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Journal of Analytical Methods in Chemistry

Danielle Cristina da Silva, Cláudio Celestino Oliveira
Method for extraction and determination of amoxicillin, caffeine, ciprofloxacin, norfloxacin, tetracycline, diclofenac, ibuprofen, nimesulide, levonorgestrel, and 17 α -ethynylestradiol exploiting micellar liquid chromatography with PDA detector and solid-phase extraction was proposed. The usage of toxic solvents was low; the chromatographic separation of the medicaments was performed using a C18 column and mobile phases A and B containing 15.0% (v/v) ethanol, 3.0% (m/v) sodium dodecyl sulfate (SDS), and 0...
2018: Journal of Analytical Methods in Chemistry
Francesca Buiarelli, Patrizia Di Filippo, Carmela Riccardi, Donatella Pomata, Riccardo Marsiglia, Carla Console, Daniele Puri
Fosetyl-aluminum is a synthetic fungicide administered to plants especially to prevent diseases caused by the members of the Peronosporales and several Phytophthora species. Herein, we present a selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyze residues of fosetyl-A1 in air particulate matter. This study was performed in perspective of an exposure assessment of this substance of health concern in environments where high levels of fosetly-Al, relatively to airborne particulate matter, can be found after spraying it...
2018: Journal of Analytical Methods in Chemistry
Svetla Todinova, Yuliana Raynova, Krassimira Idakieva
The thermal unfolding of hemocyanin isoforms, β -HaH and α D + N -HaH, isolated from the hemolymph of garden snails Helix aspersa maxima, was studied by means of differential scanning calorimetry (DSC). One transition, with an apparent transition temperature ( T m ) at 79.88°C, was detected in the thermogram of β -HaH in 20 mM HEPES buffer, containing 0.1 M NaCl, 5 mM CaCl2, and 5 mM MgCl2 , pH 7.0, at scan rate of 1.0°C min-1 . By means of successive annealing procedure, two individual transitions were identified in the thermogram of α D + N -HaH...
2018: Journal of Analytical Methods in Chemistry
Sriram Valavala, Nareshvarma Seelam, Subbaiah Tondepu, V Shanmukha Kumar Jagarlapudi, Vivekanandan Sundarmurthy
A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modified release capsules. The residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modified release capsules by considering the solubility of the dipyridamole and excipients in the different manufacturing stages. The method was developed and optimized by using fused silica DB-624 (30 m × 0...
2018: Journal of Analytical Methods in Chemistry
Bashir Daoud Agha Dit Daoudy, Mohammad Ammar Al-Khayat, Francois Karabet, Mohammad Amer Al-Mardini
Formaldehyde is a highly reactive impurity that can be found in many pharmaceutical excipients. Trace levels of this impurity may affect drug product stability, safety, efficacy, and performance. A static headspace gas chromatographic method was developed and validated to determine formaldehyde in pharmaceutical excipients after an effective derivatization procedure using acidified ethanol. Diethoxymethane, the derivative of formaldehyde, was then directly analyzed by GC-FID. Despite the simplicity of the developed method, however, it is characterized by its specificity, accuracy, and precision...
2018: Journal of Analytical Methods in Chemistry
Kátia S D Nunes, Márcia R Assalin, José H Vallim, Claudio M Jonsson, Sonia C N Queiroz, Felix G R Reyes
A multiresidue method for detecting and quantifying sulfonamides (sulfapyridine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfamethoxypyridazine) and trimethoprim in tilapia fillet ( Oreochromis niloticus ) using liquid chromatography coupled to mass spectrometry was developed and validated. The sample preparation was optimized using the QuEChERS approach. The chromatographic separation was performed using a C18 column and 0.1% formic acid in water and acetonitrile as the mobile phase in the isocratic elution mode...
2018: Journal of Analytical Methods in Chemistry
Ding-Qiang Luo, Shan-Shan Zhao, Yu-Rong Tang, Qing-Jun Wang, Hai-Jing Liu, Shuang-Cheng Ma
To evaluate the effect of 60 Co-γ irradiation sterilization technology on the chemical composition of saffron, we collected 10 batches of saffron samples and treated them with different irradiation doses. UPLC characteristic chromatogram showed that there was no significant effect of irradiation on 13 common peak areas. The results of cluster analysis and principal component analysis showed that there were no differences in the chemical composition in nonirradiated and irradiated samples. UPLC/Q-TOF-MS identified 40 characteristic components of saffron, and the results showed that all of these were detected in the saffron samples both with and without irradiation...
