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Journal of Chromatographic Science

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https://www.readbyqxmd.com/read/28655177/stability-indicating-tlc-densitometric-assay-for-methyltestosterone-and-quantum-chemical-calculations
#1
Syed Ghulam Musharraf, Qamar Ul Arfeen, Faraz Ul Haq, Aliya Khatoon, Rahat Azher Ali
Methyltestosterone is a synthetic testosterone derivative commonly used for the treatment of testosterone deficiency in males and one the anabolic steroids whose use is banned by World Anti-Doping Agency (WADA). This study presents a simple, cost-effective and rapid stability-indicating assay for densitometric quantification of methyltestosterone in pharmaceutical formulation. The developed method employed pre-coated TLC plates with mobile phase hexane:acetone (6.5:3.5 v/v). Limit of detection and limit of quantitation were found to be 2...
June 26, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28651375/chromatographic-and-computational-assessment-of-lipophilicity-of-new-anticancer-acetylenequinoline-derivatives
#2
Krzysztof Marciniec, Stanislaw Boryczka
The lipophilicity of a series of anticancer propargylquinoline derivatives is investigated using both chromatographic and computational methods. The parameters of the tested compounds' relative lipophilicity (logkw) are determined experimentally by the high-performance liquid chromatographic method (RP-HPLC, Accucore C18 column), using mixtures of acetonitrile and water as mobile phases. Mobile phase acetonitrile concentrations range between 50 and 80%. The logk values of the investigated compounds are linearly dependent upon the acetonitrile concentration...
June 23, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28633284/determination-of-some-%C3%AE-blockers-and-%C3%AE-2-agonists-in-plasma-and-urine-using-liquid-chromatography-tandem-mass-spectrometry-and-solid-phase-extraction
#3
Alaa A Salem, Ibrahim Wasfi, Salama S Al-Nassib, Mahmoud Allawy Mohsin, Nawal Al-Katheeri
A highly sensitive method for the determinations of acebutolol, clenbuterol, nadolol, oxprenolol, propranolol, terbutaline and timolol β-blockers and β2-agonists in plasma and urine was developed. The method was optimized using electrospray ionization liquid chromatography-tandem mass spectrometry (LC-ESI-MS-MS) and clean screen solid phase extraction cartridges. Matrix effect was reduced by removing co-extractives from the SPE cartridges using methanol prior to drugs' elution. Using blood and serum matrices for calibration and applying the internal standard method has also contributed to the reduction of matrix effect...
June 13, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28605412/accuracy-profiles-for-analyzing-residual-solvents-in-textiles-by-gc-ms
#4
Qibei Bao, Kejie Fu, Qingqing Ren, Yingying Zhong, Dan Qian
Excess residual solvents (RSs) in clothes or other textiles could be toxic and pose risks to both humans and the environment. N,N-Dimethylformamide (DMF), N,N-dimethylacetamide (DMAc) and 1-methyl-2-pyrrolidinone (NMP) are important chemicals frequently used as solvents in the textile industry. Several organizations have proposed limiting DMF, DMAc and NMP in textiles, but an appropriate detection method has not been proposed. A sensitive GC-MS method for the quantification of DMF, DMAc and NMP in textiles was developed...
June 9, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28595353/determination-of-hydroxylated-polybrominated-diphenyl-ethers-in-chinese-aquatic-products-by-lc-ms-ms
#5
Decong Hu, Xiaozhong Hu, Wei Chen, Hui Wang, Hong Wang, Kuanzheng Zhu, Bin Wu, Changjun Lin
In this reported work, a sensitive and reliable method for detecting 11 hydroxylated polybrominated diphenyl ethers (OH-PBDEs) was established by a combination of pressurized liquid extraction (PLE) and liquid chromatography tandem mass spectrometry (LC/MS/MS). The aquatic products (mainly crayfish and grass carp) from 12 cities in China's HuBei province were examined for the presence of the target OH-PBDEs. The analytical process involved first extracting the OH-PBDEs from the crayfish and grass carp using a PLE, followed by purification using gel permeation chromatography...
