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Journal of Pharmaceutical and Biomedical Analysis

Viviana Izzo, Bruno Charlier, Elena Bloise, Marine Pingeon, Marianna Romano, Antonietta Finelli, Alfonso Vietri, Valeria Conti, Valentina Manzo, Maria Alfieri, Amelia Filippelli, Fabrizio Dal Piaz
Exposure of healthcare workers to anticancer drugs requires the combined action of environmental and biological monitoring to assess the effective level of exposure to these chemicals, to improve awareness and to avoid adverse health effects on this category of workers. Cancer chemotherapeutic drugs show different mechanisms of action due to diverse chemical structures; consequently, they differ in hydrophobicity, pharmacokinetics and pharmacodynamics. Therefore, the appearance, accumulation and elimination of each of these molecules in body fluids and tissues might be extremely variable; this prompts the need for a rapid and versatile analytical protocol for the biological monitoring of possible exposure of workers involved in the manipulation, administration and disposal of cancer chemotherapeutic drugs...
March 13, 2018: Journal of Pharmaceutical and Biomedical Analysis
Peisheng Liang, Wangyong Zhu, Tianjun Lan, Qian Tao
Saliva secretion disorder is one of the most common symptoms in primary Sjögren syndrome (pSS). Salivary biomarkers related to saliva secretion disorder were identified in a pSS murine model, NOD/ShiLtJ mouse, using differential proteomic analysis. Candidate biomarkers were screened with Kyoto Encyclopedia of Genes and Genomes pathway analysis and validated in saliva and salivary glands by western blotting and immunohistochemistry (IHC). Biological functions were detected using ingenuity pathway analysis (IPA)...
March 12, 2018: Journal of Pharmaceutical and Biomedical Analysis
Münteha Nur Sonuç Karaboğa, Mustafa Kemal Sezgintürk
This paper illustrates a new and sensitive electrochemical immunosensor for the analysis of C-reactive protein. Indium Tin Oxide (ITO) disposable sheets were modified by using 3-cyanopropyltrimethoxysilane (CPTMS) self-assembled monolayers (SAMs) for the first time for immobilizing the anti-CRP antibody via covalent interactions without the need for any cross-linking agent. Cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS), as well as square wave voltammetry (SWV) methods were applied to characterize immobilization steps of anti-CRP and to determine the CRP concentration...
March 12, 2018: Journal of Pharmaceutical and Biomedical Analysis
Luca Scotti, Salvatore Genovese, Tonino Bucciarelli, Filippo Martini, Francesco Epifano, Serena Fiorito, Francesca Preziuso, Vito Alessandro Taddeo
An efficient analytical strategy based on different extraction methods of biologically active naturally occurring oxyprenylated umbelliferone and ferulic acid derivatives 7-isopentenyloxycoumarin, auraptene, umbelliprenin, boropinic acid, and 4'-geranyloxyferulic acid and quantification by UHPLC with spectrophotometric (UV/Vis) detection from Tea tree oil is reported. Absorption of the pure oil on Al2 O3 (Brockmann activity II) prior washing the resulting solid with MeOH and treatment of this latter with CH2 Cl2 resulted the best extraction methodology in terms of yields of oxyprenylated secondary metabolites...
March 10, 2018: Journal of Pharmaceutical and Biomedical Analysis
Bo Zhuang, Zhi-Ming Bi, Zi-Yuan Wang, Li Duan, Chang-Jiang-Sheng Lai, E-Hu Liu
Platycladi Cacumen (PC) is a traditional Chinese medicine used for the treatment of hemorrhages, cough, asthma and hair loss. To get a better understanding of the chemical constituents in PC, ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS) and diagnostic ion filtering strategy were firstly employed for chemical profiling of PC. A total of 43 compounds including organic acids and derivatives, flavonoids as well as phenylpropanolds were unambiguously or reasonably identified...
