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Journal of Pharmaceutical and Biomedical Analysis

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https://www.readbyqxmd.com/read/28746908/two-dimensional-liquid-chromatography-in-pharmaceutical-analysis-instrumental-aspects-trends-and-applications
#1
REVIEW
Marion Iguiniz, Sabine Heinisch
The interest in two-dimensional liquid chromatography (2D-LC) has been growing up since the last decades. This promising technique appears as a relevant solution for various analytical challenges encountered in pharmaceutical analysis. The objective of this review is to give an overview of past, current and emerging trends in 2D-LC techniques applied to pharmaceutical compounds. The referenced studies cover the late 1980s to the present. Information regarding the different aspects of this analytical technique, including chromatographic conditions, instrumental setup and compounds of interest, was compiled and summarized into a synoptic table...
July 15, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28746909/optoelectronic-iron-detectors-for-pharmaceutical-flow-analysis
#2
Natalia Rybkowska, Robert Koncki, Kamil Strzelak
Compact flow-through optoelectronic detectors fabricated by pairing of light emitting diodes have been applied for development of economic flow analysis systems dedicated for iron ions determination. Three analytical methods with different chromogens selectively recognizing iron ions have been compared. Ferrozine and ferene S based methods offer higher sensitivity and slightly lower detection limits than method with 1,10-phenantroline, but narrower ranges of linear response. Each system allows detection of iron in micromolar range of concentration with comparable sample throughput (20 injections per hour)...
July 14, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28743077/characterization-and-quantitative-analysis-of-phenolic-derivatives-in-longxuetongluo-capsule-by-hplc-dad-it-tof-ms
#3
Jing Sun, Yuelin Song, Hui Sun, Wenjing Liu, Yunfeng Zhang, Jiao Zheng, Qian Zhang, Yunfang Zhao, Wei Xiao, Pengfei Tu, Jun Li
Longxuetongluo Capsule (LTC), which is derived from the total phenolic extract of Chinese dragon's blood, has been proved to be safe as well as effective towards ischemic stroke. However, the effective material basis remains unclear. The present study thereby focused on the clarification of the qualitative and quantitative properties for the phenolic derivatives in LTC. Regarding homolog-focused chemical profiling, the mass fragmentation patterns of the primary subtypes of phenolic compounds such as homoisoflavanones, flavanes, chalcones, and flavonoid oligomers were summarized by assaying authentic references with hybrid ion trap time-of-flight mass spectrometry, and the chemical structures of 124 phenolic compounds, in total, were unambiguously or tentatively annotated in LTC by matching the accurate mass spectral profiles with the proposed mass cracking rules and those reference substances...
July 14, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28743076/lc-ms-ms-esi-method-for-simultaneous-quantification-of-darolutamide-and-its-active-metabolite-orm-15341-in-mice-plasma-and-its-application-to-a-pharmacokinetic-study
#4
Sreekanth Dittakavi, Pavan Kumar V S P Nagasuri, Suresh P Sulochana, Syed Mohd Saim, Sadanand R Mallurwar, Mohd Zainuddin, Purushottam Dewang, Sriram Rajagopal, Ramesh Mullangi
A sensitive and rapid LC-MS/MS method was developed and validated for the simultaneous quantitation of darolutamide and its active metabolite i.e. ORM-15341 in 50μL mice plasma using bicalutamide as an internal standard (I.S.) as per regulatory guidelines. Sample processing was accomplished through liquid-liquid extraction. Chromatographic separation was achieved using an Atlantis C18 column with an isocratic mobile phase comprising 0.2% formic acid:acetonitrile (35:65, v/v) at a flow rate of 0.8mL/min within 2...
July 13, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28735185/mil-101-cr-go-for-dispersive-micro-solid-phase-extraction-of-pharmaceutical-residue-in-chicken-breast-used-in-microwave-assisted-coupling-with-hplc-ms-ms-detection
#5
Yudan Wang, Xinpeng Dai, Xi He, Lin Chen, Xiaohong Hou
In this work, MIL-101(Cr)@GO (Graphite Oxide) was synthesized using a hydrothermal synthesis method and was applied as a dispersive micro-solid-phase extraction (D-μ-SPE) sorbent for the efficient concentration of four residual drugs (metronidazole, MNZ; tinidazole, TNZ; chloramphenicol, CAP; sulfamethoxazole, SMX). Meanwhile, the extraction process was optimized by combining it with microwave-assisted extraction. Factors affecting the D-μ-SPE efficiency, such as selection of sorbent materials, pH of the sample solution, salting-out effect, amount of used material, extraction time, desorption solvent and desorption time, were studied...
