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Journal of Pharmaceutical and Biomedical Analysis

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https://www.readbyqxmd.com/read/27915197/liquid-chromatography-tandem-mass-spectrometric-determination-of-propofol-in-rat-serum-and-hair-at-attogram-level-after-derivatization-with-3-bromomethyl-propyphenazone
#1
Alaa Khedr, Soad S Abd El-Hay, Ahmed K Kammoun
A sensitive, selective and precise liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of propofol (PRO) in rat serum and hair has been developed. 3-Bromomethyl-propyphenazone was used as derivatization reagent forming propofol-methyl-propyphenazone compound. The derivatization reaction was optimized and validated for maximum MS sensitivity. The MS instrumental sensitivity reached to 10 attogram. The serum samples were extracted by using Chromabond C8 columns, while hair samples extracted with methanol...
November 28, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27918992/investigation-of-the-metabolites-of-the-hif-stabilizer-fg-4592-roxadustat-in-five-different-in-vitro-models-and-in-a-human-doping-control-sample-using-high-resolution-mass-spectrometry
#2
Annelie Hansson, Mario Thevis, Holly Cox, Geoff Miller, Daniel Eichner, Ulf Bondesson, Mikael Hedeland
FG-4592 is a hypoxia-inducible factor (HIF) stabilizer, which can increase the number of red blood cells in the body. It has not been approved by regulatory authorities, but is available for purchase on the Internet. Due to its ability to improve the oxygen transportation mechanism in the body, FG-4592 is of interest for doping control laboratories, but prior to this study, little information about its metabolism was available. In this study, the metabolism of FG-4592 was investigated in a human doping control sample and in five in vitro models: human hepatocytes and liver microsomes, equine liver microsomes and S9 fraction and the fungus Cunninghamella elegans...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27916506/quantification-of-biologically-active-o-prenylated-and-unprenylated-phenylpropanoids-in-dill-anethum-graveolens-anise-pimpinella-anisum-and-wild-celery-angelica-archangelica
#3
Vito Alessandro Taddeo, Salvatore Genovese, Philippe de Medina, Roberta Palmisano, Francesco Epifano, Serena Fiorito
An analytical strategy based on different extraction methodologies and HPLC with spectrophotometric (UV-vis) detection has been developed to investigate the presence of and to quantitate biologically active selected unprenylated and O-prenylated phenylpropanoids, namely umbelliferone, 4'-geranyloxyferulic acid, 7-isopentenyloxycoumarin, auraptene, and umbelliprenin in dill (Anethum graveolens L.), anise (Pimpinella anisum L.), and wild celery (Angelica archangelica L.). Absolute ethanol or 7:3 water/ethanol mixtures were seen to be the most powerful extraction solvents to perform "classic" maceration or ultrasound-assisted one in terms of yields in secondary metabolites...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915199/deep-eutectic-solvents-as-green-media-for-extraction-of-flavonoid-glycosides-and-aglycones-from-platycladi-cacumen
#4
Bo Zhuang, Li-Li Dou, Ping Li, E-Hu Liu
Deep eutectic solvents (DESs) are emerging as alternatives to conventional ionic liquids and organic solvents due to their unique advantages. In the present study, the tuneability of DESs as tailor-made solvents to efficiently extract polar and non-polar bioactive compounds from Platycladi Cacumen was detailedly investigated. Totally 12 types of choline chloride-, betaine-, and l-proline-based DESs were synthesized for initial screening, and extraction conditions was optimized by single-factor experiment. Experiments with different DESs and principal components analysis demonstrated that the extractability of both flavonoid glycosides and aglycones was greater with certain designed DESs than conventional solvents...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915198/a-new-approach-to-the-rapid-separation-of-isomeric-compounds-in-a-silybum-marianum-extract-using-uhplc-core-shell-column-with-f5-stationary-phase
#5
Jakub Fibigr, Dalibor Šatínský, Petr Solich
In this paper, a new ultra-high performance liquid chromatography (UHPLC) method using a core-shell column with a pentafluorophenyl stationary phase for separation of seven active compounds of a Silybum marianum extract was developed and validated. Silymarin, an extract of Silybum marianum, is known for its abilities to protect the liver from toxic substances, hepatitis therapy, and anti-tumour activity. Silymarin is currently being widely used in commercial preparations and herbal teas. Separation of seven compounds contained in the Silybum marianum extract (taxifolin, silychristin, silydianin, silybin A, silybin B, isosilybin A, isosilybin B) and other substances occurring in real samples was performed on the Kinetex 1...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915196/identification-and-characterization-of-a-new-dapoxetine-impurity-by-nmr-transformation-of-n-oxide-by-cope-elimination