March 9, 2018: Journal of Pharmaceutical and Biomedical Analysis
Shuyu Zhan, Baoyue Ding, Yu-Er Ruan, Xuan Huang, Guoqiang Liu, Xiaoqing Lv, Xiong Huang, Mingjuan Li, Ninghua Jiang, Qing Shao
Microdialysis is a powerful in vivo sampling technique for pharmacokinetic-pharmacodynamic (PK-PD) modeling of drugs in pre-clinical and clinical studies. However, the noticeable limitations of previous studies using microdialysis were that animals anesthesia in the whole experiment and the combination of microdialysis and blood sampling for drug and (or) effect detection, which can obviously influence PK and PD behavior of drugs. In this study, a simple blood microdialysis sampling system in freely-moving rats was established for simultaneous study of PK and PD of Shengmai injection (SMI) effect on inducing real-time nitric oxide (NO) release on isoproterenol (ISO) induced myocardial ischemia rats...
March 9, 2018: Journal of Pharmaceutical and Biomedical Analysis
Caiqin Yang, Wei Guo, Yulong Lin, Qianqian Lin, Jiaojiao Wang, Jing Wang, Yanli Zeng
In this study, a new cocrystal of felodipine (Fel) and glutaric acid (Glu) with a high dissolution rate was developed using the solvent ultrasonic method. The prepared cocrystal was characterized using X-ray powder diffraction, differential scanning calorimetry, thermogravimetric (TG) analysis, and infrared (IR) spectroscopy. To provide basic information about the optimization of pharmaceutical preparations of Fel-based cocrystals, this work investigated the thermal decomposition kinetics of the Fel-Glu cocrystal through non-isothermal thermogravimetry...
March 8, 2018: Journal of Pharmaceutical and Biomedical Analysis
Jiaxing Kong, Jialei Shi, Zheyan Chen, Yuan Zeng, Hui Chang, Jiannong Ye, Qingcui Chu
A tributyl phosphate assisted hollow-fiber liquid-phase microextraction coupled with capillary electrophoresis-contactless coupled conductivity detection (HF-LPME/CE-C4 D) method has been developed for trace analysis of common short-chain fatty acids (SCFAs) without derivatization. Under the optimum conditions, ten SCFAs including a pair of isomers were well separated from their homologous FAs and the main coexisting inorganic anions within 40 min. Tributyl phosphate assisted HF-LPME produced excellent purification and enrichment for the model sample with high-salt matrix, microbial degradation fluid, and the limits of detection could reach 0...
March 8, 2018: Journal of Pharmaceutical and Biomedical Analysis
Wenge Chen, Yunlong Cheng, Jianzhong Chen, Jiahang Chen, Kai Jiang, Yuyang Zhou, Lee Jia
Mifepristone (RU486) is developed originally as a contraceptive used by hundreds of millions of women world-wide, and also reported as a safe and long-term psychotic depressant, or as a cancer chemotherapeutic agent used by both sexes. In our preliminary study aimed at developing mifepristone as a cancer metastatic chemopreventive, we coincidentally observed that blood mifepristone concentrations in female rats seem to be higher than those in male ones post administration. To substantiate if the pharmacokinetic differences between sexes exist, we established a fast UPLC-MS/MS method to determine mifepristone concentrations in plasma, and analyzed blood concentrations of mifepristone over time in rats and dogs of both sexes...
March 8, 2018: Journal of Pharmaceutical and Biomedical Analysis
Yongqiang Liu, Melissa Siard, Amanda Adams, Michael L Keowen, Travis K Miller, Frank Garza, Frank M Andrews, Navindra P Seeram
The human health benefits attributed to turmeric/curcumin spice has resulted in its wide utilization as a dietary supplement for companion pets and other animals including horses. While the quantification of free curcuminoids (curcumin, demethoxycurcumin, bisdemethoxycurcumin) and their phase-2 metabolites (curcumin-O-sulfate, curcumin-O-glucuronide) have been extensively investigated in human and rodent biological samples (primarily plasma and serum), there is lack of similar data for horses. Herein, we report a validated LC-ESI-MS/MS method for the simultaneous quantification of the aforementioned free curcuminoids and their metabolites in equine plasma...