July 11, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28743078/metabolite-identification-of-azd8055-in-sprague-dawley-rats-after-a-single-oral-administration-using-ultra-performance-liquid-chromatography-and-mass-spectrometry
#6
Md Mamunur Rashid, Hyun-A Oh, Hyunbeom Lee, Byung Hwa Jung
AZD8055 is an ATP-competitive specific dual mTOR inhibitor and exhibited potent antitumor activity on several types of solid tumors. However, the metabolism of AZD8055 in the body still remains unknown. In this study, metabolite identification of AZD8055 was performed using ultra high-performance liquid chromatography-ion trap mass spectrometry (UHPLC-IT-MS) through both in vitro and in vivo approaches using rat liver microsomes (RLMs) and rat plasma, urine and feces, respectively. A total of eight putative metabolites (five phase I and three phase II) were identified, and a tentative metabolic pathway was suggested for the first time...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28732306/photostability-testing-using-online-reactor-hplc-hyphenation-and-mass-spectrometric-compound-identification-illustrated-by-ketoprofen-as-model-compound
#7
Jaber Assaf, Diego Zulkiewicz Gomes, Bernhard Wuest, Maria Kristina Parr
Investigations on the photochemical stability of pharmaceutical substances are mandatory in drug development and licensing as photo-induced degradation of an active pharmaceutical ingredient (API) may not only lead to decreased API concentrations but also to toxic or reactive products. Thus, the US Food and Drug Administration (FDA) and the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) issued Guidance for Industry Q1B "Photostability Testing of New Drug Substances and Products" for testing of pure but also packed drugs...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28728067/an-optimized-hplc-uv-method-for-quantitatively-determining-sesquiterpenes-in-nardostachyos-radix-et-rhizoma
#8
Vu Ngoc Han Le, Trong Quan Khong, Min Kyun Na, Kyung Tae Kim, Jong Seong Kang
Nardostachyos Radix et Rhizoma (NR), the root and rhizome from either Nardostachys jatamansi Batal or Nardostachys jatamansi DC, is known to have biological functions including neuro-protective and anti-pancreatitis activity. The main bioactive compounds within NR are all classified as sesquiterpenes, and include desoxo-narchinol A, nardosinonediol, and nardosinone. Although NR is a valuable herb that is widely used in many Asian countries, robust quality control protocols for NR are still in question, especially those that can analyze the three main active compounds...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28720350/an-overview-of-in-vitro-dissolution-release-methods-for-novel-mucosal-drug-delivery-systems
#9
REVIEW
Mario Jug, Anita Hafner, Jasmina Lovrić, Maja Lusina Kregar, Ivan Pepić, Željka Vanić, Biserka Cetina-Čižmek, Jelena Filipović-Grčić
In vitro dissolution/release tests are an important tool in the drug product development phase as well as in its quality control and the regulatory approval process. Mucosal drug delivery systems are aimed to provide both local and systemic drug action via mucosal surfaces of the body and exhibit significant differences in formulation design, as well as in their physicochemical and release characteristics. Therefore it is not possible to devise a single test system which would be suitable for release testing of such complex dosage forms...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28719814/enantiomeric-separation-of-seven-%C3%AE-agonists-by-nace-study-of-chiral-selectivity-with-diacetone-d-mannitol-boric-acid-complex
#10
Lili Lv, Lijuan Wang, Jun Li, Yajun Jiao, Shengnan Gao, Jiachang Wang, Hongyuan Yan
A rapid and effective nonaqueous capillary electrophoresis (NACE)-ultraviolet (UV) method was developed for the enantiomeric separation of seven β-agonists. Diacetone-d-mannitol-boric acid complex was used as a new chiral selector. It was in situ synthesized by the reaction of diacetone-d-mannitol and boric acid in methanol medium containing triethylamine. The effects of diacetone-d-mannitol, boric acid, and triethylamine concentrations on the enantioseparation were carefully investigated. Under the optimized conditions, baseline enantioseparation could be obtained for six of the tested β-agonists within 12min...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28719813/comparative-stability-indicating-chromatographic-methods-for-determination-of-4-hexylresorcinol-in-pharmaceutical-formulation-and-shrimps
