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  • 更新日期:2020-01-16
  • 更新日期:2020-01-14
  • The current status of anti GPCR drugs against different cancers
    J. Pharm. Anal. (IF 4.44) Pub Date : 2020-01-11
    Sana Usman; Maria Khawer; Shazia Rafique; Zara Naz; Komal Saleem
  • Metabolic profiling of four synthetic stimulants, including the novel indanyl-cathinone 5-PPDi, after human hepatocyte incubation
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-12-28
    David Fabregat-Safont; Marie Mardal; Juan V. Sancho; Félix Hernández; Kristian Linnet; María Ibáñez
  • Analysis of TRPA1 antagonist, A-967079, in plasma using high-performance liquid chromatography tandem mass-spectrometry
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-12-13
    Obed A. Gyamfi; Nesta Bortey-Sam; Abigail B. Donkor; Carl W. White; Brian A. Logue
  • Hollow fiber-based liquid phase microextraction followed by analytical instrumental techniques for quantitative analysis of heavy metal ions and pharmaceuticals
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-12-12
    Wajid Ali Khan; Muhammad Balal Arain; Yadollah Yamini; Nasrullah Shah; Tasneem Gul Kazi; Stig Pedersen-Bjergaard; Mohammad Tajik
  • 更新日期:2019-12-13
  • Carbon nanotubes: Evaluation of toxicity at biointerfaces
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-04-25
    Debashish Mohanta, Soma Patnaik, Sanchit Sood, Nilanjan Das

    Carbon nanotubes (CNTs) are a class of carbon allotropes with interesting properties that make them productive materials for usage in various disciplines of nanotechnology such as in electronics equipments, optics and therapeutics. They exhibit distinguished properties viz., strength, and high electrical and heat conductivity. Their uniqueness can be attributed due to the bonding pattern present between the atoms which are very strong and also exhibit high extreme aspect ratios. CNTs are classified as single-walled carbon nanotubes (SWCNTs) and multi-walled carbon nanotubes (MWCNTs) on the basis of number of sidewalls present and the way they are arranged spatially. Application of CNTs to improve the performance of many products, especially in healthcare, has led to an occupational and public exposure to these nanomaterials. Hence, it becomes a major concern to analyze the issues pertaining to the toxicity of CNTs and find the best suitable ways to counter those challenges. This review summarizes the toxicity issues of CNTs in vitro and in vivo in different organ systems (bio interphases) of the body that result in cellular toxicity.

  • Essential oils of Origanum compactum increase membrane permeability, disturb cell membrane integrity, and suppress quorum-sensing phenotype in bacteria
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-03-07
    Abdelhakim Bouyahya, Jamal Abrini, Nadia Dakka, Youssef Bakri

    The aim of this study was to investigate antibacterial activity of Origanum compactum essential oils collected at three phenological stages on Escherichia coli and Bacillus subtilis. The antibacterial activity was evaluated using the agar-well diffusion assay. The MIC and MBC values were determined using the micro-dilution assay. The investigation of the antibacterial action was carried out by the evaluation of the effect of O. compactum essential oils on the antibacterial kinetic growth, the integrity of cell membrane and permeability of the cell membrane. The anti-quorum sensing activity was tested by the inhibition of the biofilm formation. The findings of this study showed that O. compactum essential oil has potent antibacterial activities against E. coli and B. subtilis. The lowest inhibition value against B. subtilis was obtained with O. compactum essential oil at the post-flowering stage (MIC = MBC = 0.0312% (v/v)). The antibacterial mechanisms of O. compactum essential oils are related to the disturbing of the cell membrane integrity and the increasing of the membrane permeability, which leads to the leakage of genetic materials (DNA and RNA). Moreover, O. compactum essential oils inhibited the formation of the biofilms, a phenotype that has been known to be quorum sensing regulated.

  • Elucidating the interaction of kansui and licorice by comparative plasma/tissue metabolomics and a heatmap with relative fold change
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-06-01
    Yan-Yan Chen, Juan Shen, Yu-Ping Tang, Jin-Gao Yu, Jing Wang, Shi-Jun Yue, Jie Yang, Jia-Qian Chen, Li-Mei Feng, Zhen-Hua Zhu, Wei-Wei Tao, Li Zhang, Jin-Ao Duan
  • Temperature and eluent composition effects on enantiomer separation of carvedilol by high-performance liquid chromatography on immobilized amylose-based chiral stationary phases
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-04-04
    Cristina Panella, Rosella Ferretti, Adriano Casulli, Roberto Cirilli

    Carvedilol is a chiral drug with potent antihypertensive and antianginal activities. Although it is clinically used as a racemic mixture, its enantiomers show different pharmacokinetic and pharmacodynamic profiles. Here, the direct chiral separation of racemic drug by high performance liquid chromatography using two immobilized-type amylose-based chiral stationary phases is presented. Some chromatographic parameters, such as retention and selectivity, were determined under multimodal eluent conditions and different temperatures. A temperature-dependent inversion of the elution order of enantiomers was observed in the operative temperature range of chiral chromatographic support. Finally, an effective direct enantioselective method was successfully applied to the separation of the enantiomers of carvedilol on a semipreparative scale.