#6
András Darcsi, Ákos Rácz, Szabolcs Béni
Unknown impurity associated with the degradation process of dapoxetine base was isolated. The structure elucidation of this new compound using accurate mass data, IR and NMR spectroscopy is presented herein. The unambiguous resonance assignment concluded to the formation of geometrical isomers of cinnamyloxynaphtalenes via Cope elimination of dapoxetin-N-oxide, the major oxidative and metabolic degradation product of dapoxetine. An efficient and simple synthetic approach has also been developed for the synthesis of dapoxetine-N-oxide for the first time and cinnamyloxynaphtalene in order to confirm the proposed degradation pathway and structures of the degradation products...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915194/quantitative-determination-of-salbutamol-sulfate-impurities-using-achiral-supercritical-fluid-chromatography
#7
Amandine Dispas, Vincent Desfontaine, Bertyl Andri, Pierre Lebrun, Dorina Kotoni, Adrian Clarke, Davy Guillarme, Philippe Hubert
In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of SFC for the quality control of pharmaceuticals, especially in the case of the determination of the active pharmaceutical ingredient (API). Nevertheless, quality control requires also the determination of impurities. The objectives of the present work were to (i) demonstrate the interest of SFC as a reference technique for the determination of impurities in salbutamol sulfate API and (ii) to propose an alternative to a reference HPLC method from the European Pharmacopeia (EP) involving ion-pairing reagent...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915193/metabolic-fate-and-detectability-of-the-new-psychoactive-substances-2-4-bromo-2-5-dimethoxyphenyl-n-2-methoxyphenyl-methyl-ethanamine-25b-nbome-and-2-4-chloro-2-5-dimethoxyphenyl-n-2-methoxyphenyl-methyl-ethanamine-25c-nbome-in-human-and-rat-urine-by-gc-ms
#8
Achim T Caspar, Simon D Brandt, Andreas E Stoever, Markus R Meyer, Hans H Maurer
25B-NBOMe and 25C-NBOMe are potent 5-HT2A receptor agonists that have been associated with inducing hallucinogenic effects in drug users and severe intoxications. This paper describes the identification of their metabolites in rat and human urine by liquid chromatography (LC)-high resolution (HR)-MS/MS, the comparison of metabolite formation in vitro and in vivo and in different species, the general involvement of human cytochrome-P450 (CYP) isoenzymes on their metabolism steps, and their detectability by standard urine screening approaches (SUSAs) using GC-MS, LC-MS(n), or LC-HR-MS/MS...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915191/rp-hplc-determination-of-dissociation-constant-using-solely-aqueous-mobile-phase
#9
Tereza Volná, Kamil Motyka, Jan Hlaváč
The proposed HPLC method using solely or nearly 100% aqueous mobile buffer as mobile phase offers fast determination of dissociation constant for compounds in relatively wide range of lipophilicity (log P from -2.26 to 2.26). The dissociation constant value for simpler chemical compounds can be determined via only 8 chromatographic runs. The number of needed chromatographic separations depends on the structural complexity of the tested compound. Moreover, the proposed method does not require a measurement of Yasuda-Shedlovsky extrapolation that includes several pKa determinations in solutions with different methanol content which speeds up considerably the procedure...
November 27, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915195/hydrogen-deuterium-exchange-a-unique-and-effective-method-for-ms-fragmentation-behavior-elucidation-of-ginkgolides-and-its-application-to-systematic-research-in-ginkgo-biloba
#10
Xingliang Niu, Jun Luo, Deran Xu, Hongyan Zou, Lingyi Kong
Ginkgolides, the main active constituents of Ginkgo biloba, possess significant selectively inhibition on platelet-activating factor and pancreatic lipase and attract wide attention in pharmacological research area. In our study, an effective hydrogen/deuterium (H/D) exchange method was developed by exchanging the α-Hs of lactone groups in ginkgolides with Ds, which was very useful for the elucidation of the fragmentation patterns of ginkgolides in Quadrupole Time-of-flight Mass Spectrometry (Q-TOF-MS), especially in accurately distinguishing the type and position of substituent in framework of ginkgolides...