June 8, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28541451/uplc-q-tof-ms-based-metabolic-profiling-comparison-of-two-major-bioactive-components-and-their-metabolites-in-normal-and-ckd-rat-plasma-urine-and-feces-following-oral-administration-of-fructus-corni-extract
#6
Min Zhao, Jinhua Tao, Leyue Du, Shu Jiang, Dawei Qian, Jinao Duan
Fructus Corni has been used for nourishing liver and kidney in clinical practice for many years. However, the in vivo integrated metabolism profile of its bioactive components remains unknown. In the present study, ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry coupled with the MetaboLynxTM software was established for screening and identification of the metabolites of the loganin and the morroniside in normal and chronic kidney disease (CKD) rat plasma, urine and feces after oral administration of Fructus Corni extract...
May 24, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28525599/analytical-method-for-pyrethroid-metabolites-in-urine-of-the-non-occupationally-exposed-population-by-gas-chromatography-mass-spectrometry
#7
Toshiaki Yoshida
Pyrethroids are widely being used as household insecticides or mothproof repellents. An analytical method is described for determination of urinary metabolites as biomarkers for monitoring exposure to the pyrethroids. In total, 11 urinary metabolites, 3-(2-carboxyprop-1-enyl)-2,2-dimethylcyclopropanecarboxylic acid, 3-(2-chloro-3,3,3-trifluoroprop-1-enyl)-2,2-dimethylcyclopropanecarboxylic acid, 3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylic acid, 2,2-dimethyl-3-(2-methylprop-1-enyl)cyclopropanecarboxylic acid, 4-fluoro-3-phenoxybenzoic acid, 4-methoxymethyl-2,3,5,6-tetrafluorobenzly alcohol, 2-methyl-3-phenylbenzoic acid, 4-methyl-2,3,5,6-tetrafluorobenzyl alcohol, 3-phenoxybenzoic acid, 2,3,5,6-tetrafluorobenzoic acid and 2,2,3,3-tetramethylcyclopropanecarboxylic acid, were enzymatically hydrolyzed and extracted with toluene...
May 19, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28520922/gc-ms-method-for-quantification-of-mephedrone-in-human-blood-sample
#8
Khaled M Mohamed
Abuse of mephedrone (4-methylmethcathinone) has emerged among the last few years. Intoxication and fatality associated with mephedrone have been reported in the literature. The present work describes a simple and rapid gas chromatography-mass spectrometry (GC-MS) method for detection and quantification of mephedrone in human blood samples using GC-MS. Blood was deproteinated with acetonitrile and the supernatant was derivatized and extracted in a single step with ethyl chloroformate and ethyl acetate. Methamphetamine-d5 was used as an internal standard (IS)...
May 18, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28505281/application-of-partially-substituted-3-5-dimethylphenylcarbamate-3-2-o-%C3%AE-cyclodextrin-2-hydroxypropoxy-propylsilyl-appended-silica-particles-as-chiral-stationary-phase-for-multi-mode-high-performance-liquid-chromatography
#9
Mingxuan Ma, Qunli Wei, Min Meng, Jiale Yin, Lei Du, Xia Zhu, Mengjun Min, Xueyan Zhou, Xiaoxing Yin, Yinhan Gong
A new type of partially substituted 3,5-dimethylphenylcarbamate-(3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica particles (MP-CD-HPS) have been prepared by a convenient post-immobilization derivazition procedure. The MP-CD-HPS has been successfully used as chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC) under normal phase, reversed phase and polar organic mobile phase conditions. The chromatographic evaluation results show that the MP-CD-HPS has excellent selectivity for the separation of aromatic positional isomers and enantiomers of some chiral compounds...