  • Composition analysis and antioxidant activities of the Rhus typhina L. stem
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-01-02
    Ting Liu, Zhaoqin Li, Ruiyun Li, Yue Cui, Yunli Zhao, Zhiguo Yu

    The present investigation reports the chemical composition of the Rhus typhina L. stem identified via mass spectrometry and NMR as gallic acid, 1-O-galloyl-β-D-glucose, tryptophan, scopolin, methyl gallate, fustin, quercetin, rutin, and 1,2,3,4,6-penta-O-galloyl-β-D-glucose. The antioxidant properties and the chemical composition contents of the R. typhina L. stem grown in different regions in China were determined. To determine the antioxidant activity, a total phenolic content analysis, 2, 2-diphenyl-1-picrylhydrazyl radical scavenging activity assay, ferric reducing antioxidant power assay, and β-carotene linoleic acid model system were conducted. The results showed that the Rhus typhina L. stem possessed high antioxidant capacities due to its high phenolic content. The contents of the nine isolated compounds were determined by UPLC-ESI-MS/MS. The calibration curves of the nine isolated compounds were linear within the concentration range and the average recoveries were high. The result showed that 1-O-galloyl-β-D-glucose, gallic acid, methyl gallate, and 1,2,3,4,6-penta-O-galloyl-β-D-glucose could be the compounds mainly responsible for the antioxidant capacity of the R. typhina L. stem. This reveals that the R. typhina L. stem is a good source of antioxidants.

  • Irbesartan desmotropes: Solid-state characterization, thermodynamic study and dissolution properties
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-10
    Andrea Mariela Araya-Sibaja, Carlos Eduardo Maduro de Campos, Cinira Fandaruff, José Roberto Vega-Baudrit, Teodolito Guillén-Girón, Mirtha Navarro-Hoyos, Silvia Lucía Cuffini

    Irbesartan (IBS) is a tetrazole derivative and antihypertensive drug that has two interconvertible structures, 1H- and 2H-tautomers. The difference between them lies in the protonation of the tetrazole ring. In the solid-state, both tautomers can be isolated as crystal forms A (1H-tautomer) and B (2H-tautomer). Studies have reported that IBS is a polymorphic system and its forms A and B are related monotropically. These reports indicate form B as the most stable and less soluble form. Therefore, the goal of this contribution is to demonstrate through a complete solid-state characterization, thermodynamic study and dissolution properties that the IBS forms are desmotropes that are not related monotropically. However, the intention is also to call attention to the importance of conducting strict chemical and in solid-state quality controls on the IBS raw materials. Hence, powder X-ray diffraction (PXRD) and Raman spectroscopy (RS) at ambient and non-ambient conditions, differential scanning calorimetry (DSC), hot stage microscopy (HSM), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM) techniques were applied. Furthermore, intrinsic dissolution rate (IDR) and structural stability studies at 98% relative humidity (RH), 25 °C and 40 °C were conducted as well. The results show that in fact, form A is approximately four-fold more soluble than form B. In addition, both IBS forms are stable at ambient conditions. Nevertheless, structural and/or chemical instability was observed in form B at 40 °C and 98% RH. IBS has been confirmed as a desmotropic system rather than a polymorphic one. Consequently, forms A and B are not related monotropically.

  • Voltammetric sensor based on cobalt-poly(methionine)-modified glassy carbon electrode for determination of estriol hormone in pharmaceuticals and urine
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-04-05
    Eliziana S. Gomes, Fernando R.F. Leite, Bruno R.L. Ferraz, Henrique A.J.L. Mourão, Andréa R. Malagutti

    A voltammetric sensor based on the electropolymerization of cobalt-poly(methionine) (Co-poly(Met)) on a glassy carbon electrode (GCE) was developed and applied for the determination of estriol by differential pulse voltammetry (DPV) for the first time. The electrochemical properties of the Co-poly(Met)/GCE were analysed by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to characterize the polymers on the GCE surface. The deposition of the Co-poly(Met) film on the GCE surface enhanced the sensor electronic transfer. CV studies revealed that estriol exhibits an irreversible oxidation peak at +0.58 V for the Co-poly(Met)/GCE (vs. Ag/AgCl reference electrode) in 0.10 mol/L Britton-Robinson buffer solution (pH = 7.0). Different voltammetric scan rates (10–200 mV/s) suggested that the estriol oxidation on the Co-poly(Met)/GCE surface is controlled by adsorption and diffusion processes. Based on the optimized DPV conditions, the linear responses for estriol quantification were from 0.596 μmol/L to 4.76 μmol/L (R2 = 0.996) and from 5.66 μmol/L to 9.90 μmol/L (R2 = 0.994) with a limit of detection (LOD) of 0.0340 μmol/L and a limit of quantification (LOQ) of 0.113 μmol/L. The DPV-Co-poly(Met)/GCE method provided good intra-day and inter-day repeatability with RSD values lower than 5%. Also, no interference of real sample matrices was observed on the estriol voltammetric response, making the DPV-Co-poly(Met)/GCE highly selective for estriol. The accuracy test showed that the estriol recovery was in the ranges 96.7%–103% and 98.7%–102% for pharmaceutical tablets and human urine, respectively. The estriol quantification in pharmaceutical tablets performed by the Co-poly(Met)/GCE-assisted DPV method was comparable to the official analytical protocols.

  • Highly sensitive simultaneous electrochemical determination of myricetin and rutin via solid phase extraction on a ternary Pt@r-GO@MWCNTs nanocomposite
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-03-22
    Satar Tursynbolat, Yrysgul Bakytkarim, Jianzhi Huang, Lishi Wang

    The simultaneous electrochemical determination of myricetin and rutin remains a challenge due to their indistinguishable potentials. To solve this problem, we constructed a ternary platinum nanoparticle, reduced graphene oxide, multi-walled carbon nanotubes ([email protected]@MWCNTs) nanocomposite via a facile one-pot synthetic method. Under the optimized conditions, the ternary [email protected]@MWCNTs nanocomposite exhibited good electrocatalytic activity toward myricetin and rutin via solid phase extraction and excellent performance for the simultaneous determination of myricetin and rutin. The oxidation peak current of myricetin was proportional to its concentrations in the range of 0.05–50 μM with a detection limit of 0.01 μM (S/N = 3). The linear range for rutin was 0.05–50 μM with a detection limit of 0.005 μM (S/N = 3). The ternary nanocomposite sensor also exhibited good reproducibility and stability, and was successfully used for the simultaneous determination of myricetin and rutin in real orange juice samples with recoveries ranging between 100.57% and 108.46%.