2018: Journal of Analytical Methods in Chemistry
Babiker Yagoub Abdulkair, Amin O Elzupir, Abdulaziz S Alamer
An accurate IPC-UV method was developed and validated for the determination of nitrite (NI) and nitrate (NA) in meat products. The best separation was achieved on a phenyl-hexyl column (150 mm × 4.6 mm, 3  µ m) with a mobile phase composed of 25% acetonitrile and 75% buffer (2 mM disodium hydrogen phosphate and 3 mM tetrabutylammonium bromide, pH = 4). Eluents were monitored at 205 nm. Linearity ranges were 1.86 × 10-6 -7.5  µ g·ml-1 and 0.09-5.0  µ g·ml-1 for NI and NA, respectively...
2018: Journal of Analytical Methods in Chemistry
Maria Pilo, Roberta Farre, Joanna Izabela Lachowicz, Elisabetta Masolo, Angelo Panzanelli, Gavino Sanna, Nina Senes, Ana Sobral, Nadia Spano
Enzyme-based sensors have emerged as important analytical tools with application in diverse fields, and biosensors for the detection of glucose using the enzyme glucose oxidase have been widely investigated. In this work, the preparation of biosensors by electrochemical polymerization of (poly)thiophenes, namely 2,2'-bithiophene (2,2'-BT) and 4,4'-bis(2-methyl-3-butyn-2-ol)-2,2'-bithiophene (4,4'-bBT), followed by immobilization of glucose oxidase on the films, is described. N-cyclohexyl-N'-(2-morpholinoethyl)carbodiimide metho- p -toluenesulfonate (CMC) was used as a condensing agent, and p -benzoquinone (BQ) was used as a redox mediator in solution...
2018: Journal of Analytical Methods in Chemistry
Naz Hasan Huda, Bhawna Gauri, Heather A E Benson, Yan Chen
The objective of this study was to develop and validate a method for quantitative analysis of rivastigmine hydrogen tartrate (RHT) in dual-ligand polymeric nanoparticle formulation matrices, drug release medium, and cellular transport medium. An isocratic HPLC analysis method using a reverse phase C18 column and a simple mobile phase without buffer was developed, optimised, and fully validated. Analyses were carried out at a flow rate of 1.5 mL/min at 50°C and monitored at 214 nm. This HPLC method exhibited good linearity, accuracy, and selectivity...
2018: Journal of Analytical Methods in Chemistry
Maydla Dos Santos Vasconcelos, Wilson Espíndola Passos, Caroline Honaiser Lescanos, Ivan Pires de Oliveira, Magno Aparecido Gonçalves Trindade, Anderson Rodrigues Lima Caires, Rozanna Marques Muzzi
The techniques used to monitor the quality of the biodiesel are intensely discussed in the literature, partly because of the different oil sources and their intrinsic physicochemical characteristics. This study aimed to monitor the thermal degradation of the fatty acid methyl esters of Sesamum indicum L. and Raphanus sativus L. biodiesels (SILB and RSLB, resp.). The results showed that both biodiesels present a high content of unsaturated fatty acids, ∼84% (SILB) and ∼90% (RSLB). The SILB had a high content of polyunsaturated linoleic fatty acid (18  :  2), about 49%, and the oleic monounsaturated (18  :  1), ∼34%...
2018: Journal of Analytical Methods in Chemistry
Yong Dae Park, Jeum-Jong Kim, Sungbeom Lee, Chul-Hong Park, Hyoung-Woo Bai, Seung Sik Lee
Accumulation of β -amyloid (A β ) plaques comprising A β 40 and A β 42 in the brain is the most significant factor in the pathogenesis of Alzheimer's disease (AD). Thus, the detection of A β plaques has increasingly attracted interest in the context of AD diagnosis. In the present study, a fluorescent pyridazine-based dye that can detect and image A β plaques was designed and synthesized, and its optical properties in the presence of A β aggregates were evaluated. An approximately 34-fold increase in emission intensity was exhibited by the fluorescent probe after binding with A β aggregates, for which it showed high affinity ( K D  = 0...
2018: Journal of Analytical Methods in Chemistry
Ireneusz Sowa, Sylwia Zielińska, Jan Sawicki, Anna Bogucka-Kocka, Michał Staniak, Ewa Bartusiak-Szcześniak, Maja Podolska-Fajks, Ryszard Kocjan, Magdalena Wójciak-Kosior
Chelidonium majus L. is a rich source of isoquinoline alkaloids with confirmed anti-inflammatory, choleretic, spasmolytic, antitumor, and antimicrobial activities. However, their chromatographic analysis is difficult because they may exist both in charged and uncharged forms and may result in the irregular peak shape and the decrease in chromatographic system efficacy. In the present work, the separation of main C. majus alkaloids was optimized using a new-generation XB-C18 endcapped core-shell column dedicated for analysis of alkaline compounds...