May 13, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28505277/esterification-of-ibuprofen-in-soft-gelatin-capsules-formulations-identification-synthesis-and-liquid-chromatography-separation-of-the-degradation-products
#10
Michal Douša, Ludek Meca, Petr Gibala, Josef Jirman, Marcela Tkadlecová, Jan Srbek, Jana Šalandová, Eva Kovalcíková, Jirí Brichác
Unknown impurities were identified in ibuprofen (IBU) soft gelatin capsules (SGCs) during long-term stability testing by a UHPLC method with UV detection and its chemical formula was determined using high resolution/accurate mass (HRAM) LC-MS. Reference standards of the impurities were subsequently synthesized, isolated by semi-preparative HPLC and characterized using HRAM LC-MS, NMR and IR. Two impurities were formed by esterification of IBU with polyethylene glycol (PEG), which is used as a fill of the SGCs, and were identified as IBU-PEG monoester and IBU-PEG diester...
May 13, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28505230/degradation-and-impurity-profile-study-of-ciclopirox-olamine-after-pre-column-derivatization-a-risk-based-approach
#11
Madhuri Baghel, Sadhana Rajput
The present study focus on ICH prescribed stress degradation of ciclopirox olamine after precolumn derivatization. For establishing stability-indicating assay, the reaction solutions in which different degradation products were formed were mixed, and the separation was optimized by applying principle of QbD. A risk-analysis tools based on cause-effect risk assessment matrix with control-noise-experimentation (CNX) approach was utilized for identifying the high risk variable affecting the analytical attributes...
May 13, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28498911/different-chromatographic-methods-for-simultaneous-determination-of-mefenamic-acid-and-two-of-its-toxic-impurities
#12
Martha M Morcoss, Nada S Abdelwahab, Nouruddin W Ali, Mohammed T Elsaady
Two sensitive, accurate and precise chromatographic methods mentioned as TLC-densitometric method and RP-HPLC-DAD method, were developed and validated for the simultaneous determination of mefenamic acid (MEF) and its two toxic impurities, benzoic acid (BA) and 2,3-dimethylaniline (DMA). In the proposed TLC-densitometric method a developing system consisting of chloroform:acetone:acetic acid:ammonia solution(70:30:2:2, v/v/v/v) was used, TLC aluminum plates 60 F254 was used as a stationary phase and the separated bands were UV-scanned at 225 nm...
May 11, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28498908/development-validation-and-application-of-a-stability-indicating-hplc-method-to-quantify-lidocaine-from-polyethylene-co-vinyl-acetate-eva-matrices-and-biological-fluids
#13
Prabhat Bhusal, Manisha Sharma, Jeff Harrison, Georgina Procter, Gavin Andrews, David S Jones, Andrew G Hill, Darren Svirskis
An efficient and cost-effective quantification procedure for lidocaine by HPLC has been developed to estimate lidocaine from an EVA matrix, plasma, peritoneal fluid and intra-articular fluid (IAF). This method guarantees the resolution of lidocaine from the degradation products obtained from alkaline and oxidative stress. Chromatographic separation of lidocaine was achieved with a retention time of 7 min using a C18 column with a mobile phase comprising acetonitrile and potassium dihydrogen phosphate buffer (pH 5...
May 11, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28486602/determination-of-total-petroleum-hydrocarbons-in-australian-groundwater-through-the-improvised-gas-chromatography-flame-ionization-detection-technique
#14
Maria Vilma Faustorilla, Zuliang Chen, Rajarathnam Dharmarajan, Ravendra Naidu
Assessment of total petroleum hydrocarbons (TPHs) from contaminated sites demands routine and reliable measurement at trace levels. However, the detection limits of these methods need to be improved. This study developed the programmable temperature vaporization-large volume injection (PTV-LVI) method to quantify TPHs through gas chromatography-flame ionization detection. This configuration enhances the method sensitivity for trace level detections through large volume injections and pre-concentration of analytes along the injection liner...
May 9, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28486578/development-of-a-validated-comparative-stability-indicating-assay-method-for-some-h2-receptor-antagonists
#15
Sameh Ahmed, Salwa R Elshaboury, Niveen A Mohamed, Shereen Farrag
A comparative force degradation high performance thin layer chromatography (HPTLC) method was developed and validated for some H2-receptor antagonists. The studied H2-receptor antagonists were ranitidine (RAN), nizatidine (NIZ) and famotidine (FAM). The degradation behaviors of the studied H2-receptor antagonists were studied under different stress conditions (hydrolytic, thermal and oxidative) conditions as well as storage conditions according to International Conference on Harmonization (ICH) recommendations...