  • Pharmacokinetics and enterohepatic circulation of jervine, an antitumor steroidal alkaloid from Veratrum nigrum in rats
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-04-25
    Bingjing Zheng, Caihong Wang, Wenwen Song, Xiaoxia Ye, Zheng Xiang
  • Thermodynamics of clay – Drug complex dispersions: Isothermal titration calorimetry and high-performance liquid chromatography
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-12-05
    Ana-Maria Totea, Juan Sabin, Irina Dorin, Karl Hemming, Peter R. Laity, Barbara R. Conway, Laura Waters, Kofi Asare-Addo
  • Comparing different domains of analysis for the characterisation of N-Glycans on monoclonal antibodies
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-11-29
    Sara Carillo, Raquel Pérez-Robles, Craig Jakes, Meire Ribeiro da Silva, Silvia Millán Martín, Amy Farrell, Natalia Navas, Jonathan Bones
  • 更新日期:2019-12-11
  • 更新日期:2019-12-11
  • Comparative analysis of constitutes and metabolites for traditional Chinese medicine using IDA and SWATH data acquisition modes on LC-Q-TOF MS
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-11-19
    Dian Kang, Qingqing Ding, Yangfan Xu, Xiaoxi Yin, Huimin Guo, Tengjie Yu, He Wang, Wenshuo Xu, Guangji Wang, Yan Liang
  • Isoflavones influencing on pharmacokinetic profiles of main iridoids from Gardeniae Fructus in rats
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-11-14
    Ruirui Chang, Jialin Liu, Taohong Huang, Qiang Li, Jun Wen, Weidong Chen, Tingting Zhou
  • Vancomycin pretreatment attenuates acetaminophen-induced liver injury through 2-hydroxybutyric acid
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-11-06
    Ningning Zheng, Yu Gu, Ying Hong, Lili Sheng, Linlin Chen, Feng Zhang, Zimiao Weng, Weidong Zhang, Zean Zhang, Wei Jia, Houkai Li
  • Plant-derived secondary metabolites as the main source of efflux pump inhibitors and methods for identification
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-11-05
    Armel Jackson Seukep, Victor Kuete, Lutfun Nahar, Satyajit D. Sarker, Mingquan Guo
  • 更新日期:2019-12-11
  • 更新日期:2019-12-11
  • Erucic acid from Isatis indigotica Fort. Suppresses influenza A virus replication and inflammation in vitro and in vivo through modulation of NF-κB and p38 MAPK pathway
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-10-04
    Xiaoli Liang, Yuan Huang, Xiping Pan, Yanbing Hao, Xiaowei Chen, Haiming Jiang, Jing Li, Beixian Zhou, Zifeng Yang
  • Estimation of boswellic acids in herbal formulations containing Boswellia serrata extract and comprehensive characterization of secondary metabolites using UPLC-Q-Tof-MSe
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-10-01
    Kumar Katragunta, Bandi Siva, Niharika Kondepudi, P.R. Rao Vadaparthi, Nadendla Rama Rao, Ashok Kumar Tiwari, Katragadda Suresh Babu
  • 更新日期:2019-12-11
  • Potential synergic mechanism of Wutou-Gancao herb-pair by inhibiting efflux transporter P-gp
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-09-26
    Yufei HE, Zihong WEI, Ying XIE, Xiulin YI, Yong ZENG, Yazhuo LI, Changxiao LIU
  • 更新日期:2019-12-11
  • Development of a UHPLC-MS/MS method for the quantification of ilaprazole enantiomers in rat plasma and its pharmacokinetic application
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-09-17
    Fengting Ou, Ying Zhou, Jinxiu Lei, Su Zeng, Fuhai Wu, Ning Zhang, Lushan Yu
  • 更新日期:2019-12-11
  • FITC labeling of human insulin and transport of FITC-insulin conjugates through MDCK cell monolayer
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-29
    Darshana Shah, Yuxing Guo, Joseph Ocando, Jun Shao
  • 更新日期:2019-12-11
  • 更新日期:2019-12-11
  • Comparative analysis of twenty-five compounds in different parts of Astragalus membranaceus var. mongholicus and Astragalus membranaceus by UPLC-MS/MS
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-06-25
    Yuan Li, Sheng Guo, Yue Zhu, Hui Yan, Da-wei Qian, Han-qing Wang, Jian-qiang Yu, Jin-ao Duan

    As a traditional Chinese medicine, the root of Astragalus membranaceus var. mongholicus (AMM) or A. membranaceus (AM) has been widely used in China and other Asian countries for thousands of years. Till now, the flavonoids, phenolic acids and saponins are considered as the main active components contributed to their therapeutic effect in these plants. In order to clarify the distribution and contents of these compounds in different organs of these plants, a rapid and sensitive analytical method for simultaneous determination of 25 active compounds including seven types (dihydroflavones, isoflavane, isoflavones, flavones, pterocarpans, phenolic acid and saponins) within 10 min was established using ultra-pressure liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). Then, the established method was fully validated and successfully applied to the determination of the contents of these analytes in different parts (root, rhizome, stem, leaf and flower) of AMM and AM. The results indicated that the contents of the same type of compounds in two different species plants are significantly different. Moreover, the obvious differences were also found for the distribution and contents of different type of compounds in five organs of the same species. The present study could provide necessary information for the rational development and utilization of AMM and AM resource.