March 7, 2018: Journal of Pharmaceutical and Biomedical Analysis
Atul Bhatnagar, Matthew J McKay, Megan Crumbaker, Ketan Ahire, Peter Karuso, Howard Gurney, Mark P Molloy
Abiraterone acetate is administered as a prodrug to patients with metastatic, castration-resistant prostate cancer (mCRPC) and is readily metabolized into the potent 17a-hydroxylase/17,20-lyase (CYP17) enzyme inhibitor and androgen receptor inhibitor abiraterone and Δ(4)-abiraterone (D4A), respectively. To investigate pharmacokinetic variability in abiraterone acetate metabolism we developed highly sensitive liquid chromatography/mass spectrometry (LC/MS) assays for the simultaneous quantitation of abiraterone and D4A in human plasma using high-resolution mass spectrometry (HRMS) on an Orbitrap mass spectrometer...
March 6, 2018: Journal of Pharmaceutical and Biomedical Analysis
C Gassner, R Karlsson, F Lipsmeier, J Moelleken
Previously we have introduced two SPR-based assay principles (dual-binding assay and bridging assay), which allow the determination of two out of three possible interaction parameters for bispecific molecules within one assay setup: two individual interactions to both targets, and/or one simultaneous/overall interaction, which potentially reflects the inter-dependency of both individual binding events. However, activity and similarity are determined by comparing report points over a concentration range, which also mirrors the way data is generated by conventional ELISA-based methods So far, binding kinetics have not been specifically considered in generic approaches for activity assessment...
March 6, 2018: Journal of Pharmaceutical and Biomedical Analysis
Mónika Bakonyi, Attila Gácsi, Anita Kovács, Mária-Budai Szűcs, Szilvia Berkó, Erzsébet Csányi
The application of local anesthetics, usually administered by subcutaneous injection, is common in the course of diagnostic, therapeutic, and cosmetic dermatology procedures. The effective dermal delivery of lidocaine could offer a solution to many adverse effects caused by needle insertion, such as pain, local reactions or toxicity, and additionally, it avoids the disruption of anatomical landmarks. Therefore, novel dermal formulations of local anesthetics are needed to overcome the barrier function of the skin and provide sufficient and prolonged anesthesia...
March 6, 2018: Journal of Pharmaceutical and Biomedical Analysis
Peristera-Maria Toziou, Panagiotis Barmpalexis, Paraskevi Boukouvala, Susan Verghese, Ioannis Nikolakakis
Since culture-based methods are costly and time consuming, alternative methods are investigated for the quantification of probiotics in commercial products. In this work ATR- FTIR vibration spectroscopy was applied for the differentiation and quantification of live Lactobacillus (La 5) in mixed populations of live and killed La 5, in the absence and in the presence of enteric polymer Eudragit® L 100-55. Suspensions of live (La 5_L) and killed in acidic environment bacillus (La 5_K) were prepared and binary mixtures of different percentages were used to grow cell cultures for colony counting and spectral analysis...
March 5, 2018: Journal of Pharmaceutical and Biomedical Analysis
Dandan Yao, Lei Zhang, Jiaojiao Huang, Chenghong Sun, Yu Zhang, Xiaoli Gu, Chong-Zhi Wang, Fei Li, Lina Chen, Chun-Su Yuan
In this work, surface magnetic molecularly imprinted polymers (SMMIPs) were synthesized and used as artificial receptors in the dispersive magnetic solid phase extraction (DMSPE) for capturing potential neuronal nitric oxide synthase-post synaptic density protein-95 (nNOS-PSD-95) uncouplers, which is known as neuroprotection against stroke. Factors that affected selective separation and adsorption of the artificial receptors, such as the amount of template, the types of functional monomer and porogen solvents, and the molar ratio of template/functional monomer/cross-linker were optimized...
