H12Cl3N5O3 and C10H11Cl4N2O2), carbamazepine and caffeine (C15H11N2O2Cl and C8H9N4O2Cl) was identified and elucidated using liquid chromatography-time of flight mass spectrometry (LC-TOF/MS).


2015 ◽  
Vol 65 (2) ◽  
pp. 159-169 ◽  
Author(s):  
Paweł Szpot ◽  
Grzegorz Buszewicz

Abstract This report presents the application of ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry with positive electrospray ionization, to determine ramipril in human plasma. First, the proteins in human plasma were precipitated using acetonitrile, then the supernatant was extracted by ethyl acetate at pH 3 and finally, the extract was analyzed using a UPLC-QTOF- MS system. The method was validated and the coefficient of determination (R2) was > 0.999, the lower limit of quantification (LLOQ) was 0.5 ng mL-1. Precision, recovery and stability were determined for three different concentrations of ramipril. RSD for this method ranged from 3.3 to 8.6 %. The intra-day mean recovery was from 65.3 to 97.3 %. In addition, the fragmentation of ramipril was studied. Due to high resolution of the spectrometer, it was possible to measure fragment masses accurately and determine their molecular and chemical formulas with high accuracy.


2021 ◽  
Vol 11 (9) ◽  
pp. 3788
Author(s):  
Lucía López-Salas ◽  
Isabel Borrás-Linares ◽  
David Quintin ◽  
Presentación García-Gomez ◽  
Rafael Giménez-Martínez ◽  
...  

Nowadays, the transformation activity of the food industry results in the generation of a huge amount of daily discarded vegetables wastes. One of those undervalued by-products are produced during the post-harvesting and processing process of artichokes. In the present research, the potential of artichokes’ bracts and stalks have been evaluated as a natural source of phenolic compounds which could be used as bioactive food ingredients, among others. In this study, the bioactive composition of those wastes has been evaluated using recent advances in extraction and analytical technologies, concretely, pressurized liquid extraction (PLE) followed by high-performance liquid chromatography (HPLC) coupled to electrospray time-of flight mass spectrometry (ESI-TOF/MS) analysis. To achieve this goal, first, the extraction process was evaluated by a comparative study using GRAS (Generally Recognized As Safe) solvents (mixtures of ethanol and water) at different temperatures (40–200 °C). The second step was to deeply characterize the composition of individual polyphenols by HPLC-ESI-TOF/MS in order to establish a comparison among the different PLE conditions applied to extract the phenolic fraction. The analysis revealed a wide variety of phenolic-composition, mainly phenolic acids and flavonoids. The results also highlighted that high percentages of ethanol and medium-high temperatures pointed out to be useful PLE conditions for recovering this kind of phytochemicals, which could be used in different applications, such as functional food ingredients, cosmetics, or nutraceuticals.


1970 ◽  
Vol 7 (1) ◽  
pp. 34-37
Author(s):  
R. K. Sharma ◽  
Dr.H. S. Shah ◽  
Dr. J.K. K Gohel

As a matter of fact, surgery (cholecystectomy or gall bladder removal) is the most common form of treatment for cholelithiasis (gallstones). However, the fact that surgically removing gallstones requires the removal of an entire organ has led to a growing interest in non-surgical treatments for gallstones. Besides alleviating symptoms, treatment for gallstones is necessary to avoid a progression that can result in severe conditions such as acute cholelithiasis. But so far as the medical management of cholelithiasis is concerned, it is not up to the mark in modern healing system. Although ursodiol or chenodiol in the form of oral bile acid pills, extracorporeal shock-wave lithotripsy (ESWL), contact dissolution therapy [injecting a solvent known a Methyl tertiary-butyl ether (MTBE) into the gallbladder to dissolve the gallstones], Percutaneous Cholecystostomy are good non-surgical measures, their roles are either limited or these are not free from adverse effects. Obviously, there is an urgent need of help from Alternative therapy to counter these difficulties. This article is a step in the direction of making an availability of a safe and effective non-surgical management of cholelithiasis to the ailing mankind.


Author(s):  
Hao A. O. Wang ◽  
Michael S. Krzemnicki

A concept of “first measure, then determine” which elements are of interest is introduced for multi-element analysis using LA-ICP-TOF-MS. Geochemical data visualization using t-SNE is advantageous over PCA for determining the provenances of emerald.


2006 ◽  
Vol 5 (5) ◽  
pp. 1085-1094
Author(s):  
Sudheer Kumar Shukla ◽  
Prerana Tripathi ◽  
Mukesh Pandey ◽  
Amit Dubey ◽  
Misra Shiv Mangal ◽  
...  

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