  • Analytical methodologies for determination of methotrexate and its metabolites in pharmaceutical, biological and environmental samples
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-06-20
    Forough Karami, Sara Ranjbar, Younes Ghasemi, Manica Negahdaripour
  • Rapid identification of chemical profile in Gandou decoction by UPLC-Q-TOF-MSE coupled with novel informatics UNIFI platform
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-05-15
    Li Xu, Yi Liu, Hongfei Wu, Huan Wu, Xiaochuang Liu, An Zhou

    Gandou decoction (GDD), a well-known traditional Chinese medicine (TCM) formula, has been widely used for decades to treat Wilson's disease (WD) in China due to its remarkable clinical effects. However, the chemical constituents of GDD still remain unclear because of their complexity. In this work, a reliable and sensitive strategy based on ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MSE) and UNIFI informatics platform was applied to investigate the chemical components in GDD. In total, 96 compounds including anthraquinones, alkaloids, protostane triterpenoids, flavonoids, triterpenoid saponins, tannins, curcuminoids, etc, were identified or tentatively characterized from GDD by comparing their retention time, accurate mass within 5 ppm error and MSE fragmentation patterns. Among them, eleven compounds were confirmed unambiguously with reference standards. Representative compounds in different chemical structure types were performed analysis of fragmentation patterns and characteristic ions. Moreover, to better understand the chemical contribution of individual herbs to the whole decoction, the corresponding each herb in GDD was also detected. This study developed a rapid method for characterizing the chemical constituents in GDD, which could not only be used for chemical standardization and quality control, but also be helpful for further research of GDD in vivo.

  • Analysis of pesticide residues in commercially available chenpi using a modified QuEChERS method and GC-MS/MS determination
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-01-31
    Shuang Li, Peipei Yu, Ceng Zhou, Ling Tong, Dongxiang Li, Zhiguo Yu, Yunli Zhao

    To ensure the safety of the commercially available chenpi, a convenient and fast analytical method was developed for the determination of 133 pesticide residues in chenpi using gas chromatography-tandem mass spectrometry (GC-MS/MS). In this study, different extraction solvents, redissolution solvents and adsorbents were tested according to the recovery and purification effect to obtain a modified QuEChERS method. The samples were extracted with acetonitrile. During the clean-up step, octadecyl-modified silica (C18) and graphitized carbon black (GCB) were selected, and aminopropyl (NH2) was used instead of primary secondary amine (PSA) because of its weaker ion exchange capacity which had little effect on the recovery of ditalimfos. Samples were quantified by matrix-matched calibration with internal standards. All pesticides showed good linearity in the respective range, both with values of r2 > 0.99. The average recoveries of the pesticides spiked samples ranged from 70.0% to 112.2% with the RSDs of 0.2%–14.4%. The modified QuEChERS method was validated and applied to twenty real samples. Five pesticides were found in eight batches, but no pesticide exceeded the maximum residue limits (MRL, MRL reference to European commission).

  • Quality control of Semen Ziziphi Spinosae standard decoction based on determination of multi-components using TOF-MS/MS and UPLC-PDA technology
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-01-02
    Di Wang, Qing Li, Ran Liu, Huarong Xu, Yidi Yin, Yifan Wang, Huijia Wang, Kaishun Bi

    A sensitive, fast and comprehensive method for the quality assessment of Semen Ziziphi Spinosae (SZS) standard decoction with characterization of its chemical components was developed and validated. UPLC-Q/TOF-MS/MS system was used to identify thirty-six chemical components of SZS standard decoction which included nucleosides, phenolic acids, alkaloids, and flavonoids. Furthermore, a UPLC-PDA method was validated to simultaneously determine adenosine, protocatechuic acid, magnoflorine, catechin, protocatechin, vicenin II, spinosin, kaempferol-3-rutinoside, and 6'''-feruloylspinosin which represent four species of characteristic compounds. The qualitative method had been validated according to Chinese Pharmacopoeia (2015 edition) in terms of lineary, repeatability, recovery and stability for all analytes, with the results showing good precision, accuracy and stability. In conclusion, the method using UPLC combined with MS and PDA provided a novel way for the standardization and identification of SZS standard decoction, and also offered a basis for qualitative analysis and quality assessment of the preparations for SZS standard decoction.

  • Study on degradation kinetics of epalrestat in aqueous solutions and characterization of its major degradation products under stress degradation conditions by UHPLC-PDA-MS/MS
    J. Pharm. Anal. (IF 4.44) Pub Date : 2018-08-15
    Hong Sun, Suyan Liu, Xun Gao, Zhili Xiong, Zhonggui He, Longshan Zhao

    Drug stability is closely related to drug safety and needs to be considered in the process of drug production, package and storage. To investigate the stability of epalrestat, a carboxylic acid derivative, a reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed in this study and applied to analyzing the degradation kinetics of epalrestat in aqueous solutions in various conditions, such as different pH, temperatures, ionic strengths, oxidation and irradiation. The calibration curve was A = 1.6 × 105C–1.3 × 103 (r = 0.999) with the liner range of 0.5–24 μg/mL, the intra-day and inter-day precision was less than 2.0%, as was the repeatibility. The average accuracy for different concentrations was more than 98.5%, indicating that perfect recoveries were achieved. Degradation kinetic parameters such as degradation rate constants (k), activation energy (Ea) and shelf life (t0.9) under different conditions were calculated and discussed. The results indicated that the degradation behavior of epalrestat was pH-dependent and the stability of epalrestat decreased with the rised irradiation and ionic strength; however, it was more stable in neutral and alkaline conditions as well as lower temperatures. The results showed that the degradation kinetics of epalrestat followed first-order reaction kinetics. Furthermore, the degradation products of epalrestat under stress conditions were identified by UHPLC-PDA-MS/MS, with seven degradation products being detected and four of them being tentatively identified.