March 3, 2018: Journal of Pharmaceutical and Biomedical Analysis
Hao Xiao, Mingyue Sun, Ruiyue Zhao, Haiyan Hong, Aili Zhang, Shuxian Zhang, Futao Liu, Yan Zhang, Yajing Liu, Lin Zhu, Hank F Kung, Jinping Qiao
Cassette dosing is also known as N-in-One dosing: several compounds are simultaneously administrated to a single animal and then the samples are rapidly detected by LC-MS/MS. This approach is a successful strategy to enhance the efficiency of drug discovery and reduce animal usage. However, no report on the utility of the cassette approach in radiotracer discovery has appeared in the literature. This study designed a cassette microdose with LC-MS/MS method to enhance the throughput for screening radiopharmaceutical biodistribution in the rat brain directly...
March 3, 2018: Journal of Pharmaceutical and Biomedical Analysis
Xinguang Sun, Yunfeng Zhang, Yinjun Yang, Jingjing Liu, Wei Zheng, Baiping Ma, Baolin Guo
Radix Dipsaci (RD), the dried root of Dipsacus asper, is used in traditional Chinese medicine as a remedy for bone fractures, traumatic hematoma, threatened abortion, and uterine bleeding. A novel ultra high-performance liquid chromatography coupled with quadrupole-time-of-flight tanderm mass spectrometry (UHPLC-Q-TOF/MS) approach was performed to rapidly characterize the chemical constituents of RD. Consequently, 21 compounds, including 12 iridoid glycosides (IGs), 4 furofuran lignans (FLs), and 5 phenolic acids (PAs) were discovered and identified from RD...
March 3, 2018: Journal of Pharmaceutical and Biomedical Analysis
Prashant S Devrukhakar, Shiva Shankar M, Shankar G, Srinivas R
Timolol (TIM) is a potent β-adrenergic blocker, useful in treatment of ocular hypertension or open-angle glaucoma. Development and validation of stability indicating LCMS assay method for TIM was accomplished coherent with ICH guideline. Successful chromatographic separation of TIM with its four degradation products was attained by using gradient elution mode on reverse phase column using ammonium acetate buffer, pH 4.6 as mobile phase A and organic solvent as the mobile phase B. Chromatographic conditions were set such as 1...
February 28, 2018: Journal of Pharmaceutical and Biomedical Analysis
Gurulingappa Hallur, Buchi Reddy Purra, Suresh P Sulochana, Neeraj Kumar Saini, Prasanthi Daram, Mohd Zainuddin, Ramesh Mullangi
A sensitive, specific, selective and rapid LC-ESI-MS/MS method has been developed and validated for the quantification of apalutamide in mice plasma using apalutamide-d3 as an internal standard (I.S.). Sample preparation was accomplished through a simple protein precipitation process. Chromatography of apalutamide and the I.S. was achieved on an Atlantis dC18 column using an isocratic mobile phase comprising 0.2% formic acid in water and acetonitrile (20:80, v/v) delivered at a flow rate of 0.8 mL/min. LC-MS/MS was operated under the multiple reaction-monitoring mode (MRM) using the electrospray ionization technique in positive ion mode and the transitions of m/z 478 → 450 and m/z 481 → 453 were used to measure the derivative of apalutamide and the I...
February 27, 2018: Journal of Pharmaceutical and Biomedical Analysis
Yulia B Monakhova, Jawed Fareed, Yiming Yao, Bernd W K Diehl
Nuclear magnetic resonance (NMR) spectroscopy is regarded as one of the most powerful and versatile analytical approaches to assure the quality of heparin preparations. In particular, it was recently demonstrated that by using1 H NMR coupled with chemometrics heparin and low molecular weight heparin (LMWH) samples derived from three major animal species (porcine, ovine and bovine) can be differentiated [Y.B. Monakhova et al. J. Pharm. Anal. 149 (2018) 114-119]. In this study, significant improvement of existing chemometric models was achieved by switching to 2D NMR experiments (heteronuclear multiple-quantum correlation (HMQC) and diffusion-ordered spectroscopy (DOSY))...
February 26, 2018: Journal of Pharmaceutical and Biomedical Analysis
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