November 26, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27918991/sample-preparation-of-serum-to-allow-capillary-electrophoresis-analysis-of-prostate-specific-antigen-isoforms
#11
Noemi Farina-Gomez, Silvia Barrabes, Jorge E Gomez-Lopez, Monica Gonzalez, Angel Puerta, Diana Navarro-Calderon, Eduardo Albers-Acosta, Carlos Olivier, Jose C Diez-Masa, Rosa Peracaula, Mercedes de Frutos
Prostate cancer is the second most frequently diagnosed cancer in men worldwide. Currently prostate specific antigen (PSA) serum concentration is the most used prostate cancer marker, but it only shows limited specificity. Because PSA glycosylation is altered by prostate cancer, detecting glycosylation changes could increase PSA specificity as a prostate cancer marker. Changes in PSA glycosylation can modify its electrophoretic- behavior and techniques such as capillary zone electrophoresis (CZE) and two-dimensional electrophoresis (2-DE) could be applied to detect changes in PSA glycosylation...
November 24, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27902942/a-simple-and-sensitive-liquid-chromatography-tandem-mass-spectrometry-method-for-trans-%C3%AE%C2%B5-viniferin-quantification-in-mouse-plasma-and-its-application-to-a-pharmacokinetic-study-in-mice
#12
Jiseon Kim, Jee Sun Min, Doyun Kim, Yu Fen Zheng, Karabasappa Mailar, Won Jun Choi, Choongho Lee, Soo Kyung Bae
In this study, a simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of trans-ε-viniferin in small volumes (10μl) of mouse plasma using chlorpropamide as an internal standard was developed and validated. Plasma samples were precipitated with acetonitrile and separated using an Eclipse Plus C18 column (100×4.6mm, 1.8-μm) with a mobile phase consisting of 0.1% formic acid in acetonitrile and 0.1% formic acid in water (60:40v/v) at a flow rate of 0.5ml/min...
November 24, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27907855/lc-ms-ms-assay-for-the-quantitation-of-the-tyrosine-kinase-inhibitor-neratinib-in-human-plasma
#13
Brian F Kiesel, Robert A Parise, Alvin Wong, Kiana Keyvanjah, Samuel Jacobs, Jan H Beumer
Neratinib is an orally available tyrosine kinase inhibitor targeting HER2 (ERBB2) and EGFR (ERBB). It is being clinically evaluated for the treatment of breast and other solid tumors types as a single agent or in combination with other chemotherapies. In support of several phase I/II clinical trials investigating neratinib combinations, we developed and validated a novel LC-MS/MS assay for the quantification of neratinib in 100μL of human plasma with a stable isotopic internal standard. Analytes were extracted from plasma using protein precipitation and evaporation of the resulting supernatant followed by resuspension...
November 22, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27915192/the-profiling-of-the-metabolites-of-hirsutine-in-rat-by-ultra-high-performance-liquid-chromatography-coupled-with-linear-ion-trap-orbitrap-mass-spectrometry-an-improved-strategy-for-the-systematic-screening-and-identification-of-metabolites-in-multi-samples
#14
Jianwei Wang, Peng Qi, Jinjun Hou, Yao Shen, Min Yang, Qirui Bi, Yanping Deng, Xiaojian Shi, Ruihong Feng, Zijin Feng, Wanying Wu, Dean Guo
Drug metabolites identification and construction of metabolic profile are meaningful work for the drug discovery and development. The great challenge during this process is the work of the structural clarification of possible metabolites in the complicated biological matrix, which often resulting in a huge amount data sets, especially in multi-samples in vivo. Analyzing these complex data manually is time-consuming and laborious. The object of this study was to develop a practical strategy for screening and identifying of metabolites from multiple biological samples efficiently...
November 21, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27889670/selective-recognition-of-cis-trans-isomers-of-platinum-drugs-and-the-detection-of-triplex-dna-based-on-fluorescence-reversible-model-of-quantum-dots
#15
Xiaoling Xu, Fang Gao, Xincai Xiao, Yan Hu, Chaozhen Zhu, Dan Zhao
The identification of spatial structures of drugs and the researches on their interaction mechanism with DNA are always attractive to the researchers. However, their realization is lack of simple and fast method. This paper reports the establishment of multiple-functional detection platform based on the "turn off-on" model of ZnCdSe quantum dots. In this system, ZnCdSe quantum dots work as the fluorescent probe, platinum anti-cancer drugs as the quencher and triplex DNA as the trapping agent. The seemingly similar cisplatin and transplatin exhibited different fluorescent recovery behaviors due to their difference in structure, and thus realized the selective detection of cisplatin and transplatin with the reaction time set at 10min as well as the quantitation of cisplatin over the range of 2...