  • Primmorph extracts and mesohyls of marine sponges inhibit proliferation and migration of hepatocellular carcinoma cells in vitro.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Hanaa Rady,Sohair Salem,Mohamed Ez El-Arab

    Cancer recurrence and severe side effects of currently being used chemotherapeutic agents reduce their clinical efficacy. Thus, there is a constant need to develop alternative anticancer drugs. Sustainable supply is an important challenge facing marine-based drug discovery. Primmorph, a 3D cell culture system, could provide a sustainable source to produce metabolites for anticancer drugs from marine sponges. In the present work, the anticancer activity of primmorph extracts and mesohyls of Negombata magnifica, Hemimycle arabica, Crella spinulata, and Stylissa carteri sponges was evaluated. Antiproliferative activity was studied in terms of cytotoxicity, colony formation, cell cycle, and apoptosis. Migration was assessed by migration assay and matrix metalloproteinase activity. The expression of proliferation and migration-related genes was analyzed using real time PCR. Migration and proliferation activities of HepG2 cells were inhibited by treatment with primmorph extracts and mesohyls of N. magnifica, H. arabica, and C. spinulata. The mesohyl of S. carteri did not show any anticancer activity although the primmorph extract led to cell cycle arrest. Among the selected sponge species, the primmorph extract of C. spinulata was the most promising anticancer agent regarding antiproliferative and antimigratory activities. In addition, primmorph extracts have the advantage of working under well-defined and controlled conditions, which allows the easy application as a bioreactor.

  • Interaction of repaglinide with bovine serum albumin: Spectroscopic and molecular docking approaches.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Suma K Pawar,Seetharamappa Jaldappagari

    Repaglinide (RPG) regulates the amount of glucose by stimulating the pancreas to release insulin in the blood. In view of its biological importance, we have examined the interaction between RPG and a model protein, bovine serum albumin (BSA) employing various spectroscopic, electrochemical and molecular docking methods. Fluorescence spectra of BSA were recorded in the presence and absence of RPG in phosphate buffer of pH 7.4. Fluorescence intensity of BSA was decreased upon the addition of increased concentrations of RPG, indicating the interaction between RPG and BSA. Stern-Volmer quenching analysis results revealed that RPG quenched the intensity of BSA through dynamic quenching mechanism. This was further confirmed from the time-resolved fluorescence measurements. The binding constant as calculated from the spectroscopic and voltammetric results was observed to be in the order of 104 M-1 at 298 K, suggesting the moderate binding affinity between RPG and BSA. Competitive experimental results revealed that the primary binding site for RPG on BSA was site II. Absorption and circular dichroism studies indicated the changes in the secondary structure of BSA upon its interaction with RPG. Molecular simulation studies pointed out that RPG was bound to BSA in the hydrophobic pocket of site II.

  • Spectrum-effect relationship between HPLC fingerprints and bioactive components of Radix Hedysari on increasing the peak bone mass of rat.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Xin-Yue Chen,San-Hu Gou,Zhi-Qiang Shi,Zhi-Yuan Xue,Shi-Lan Feng

    The traditional Chinese medicine of Radix Hedysari plays an important role in invigorating gas for ascending, benefiting blood for promoting production of fluid, and promoting circulation for removing obstruction in collaterals, which is consistent with the principle of treatment for osteoporosis. This study is designed to investigate the bioactive components on increasing peak bone mass (PBM) by exploring the spectrum-effect relationship between chromatography fingerprints and effect. Multiple indicators are selected to evaluate the pharmacological activity. In fingerprints, 21 common peaks are obtained, five of which are identified. Furthermore, gray relational analysis (GRA) is a quantitative method of gray system theory and is used to describe the correlation degree of common peaks and pharmacological activities with relational value. 21 components are then divided into three different regions, of which ononin and calycosin play an extremely significant role in increasing PBM. In addition, factor analysis and hierarchical cluster analysis (HCA) are used to screen the optimal producing area for Radix Hedysari. This provides a comprehensive and efficient method to improve the quality evaluation of Radix Hedysari, confirming the bioactive components for PBM-enhancement and further develop its medicinal value.

  • Determination of iohexol by capillary blood microsampling and UHPLC-MS/MS.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Valentin Ion,Caroline Legoff,Etienne Cavalier,Pierre Delanaye,Anne-Catherine Servais,Daniela-Lucia Muntean,Marianne Fillet

    One of the most important tools used to evaluate kidney function in the context of chronic kidney disease or other renal function related pathologies is the exploration of glomerular filtration rate (GFR). Iohexol is up to this moment a good candidate molecule for the GFR assessment since it exhibits minimum protein binding rates and minimum extra-renal clearance, being neither secreted nor reabsorbed at the tubular level. This study proposes and evaluates a new LC-MS/MS method for the iohexol determination from capillary blood, prelevated using volumetric absorbative microsampling (VAMS) systems. As an alternative to VAMS, a brand new HemaPEN® device for micro-prelevation was also tested. A new high throughput sample preparation protocol adapted for iohexol quantification from whole blood VAMS samples was developed. The medium term stability study of iohexol in dried whole blood VAMS samples that was conducted showed a good stability of this molecule for up to 12 days. By collecting only 10 μL of blood, iohexol can be analyzed from dried whole blood VAMS samples for concentration ranges between 1 and 250 μg/mL. Due to the analyte stability in VAMS for up to 12 days, this approach might be successfully applied for GFR assessment for clinical cases allowing minimum invasiveness and even delayed analysis.