#11
Rafeek F Shokry, Lories I Bebawy, Mohamed R Elghobashy, Samah S Abbas
Three chromatographic stability-indicating methods were developed for determination of 4-hexylresorcinol in pure form and in a pharmaceutical formulation. Method A was based on a gradient elution liquid chromatographic HPLC determination of 4-hexylresorcinol, its related impurities and in presence of its degradation products. UPLC-MS/MS (Method B) was described for determination of the cited drug in presence of its degradation products. Method C was a thin- layer chromatography (TLC)-densitometry method for the separation and determination of the active ingredient, one of its related impurities and in presence of its degradation products...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28709128/identification-and-interconversion-of-isomeric-4-5-functionalized-1-2-3-thiadiazoles-and-1-2-3-triazoles-in-conditions-of-electrospray-ionization
#12
D M Mazur, M E Zimens, V A Bakulev, A T Lebedev
1,2,3-Triazoles and 1,2,3-thiadiazoles have been receiving permanent interest due to their exciting chemical reactivity and interesting biological properties including antibacterial, anticancer and antiviral activities. There are four compounds bearing 1H-1,2,3-triazole core in clinical studies which may appear in the market of drugs in nearest future. Definitely reliable methods of their identification and quantification should be developed by that time. Mass spectrometry showed itself as the most reliable method of analysis when dealing with trace levels of organic compounds in the mixtures and in the most complex matrices, including biological ones...
July 8, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28715790/site-and-species-specific-hydrolysis-rates-of-cocaine
#13
Levente Szöcs, Gergely Völgyi, Ákos Urai, Sándor Hosztafi, Gergő Tóth, Lajos Gergó, Béla Noszál
The hydroxide-catalyzed non-enzymatic hydrolysis of cocaine is quantified in terms of ten site- and species-specific rate constants in connection with also ten site- and species-specific acid-base equilibrium constants, comprising all the twelve coexisting species in solution. This characterization involves the major and minor decomposition pathways via benzoylecgonine and ecgonine methyl ester, respectively, leading to ecgonine, the final product. Hydrolysis has been found to be 10-330 times faster at site 2 than at site 3, depending on the ionization status of the amino moiety and the rest of the molecule...
July 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28715789/quantification-of-idp-73152-a-novel-antibiotic-in-plasma-from-mice-rats-and-humans-using-an-ultra-high-performance-liquid-chromatography-tandem-mass-spectrometry-method-for-use-in-pharmacokinetic-studies
#14
Myongjae Lee, Dohee Kim, Jeongcheol Shin, Hee-Yeol Lee, Soobong Park, Hong-Sub Lee, Jae-Hoon Kang, Suk-Jae Chung
IDP-73152, a novel inhibitor of a bacterial peptide deformylase, was recently approved as a new, investigational drug in Korea for the clinical management of infections caused by Gram positive bacteria. The objective of this study was to develop/validate a simple and robust analytical method for the determination of IDP-73152 in plasma samples from rodents and humans, and to assess the feasibility of the assay for use in pharmacokinetic studies using animal models. Plasma samples were processed using a standard method for protein precipitation and an aliquot of the extract then injected onto an UHPLC-MS/MS system...
July 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28711674/hplc-hg-afs-determination-of-arsenic-species-in-acute-promyelocytic-leukemia-apl-plasma-and-blood-cells
#15
Meihua Guo, Wenjing Wang, Xin Hai, Jin Zhou
Arsenic trioxide (ATO) has been successfully used in the treatment of acute promyelocytic leukemia (APL). To clarify the arsenic species in APL patients, high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry (HPLC-HG-AFS) and HG-AFS methods were developed and validated to quantify the plasma concentrations of inorganic arsenic (As(III) and As(V)) and methylated metabolites (MMA and DMA), and the total amounts of arsenic in blood cells and plasma. Blood cells and plasma were digested with mixtures of HNO3H2O2 and analyzed by HG-AFS...