May 9, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28472452/determination-of-ms-222-in-water-samples-by-solid-phase-extraction-coupled-with-liquid-chromatography-tandem-mass-spectrometry
#16
Dong-Hao Zhao, Qiang Wang, Xu-Feng Wang, Zhi-Guang Li, Yong-Xian Li, Ke Huang, Liu-Dong Li
A practical solid-phase extraction (SPE) method coupled with liquid chromatography/tandem mass spectrometry (LC-MS/MS) has been developed for the determination of the fish anesthetic MS-222 in water. Water samples were concentrated and purified using three SPE cartridges of different specifications. Elution curves of MS-222 were constructed using various methanol-water solutions on the different cartridges, and SPE conditions were optimized in accordance with the elution curves. The mobile phase containing methanol and 0...
May 4, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28472287/optimized-and-validated-hplc-analysis-of-st-john-s-wort-extract-and-final-products-by-simultaneous-determination-of-major-ingredients
#17
Konstantina Zeliou, Nikos I Kontaxis, Evangelia Margianni, Christos Petrou, Fotini N Lamari
Aim of this work was to develop a validated high performance liquid chromatography method for the analysis of extracts and final products of St. John's wort, according to international guidelines for bioanalytical method validation. Chromatographic separation was performed on a C18 column with a combination of gradient and isocratic steps; the mobile phase composed of ammonium acetate solution (pH 4.5; 10 mM), acetonitrile and methanol. Quantification and method validation was performed using extract spiked with external reference standards of chlorogenic acid, rutin, hyperoside, isoquercitrin, quercetin and hypericin...
May 3, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28449104/liquid-chromatographic-chemometric-techniques-for-the-simultaneous-hplc-determination-of-lansoprazole-amoxicillin-and-clarithromycin-in-commercial-preparation
#18
A Hakan Aktas, Ayse Mine Saridag
Two multivariate calibration-prediction techniques, principal component regression (PCR) and partial least-squares regression (PLSR) were applied to the chromatographic multicomponent analysis of the drug containing lansoprazole (LAN), clarithromycin (CLA) and amoxicillin (AMO). Optimum chromatographic separation of LAN, CLA and AMO with atorvastatin as the internal standard (IS) was obtained by using Xterra® RP18 column 5 μm 4.6 × 250 mm2, and 25 mM ammonium chloride buffer prepared ammonium chloride, acetonitrile and bidistilled water (45:45:10 v/v) as the mobile phase at flow rate 1...
April 26, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28449063/extraction-and-determination-of-quercetin-from-ginkgo-biloba-by-dess-based-polymer-monolithic-cartridge
#19
Xiaoqin Wang, Guizhen Li, Kyung Ho Row
Deep eutectic solvents (DES) were formed from choline chloride (ChCl). DES-modified polymer monolithic (DES-M), template molecular polymer monolithic and non-DES-M without a molecular template were synthesized in identical process. These polymer materials were characterized by field emission scanning electron microscopy and Fourier transform infrared spectroscopy. The significant selective adsorption properties of the polymers were assessed by an absorption capacity experiment and solid-phase extraction (SPE)...
April 26, 2017: Journal of Chromatographic Science
https://www.readbyqxmd.com/read/28444354/easy-assessment-of-levofloxacin-and-minocycline-in-relevant-biomimetic-media-by-hplc-uv-analysis
#20
Ana C Matos, Rosana V Pinto, Ana F Bettencourt
Simple, economic and environmental friendly high-performance liquid chromatography methods for levofloxacin and minocycline quantification in biomimetic media were developed and validate including their stability at body temperature, an often neglected evaluation parameter. Both methods are similar only differing in the wavelength setting, i.e., for levofloxacin and minocycline quantification the UV detection was set at 284 and at 273 nm, respectively. The separation of both antibiotics was achieved using a reversed-phase column and a mobile phase consisting of acetonitrile and water (15:85) with 0...
April 24, 2017: Journal of Chromatographic Science
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