  • Simultaneous determination of amino acids in different teas using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Yang Huang,Tiejie Wang,Marianne Fillet,Jacques Crommen,Zhengjin Jiang

    Tea is a widely consumed beverage and has many important physiological properties and potential health benefits. In this study, a novel method based on supercritical fluid chromatography coupled with mass spectrometry (SFC-MS) was developed to simultaneously determine 11 amino acids in different types of tea (green teas, Oolong tea, black tea and Pu-erh tea). The separation conditions for the analysis of the selected amino acids including the column type, temperature and backpressure as well as the type of additive, were carefully optimized. The best separation of the 11 amino acids was obtained by adding water (5%, v/v) and trifluoroacetic acid (0.4%, v/v) to the organic modifier (methanol). Finally, the developed SFC-MS method was fully validated and successfully applied to the determination of these amino acids in six different tea samples. Good linearity (r ≥ 0.993), precision (RSDs ≤ 2.99%), accuracy (91.95%-107.09%) as well as good sample stability were observed. The limits of detection ranged from 1.42 to 14.69 ng/mL, while the limits of quantification were between 4.53 and 47.0 ng/mL. The results indicate that the contents of the 11 amino acids in the six different tea samples are greatly influenced by the degree of fermentation. The proposed SFC-MS method shows a great potential for further investigation of tea varieties.

  • Performance comparison of chlorinated chiral stationary phases in supercritical fluid chromatography for separation of selected pyrrolidone derivatives.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Anca-Elena Dascalu,Alina Ghinet,Muriel Billamboz,Emmanuelle Lipka

    The effects of two chlorinated chiral stationary phases, namely, Lux Cellulose-2 and Lux i-Cellulose-5, flow-rate, percentage of co-solvent and chemical structures of the compounds on retention and resolution were studied within this article. In this work a backpressure of 150 bar, a temperature of 40 °C and 10% of methanol as co-solvent were chosen as operating conditions. The optimum flow-rate was 2 mL/min. The percentage of co-solvent was studied between 7.5% and 15%. We have observed that 15% of methanol gave the best results for most of the compounds. For all the derivatives, the Lux Cellulose-2 provided better resolutions going from 1.50 to 3.59 compared with Lux i-Cellulose-5.

  • Application of microfluidic chip technology in pharmaceutical analysis: A review.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Ping Cui,Sicen Wang

    The development of pharmaceutical analytical methods represents one of the most significant aspects of drug development. Recent advances in microfabrication and microfluidics could provide new approaches for drug analysis, including drug screening, active testing and the study of metabolism. Microfluidic chip technologies, such as lab-on-a-chip technology, three-dimensional (3D) cell culture, organs-on-chip and droplet techniques, have all been developed rapidly. Microfluidic chips coupled with various kinds of detection techniques are suitable for the high-throughput screening, detection and mechanistic study of drugs. This review highlights the latest (2010-2018) microfluidic technology for drug analysis and discusses the potential future development in this field.

  • Advances in capillary electro-chromatography.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Zhenkun Mao,Zilin Chen

    Capillary electrochromatography (CEC) is a micro-scale separation technique which is a hybrid between capillary electrophoresis (CE) and liquid chromatography (LC). CEC can be performed in packed, monolithic and open-tubular columns. In recent three years (from 2016 to 2018), enormous attention for CEC has been the development of novel stationary phases. This review mainly covers the development of novel stationary phases for open-tubular and monolithic columns. In particular, some biomaterials attracted increasing interest. There are no significant breakthroughs in technology and principles in CEC. The typical CEC applications, especially chiral separations are described.

  • Research advances in the detection of miRNA.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-08-28
    Jiawei Ye,Mingcheng Xu,Xueke Tian,Sheng Cai,Su Zeng

    MicroRNAs (miRNAs) are a family of endogenous, small (approximately 22 nucleotides in length), noncoding, functional RNAs. With the development of molecular biology, the research of miRNA biological function has attracted significant interest, as abnormal miRNA expression is identified to contribute to serious human diseases such as cancers. Traditional methods for miRNA detection do not meet current demands. In particular, nanomaterial-based methods, nucleic acid amplification-based methods such as rolling circle amplification (RCA), loop-mediated isothermal amplification (LAMP), strand-displacement amplification (SDA) and some enzyme-free amplifications have been employed widely for the highly sensitive detection of miRNA. MiRNA functional research and clinical diagnostics have been accelerated by these new techniques. Herein, we summarize and discuss the recent progress in the development of miRNA detection methods and new applications. This review will provide guidelines for the development of follow-up miRNA detection methods with high sensitivity and specificity, and applicability to disease diagnosis and therapy.

  • Development and validation of an LC-MS/MS method for tyrphostin A9.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Lyndsey F Meyer,Dhaval K Shah

    Here we have presented a sensitive and selective LC-MS/MS method for the quantification of tyrphostin A9, which is a selective inhibitor for platelet derived growth factor receptor tyrosine kinase and has been investigated in vitro as a potent oxidative phosphorylation uncoupler. The murine analytical method was developed for three biological matrices: cell culture media, 3T3-L1 cell lysate, and murine plasma. For each matrix the limit of detection and the limit of quantification were found to be 0.5 ng/mL and 1.0 ng/mL, respectively. The range of standard curve for each matrix was 1.0-100 ng/mL, linearity was >0.99, and the precision and accuracy were within 20%. 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propanoic acid was found to be the most suitable internal standard. The validated LC-MS/MS method was used to investigate stability and in vitro pharmacokinetics of tyrphostin A9. It was found that tyrphostin A9 is susceptible to hydrolysis, and the degradation product was identified as 3,5-di-tert-butyl-4-hydroxybenzaldehyde. Tyrphostin A9 was not stable in biological matrices, and the rate of its degradation in murine plasma was faster than that in cell culture media. In vitro pharmacokinetic studies revealed that tyrphostin A9 concentrations in the cell culture media declined in a bi-exponential manner and the concentrations inside the adipocytes remained constant, suggesting tyrphostin A9 has an intracellular binding site and is retained within the cell. The LC-MS/MS method presented here paves the way for further quantitative investigations involving tyrphostin A9.