2018: Journal of Analytical Methods in Chemistry
Dimitra K Toubanaki, Evdokia Karagouni
Nervous necrosis virus (nodavirus) has been responsible for mass mortalities in aquaculture industry worldwide, with great economic and environmental impact. A rapid low-cost test to identify nodavirus genotype could have important benefits for vaccine and diagnostic applications in small- and medium-scale laboratories in both academia and fish farming industry. A dual lateral flow biosensor for simultaneous detection of the most prevalent nodavirus genotypes (RGNNV and SJNNV) was developed and optimized. The dual biosensor consisted of two antibody-based test zones, indicative of each genotype, and a control zone...
2018: Journal of Analytical Methods in Chemistry
Gabriela Islas, Jose A Rodriguez, Irma Perez-Silva, Jose M Miranda, Israel S Ibarra
Solid-phase extraction in combination with large-volume sample stacking-capillary electrophoresis (SPE-LVSS-CE) was applied to measure chlortetracycline, doxycycline, oxytetracycline, and tetracycline in milk samples. Under optimal conditions, the proposed method had a linear range of 29 to 200  µ g·L-1 , with limits of detection ranging from 18.6 to 23.8  µ g·L-1 with inter- and intraday repeatabilities < 10% (as a relative standard deviation) in all cases. The enrichment factors obtained were from 50...
2018: Journal of Analytical Methods in Chemistry
Nevena Maljurić, Jelena Golubović, Matjaž Ravnikar, Dušan Žigon, Borut Štrukelj, Biljana Otašević
Diabetes mellitus is one of the leading world's public health problems. Therefore, it is of a huge interest to develop new antidiabetic drugs. Apart from traditional therapy of diabetes, nowadays, importance is given to natural substances with antidiabetic potential. Fomes fomentarius is a mushroom widely used for different purposes, due to its range of already confirmed activities. Fomentariol is a constituent of Fomes fomentarius , responsible for its antidiabetic potential. In that respect, it is important to develop a method for isolation and quantification of fomentariol from fungal material, which will be simple and efficient...
2018: Journal of Analytical Methods in Chemistry
Mateusz Kowalcze, Jan Wyrwa, Małgorzata Dziubaniuk, Małgorzata Jakubowska
In this work, DPV determination of anethole was presented using various carbon, two-diameter (1.5 and 3 mm) electrodes, that is, BDD, GC, CP, and CP doped by La2 O3 and CeO2 nanoparticles. La2 O3 /CPE to our best knowledge was proposed first time. Cyclic voltammograms confirmed totally irreversible electrode electrooxidation process, controlled by diffusion, in which two electrons take part. The most satisfactory sensitivity 0.885 ± 0.016  µ A/mg L-1 in 0.1 mol L-1 acetate buffer was obtained for La2 O3 /CPE with the correlation coefficient r of 0...
2018: Journal of Analytical Methods in Chemistry
Qian Wang, Rui Zhao, Yan Cui, Cuicui Liu, Liya Liang, Shijie Yan
A simple and rapid capillary electrophoresis method with diode array detector was developed for determination of sarafloxacin and difloxacin in beef. In this study, the experimental parameters affecting the determination were systematically optimized, including wavelength, buffer system, pH and concentration, and separation temperature and voltage. Under the optimal conditions, sarafloxacin and difloxacin could be quantified within 4 min using H3 BO3 /Na2 B4 O7 buffer (35 mmol/L, pH 8.8) as background electrolyte, 25 kV as separation voltage, and 22°C as the column temperature...
2018: Journal of Analytical Methods in Chemistry
Michaela Dufka, Bohumil Dočekal
A diffusive gradient in thin films (DGT) technique was employed in characterization of the particulate matter related to the urban area suffering from heavy traffic. Kinetics of mobilization metals fluxes from the metal-contaminated particulate matter was investigated. To monitor responses of the particulate matter sample, DGT probes of various thickness of diffusion layer were deployed in aqueous model suspensions of the particulate matter for different time periods. Particulate matter samples and exposed DGT resin gels were decomposed in a mixture of nitric and hydrochloric acid in a microwave pressurized PTFE-lined system...
2018: Journal of Analytical Methods in Chemistry
So Hyeon Jeon, Yong Pyo Kim, Younglim Kho, Jeoung Hwa Shin, Won Hyun Ji, Yun Gyong Ahn
A method for the quantitative determination of dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), bis(2-ethylhexyl) adipate (DEHA), bis(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), dioctyl terephthalate (DOTP), diisononyl phthalate (DINP), and diisodecyl phthalate (DIDP) in medical infusion sets was developed and validated using gas chromatography coupled with triple quadrupole mass spectrometry (GC-MS/MS) in the multiple reaction monitoring (MRM) mode. Solvent extraction with polymer dissolution for sample preparation was employed prior to GC-MS/MS analysis...
2018: Journal of Analytical Methods in Chemistry
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