November 19, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27898331/cleaning-verification-exploring-the-effect-of-the-cleanliness-of-stainless-steel-surface-on-sample-recovery
#16
Imad A Haidar Ahmad, James Tam, Xue Li, William Duffield, Thomas Tarara, Andrei Blasko
The parameters affecting the recovery of pharmaceutical residues from the surface of stainless steel coupons for quantitative cleaning verification method development have been studied, including active pharmaceutical ingredient (API) level, spiking procedure, API/excipient ratio, analyst-to-analyst variability, inter-day variability, and cleaning procedure of the coupons. The lack of a well-defined procedure that consistently cleaned coupon surface was identified as the major contributor to low and variable recoveries...
November 18, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27889669/physicochemical-analysis-in-the-evaluation-of-reconstituted-dry-emulsion-tablets
#17
Noémi Anna Niczinger, Barnabás Kállai-Szabó, Miléna Lengyel, Péter Gordon, Imre Klebovich, István Antal
The aim of this study was to characterize the formation of emulsions by droplet size analysis and turbidimetry during reconstitution from a solid dosage form, namely from dry emulsion systems, which carry an oil phase for poorly soluble active ingredients. For the dry emulsion systems tablets were prepared either from oil-in-water systems using a freeze-drying process or through direct compression containing the same oil and excipients. The ratios of oil to emulgents and oil to xanthan gum were equal in both methods...
November 18, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27889668/drug-protein-binding-of-danhong-injection-and-the-potential-influence-of-drug-combination-with-aspirin-insight-by-ultrafiltration-lc-ms-and-molecular-modeling
#18
Junfeng Zhu, Xiaojiao Yi, Peng Huang, Shuqing Chen, Yongjiang Wu
Danhong injection (DHI) is a widely used Chinese medicine injection (CMI) for the clinical treatment of cardiovascular and cerebrovascular diseases. In this study, a simple and efficient in vitro method based on ultrafiltration LC-MS and molecular modeling has been developed to study the human serum albumin (HSA) binding of the compounds in DHI. Seven major components including protocatechuic aldehyde, p-coumaric acid, salvianolic acid D, rosmarinic acid, salvianolic acid E, lithospermic acid and salvianolic acid B were identified as HSA ligands and their binding degrees in the proposed non-saturated model were 26...
November 18, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27871053/quality-by-design-in-the-development-of-hydrophilic-interaction-liquid-chromatography-method-with-gradient-elution-for-the-analysis-of-olanzapine
#19
Anja Tumpa, Ana Stajić, Biljana Jančić-Stojanović, Mirjana Medenica
This paper deals with the development of hydrophilic interaction liquid chromatography (HILIC) method with gradient elution, in accordance with Analytical Quality by Design (AQbD) methodology, for the first time. The method is developed for olanzapine and its seven related substances. Following step by step AQbD methodology, firstly as critical process parameters (CPPs) temperature, starting content of aqueous phase and duration of linear gradient are recognized, and as critical quality attributes (CQAs) separation criterion S of critical pairs of substances are investigated...
November 18, 2016: Journal of Pharmaceutical and Biomedical Analysis
https://www.readbyqxmd.com/read/27886572/a-rapid-and-sensitive-uhplc-ms-ms-method-for-quantification-of-83b1-in-plasma-and-its-application-to-bioavailability-study-in-rats
#20
Dingsheng Wen, Jing Guo, Fulin Jiang, Caishun Huang, Zhenzhen Zhao, Gui Lu, Jiangying Chen, Liuyun Qin, Zhangwei Li, Xueding Wang, Zhuoan Deng, Min Huang, Chan Albert Sun Chi, Tang Johnny Cheuk On, Guoping Zhong
Great attentions have been drawn by quinoline for its broad bioactivity as anti-fungal, anti-bacterial and anti-tumor activities. Compared with cisplatin, 83b1, a quinoline derivative, showed equal activity in anti-tumor and lower cyctotoxicity in normal cell. In this study, a simple, rapid and sensitive method for determination of 83b1 in rat plasma using UHPLC-MS/MS was developed for the first time. Loratadine was used as an internal standard (IS). Separation was performed on an Xterra MS C18 column by isocratic elution using acetonitrile: water solution with 1‰ formic acid (90:10, v/v) as mobile phase at a flow rate of 0...
November 16, 2016: Journal of Pharmaceutical and Biomedical Analysis
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