  • Synthesis of highly fluorescent carbon dots from lemon and onion juices for determination of riboflavin in multivitamin/mineral supplements.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Severino S Monte-Filho,Stefani I E Andrade,Marcelo B Lima,Mario C U Araujo

    In this work, lemon and onion biomasses commonly found in street markets are for the first time used to develop a facile, fast and low-cost one-step microwave-assisted carbonization method for synthesis of highly fluorescent carbon dots (CDs). The structure and optical properties of CDs were investigated by TEM, XRD, XRF, UV-Vis, FTIR, and fluorescence spectroscopy. CDs displayed satisfactory optical proprieties, a high quantum yield of 23.6%, and excellent water solubility, and the particle size was 4.23-8.22 nm with an average diameter of 6.15 nm. An efficient fluorescent resonance energy transfer (FRET) between the CDs and riboflavin was achieved with CDs acting as donor and riboflavin as acceptor. A linear relationship between FRET and the riboflavin concentration from 0.10 to 3.0 μg/mL was observed, allowing the development of an accurate and fast analytical method to determine this vitamin in multivitamin/mineral supplements. Despite the potential interferences in these supplements, CDs were selective for riboflavin under optimized conditions. A paired t-test at a 95% confidence level indicated no statistically significant difference between the proposed and the reference methods. Recovery test presented values ranged from 96.0% to 101.4%. The limit of detection and relative standard deviation were estimated at 1.0 ng/mL and <2.6% (n = 3), respectively. CDs were successfully synthesized in a domestic microwave oven (1450 W, 6 min), presenting satisfactory parameters when compared with results of other studies reported in the literature, suggesting that the proposed method is a potentially useful method for the synthesis of CDs and determination of riboflavin.

  • Anticancer potential of metabolic compounds from marine actinomycetes isolated from Lagos Lagoon sediment.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Olabisi Flora Davies-Bolorunduro,Isaac Adeyemi Adeleye,Moshood Olushola Akinleye,Peng George Wang

    Thirty-two actinomycetes strains were isolated from sediment samples from 12 different sites at Lagos Lagoon and identified using standard physiological and biochemical procedures as well as 16S rDNA gene sequence analysis. Secondary metabolites were extracted from the strains and their anticancer activity on the K562 (Human acute myelocytic leukemia), HeLa (cervical carcinoma), AGS (Human gastric), MCF-7 (breast adenocarcinoma) and HL-60 (Human acute promyelocytic leukemia) cell lines was determined. The metabolic extracts exhibited cytotoxicity with IC50 values ranging from 0.030 mg/mL to 4.4 mg/mL. The Streptomyces bingchenggensis ULS14 extract was cytotoxic against all the cell lines tested. The bioactivity-guided extraction and purification of the metabolic extracts from this strain yielded two purified anticancer compounds: ULDF4 and ULDF5. The structures of the extracted compounds were determined using spectroscopic analyses, including electrospray ionization mass spectrophotometer and nuclear magnetic resonance (1 Dimensional and 2 Dimensional), and were shown to be structurally similar to staurosporine and kigamicin. The IC50 of ULDF4 and ULDF5 against the HeLa cell line was 0.034 μg/mL and 0.075 μg/mL, respectively. This study is the first to reveal the anticancer potential of actinomycetes from Lagos Lagoon, which could be exploited for therapeutic purposes.

  • Effect of an extraction solvent on the antioxidant quality of Pinus densiflora needle extract.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Thamizhiniyan Venkatesan,Young-Woong Choi,Young-Kyoon Kim

    Pinus densiflora needle extract (PDNE) is widely reported to have many pharmacological activities including antioxidant potential. However, the solvent system used for extraction greatly affects its antioxidant quality. Hence, in the present study, we investigated the effect of a different ratio (vol/vol) of ethanol to water (0-100%) in the extraction of PDNE with potent antioxidant capacity. The chemical assays, 2,2-diphenyl-1 picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS), were conducted to assess the antioxidant potential of PDNE. Subsequently, the cytoprotective effect of PDNE was determined using tert-butyl hydroperoxide (TBHP)-challenged HepG2 cellular model. The needle extracts from 40% ethanol (PDNE-40) showed greater radical scavenging activity followed by 60%, 20%, 80%, 0% and 100% ethanol extracts. EC50 value of the most active extract, PDNE-40, was 8.56 ± 0.51 μg/mL, relative to 1.34 ± 0.28 μg/mL of the standard trolox (for ABTS radical), and 75.96 ± 11.60 μg/mL, relative to 4.83 ± 0.26 μg/mL of the standard trolox (for DPPH radical). Either PDNE-20 or PDNE-40 pretreatment remarkably decreased the levels of reactive oxygen species (ROS), lipid peroxides and protein carbonyls in TBHP-challenged HepG2 cells. In addition, both PDNE-20 and PDNE-40 significantly reversed the decreased ratio of reduced (GSH) to oxidized (GSSG) glutathione. Moreover, these two extracts showed a significant inhibitory effect on TBHP-induced nuclear damage and loss of cell viability. In summary, the inclusion of 40% ethanol in water for extraction of Pinus densiflora needle greatly increases the antioxidant quality of the extract.