July 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28711673/on-line-prediction-of-the-glucose-concentration-of-cho-cell-cultivations-by-nir-and-raman-spectroscopy-comparative-scalability-test-with-a-shake-flask-model-system
#16
Bence Kozma, Edit Hirsch, Szilveszter Gergely, László Párta, Hajnalka Pataki, András Salgó
In this study, near-infrared (NIR) and Raman spectroscopy were compared in parallel to predict the glucose concentration of Chinese hamster ovary cell cultivations. A shake flask model system was used to quickly generate spectra similar to bioreactor cultivations therefore accelerating the development of a working model prior to actual cultivations. Automated variable selection and several pre-processing methods were tested iteratively during model development using spectra from six shake flask cultivations...
July 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28709716/the-analytical-process-to-search-for-metabolomics-biomarkers
#17
REVIEW
M D Luque de Castro, F Priego-Capote
The scant number of available metabolomics biomarkers does not reflect the extent of the research in this field. Looking for the reasons of failure, the authors, as analytical chemists, critically discuss each of the steps in the analytical process that requires improvements. They find insufficient information about how the experimental part is developed. After revising the steps from sampling to obtainment of the analytical sample (from typical samples such as blood and urine to others less common such as sweat or saliva), the need for data and metadata for either reproduction of a given study or for taking the study as starting point after biomarker discovery is criticized...
July 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28700970/identification-of-impurities-in-macrolides-by-liquid-chromatography-mass-spectrometric-detection-and-prediction-of-retention-times-of-impurities-by-constructing-quantitative-structure-retention-relationship-qsrr
#18
Xia Zhang, Jin Li, Chen Wang, Danqing Song, Changqin Hu
Macrolides are multicomponent drugs whose impurity control is always a challenge demanding analysis method with good sensitivity and selectivity. Three separate, sensitive, accurate liquid chromatography tandem mass spectrometry methods (LC-MS) were developed for the measurement of three 16-membered ring macrolides (josamycin, josamycin propionate and midecamycin acetate) and related substances in commercial samples. The characteristics of impurities in macrolides were summarized as useful guidance for the impurity analysis of this class of drugs...
July 6, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28715791/new-approach-for-the-diagnosis-of-histamine-intolerance-based-on-the-determination-of-histamine-and-methylhistamine-in-urine
#19
Oriol Comas-Basté, M Luz Latorre-Moratalla, Roberta Bernacchia, M Teresa Veciana-Nogués, M Carmen Vidal-Carou
Histamine intolerance is a disorder in the homeostasis of histamine due to a reduced intestinal degradation of this amine, mainly caused by diamine oxidase (DAO) enzyme deficiency, which provokes its accumulation in plasma and the appearance of adverse health affects. A new approach for the diagnosis of this intolerance could be the determination of histamine and its metabolites in urine. The aim of this work was to develop and validate a rapid method to determine histamine and methylhistamine in human urine by Ultra High Performance Liquid Chromatography and Fluorimetric detection (UHPLC-FL)...
July 5, 2017: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/28710995/enhanced-and-green-extraction-polyphenols-and-furanocoumarins-from-fig-ficus-carica-l-leaves-using-deep-eutectic-solvents
#20
Tong Wang, Jiao Jiao, Qing-Yan Gai, Peng Wang, Na Guo, Li-Li Niu, Yu-Jie Fu
Nowadays, green extraction of bioactive compounds from medicinal plants has gained increasing attention. As green solvent, deep eutectic solvent (DES) have been highly rated to replace toxic organic solvents in extraction process. In present study, to simultaneous extraction five main bioactive compounds from fig leaves, DES was tailor-made. The tailor-made DES composed of a 3:3:3 molar ratio of glycerol, xylitol and D-(-)-Fructose showed enhanced extraction yields for five target compounds simultaneously compared with traditional methanol and non-tailor DESs...
July 4, 2017: Journal of Pharmaceutical and Biomedical Analysis
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