  • Preparation of polypyrrole/nanosilica composite for solid-phase microextraction of bisphenol and phthalates migrated from containers to eye drops and injection solutions.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Mehdi Ansari Dogaheh,Mansoureh Behzadi

    This paper describes the electrodeposition of polyphosphate-doped polypyrrole/nanosilica nanocomposite coating on steel wire for direct solid-phase microextraction of bisphenol A and five phthalates. We optimized influencing parameters on the extraction efficiency and morphology of the nanocomposite such as deposition potential, concentration of pyrrole and polyphosphate, deposition time and the nanosilica amount. Under the optimized conditions, characterization of the nanocomposite was investigated by scanning electron microscopy and Fourier transform infra-red spectroscopy. Also, the factors related to the solid-phase microextraction method including desorption temperature and time, extraction temperature and time, ionic strength and pH were studied in detail. Subsequently, the proposed method was validated by gas chromatography-mass spectrometry by thermal desorption and acceptable figures of merit were obtained. The linearity of the calibration curves was between 0.01 and 50 ng/mL with acceptable correlation coefficients (0.9956-0.9987) and limits of detection were in the range 0.002-0.01 ng/mL. Relative standard deviations in terms of intra-day and inter-day by five replicate analyses from aqueous solutions containing 0.1 ng/mL of target analytes were in the range 3.3%-5.4% and 5%-7.1%, respectively. Fiber-to-fiber reproducibilities were measured for three different fibers prepared in the same conditions and the results were between 7.3% and 9.8%. Also, extraction recoveries at two different concentrations were ≥96%. Finally, the suitability of the proposed method was demonstrated through its application to the analysis of some eye drops and injection solutions.

  • Compatibility of rubber stoppers for recombinant antitumor-antivirus protein injection by gas chromatography-mass spectrometry.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Zhaorui Meng,Xun Gao,Haifeng Yu,Lan Zhang,Xiangyong Yu,Longshan Zhao

    A simple, rapid, and sensitive gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the simultaneous determination of two fatty acids, methyl hexadecanoate (MH) and methyl stearate (MS), to allow the evaluation of packaging-drug compatibility. The two migrants were quantified in selective ion-monitoring (SIM) mode, with limits of detection (LOD) of 0.0030 μg/mL and 0.0121 μg/mL. Linear calibration curves for MH and MS were obtained in the concentration ranges of 0.1011-5.0570 μg/mL and 0.2015-10.0740 μg/mL, respectively. The developed method was successfully applied to estimate the safety of the injection of recombinant antitumor-antivirus protein (RAAP). The results showed that the possible maximum daily intake was 3.0 ng and 12.1 ng for MH and MS, respectively. As these values were both below the permitted daily exposure, the migrants can be considered as having low safety risk and do not affect the quality of the injection.

  • Prospects to the formation and control of potential dimer impurity E of pantoprazole sodium sesquihydrate.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Arun Kumar Awasthi,Lalit Kumar,Punit Tripathi,Madhava Golla,Cirandur Suresh Reddy,Pramod Kumar

    Pantoprazole sodium, a substituted benzimidazole derivative, is an irreversible proton pump inhibitor which is primarily used for the treatment of duodenal ulcers, gastric ulcers, and gastroesophageal reflux disease (GERD). The monographs of European Pharmacopoeia (Ph. Eur.) and United States Pharmacopoeia (USP) specify six impurities, viz.; impurities A, B, C, D, E and F, respectively for its active pharmaceutical ingredient (API). The identification and synthesis of all impurities except impurity E are well described in the literature; however, there is no report related to impurity E. The prospects to the formation and controlling of impurity E up to ≤0.03% in the synthesis of pantoprazole sodium sesquihydrate (PAN) were discussed in detail for the first time. The present work described the journey towards the successful development of an optimal preparation procedure of dimer impurity E. The most plausible mechanism involved in the formation of impurity E has been proposed.

  • Qualitative and quantitative assessment of related substances in the Compound Ketoconazole and Clobetasol Propionate Cream by HPLC-TOF-MS and HPLC.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    Wenling Yang,Xiaomei Yang,Fanghua Shi,Zhigang Liao,Yongkun Liang,Liangzhong Yu,Ruixun Wang,Qing Li,Kaishun Bi

    Related substances in pharmaceutical formulations are associated with their safety, efficacy and stability. However, there is no overall study already published on the assessment of related substances in the Compound Ketoconazole and Clobetasol Propionate Cream. In this work, a reliable HPLC-TOF-MS qualitative method was developed for the analysis of related substances in this preparation with a quick and easy extraction procedure. Besides the active pharmaceutical ingredients, two compounds named ketoconazole impurity B' optical isomer and ketoconazole impurity E were identified. Furthermore, a new HPLC method for qualitative and quantitative assessment on related substances and degradation products, which were found in the stability test, was established and validated. The single standard to determine multi-components method was applied in the quantitative analysis, which was an effective way for reducing cost and improving accuracy. This study can provide a creative idea for routine analysis of quality control of the Compound Ketoconazole and Clobetasol Propionate Cream.

  • Comparison of ELISA and HPLC-MS methods for the determination of exenatide in biological and biotechnology-based formulation matrices.
    J. Pharm. Anal. (IF 4.44) Pub Date : 2019-07-13
    A R Pinho,A Fortuna,A Falcão,A C Santos,R Seiça,C Estevens,F Veiga,A J Ribeiro

    The development of biotechnology-based active pharmaceutical ingredients, such as GLP-1 analogs, brought changes in type 2 diabetes treatment options. For better therapeutic efficiency, these active pharmaceutical ingredients require appropriate administration, without the development of adverse effects or toxicity. Therefore, it is required to develop several quantification methods for GLP-1 analogs products, in order to achieve the therapeutic goals, among which ELISA and HPLC arise. These methods are developed, optimized and validated in order to determine GLP-1 analogs, not only in final formulation of the active pharmaceutical ingredient, but also during preclinical and clinical trials assessment. This review highlights the role of ELISA and HPLC methods that have been used during the assessment for GLP-1 analogs, especially for exenatide.

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