Journal of Pharmaceutical Analysis

Preface for Advances in Pharmaceutical Analysis 2017

Zilin Chen

2018, 8(4)

Abstract(66) PDF(0)

Abstract:
The year of 2017 is of historic importance for China. It was the year that China started to step into New Period. It was also the year that I had joined Wuhan University as a Luojia professor and set up my research group for ten years since I came back to China from University of Notre Dame, United States in 2007.

Instructions to Authors

2018, 8(4): 封3-封4.

Abstract(52) PDF(0)

Abstract:

Advances in tumor-endothelial cells co-culture and interaction on microfluidics

Weiwei Li, Mashooq Khan, Sifeng Mao, Shuo Feng, Jin-Ming Lin

2018, 8(4): 210-218.

Abstract(141) PDF(6)

Abstract:
The metastasis in which the cancer cells degrade the extracellular matrix (ECM) and invade to the sur-rounding and far tissues of the body is the leading cause of mortality in cancer patients. With a lot of advancement in the field, yet the biological cause of metastasis are poorly understood. The microfluidic system provides advanced technology to reconstruct a variety of in vivo-like environment for studying the interactions between tumor cells (TCs) and endothelial cells (ECs). This review gives a brief account of both two-dimensional models and three-dimensional microfluidic systems for the analysis of TCs-ECs co-culture as well as their applications to anti-cancer drug screening. Furthermore, the advanced methods for analyzing cell-to-cell interactions at single-cell level were also discussed.

Analytical methods for investigating in vivo fate of nanoliposomes:A review

Chong Su, Yingze Liu, Yang He, Jingkai Gu

2018, 8(4): 219-225.

Abstract(108) PDF(3)

Abstract:
Nanoliposomes are considered to be the most successful nanoparticle drug delivery system, but their fate in vivo has not been fully understood due to lack of reliable bioanalytical methods, which seriously limits the development of liposomal drugs. Hence, an overview of currently used bioanalytical methods is imperative to lay the groundwork for the need of developing a bioanalytical method for liposome measurements in vivo. Currently, major analytical methods for nanoliposomes measurement in vivo include fluorescence labeling, radiolabeling, magnetic resonance imaging (MRI), mass spectrometry and computed tomography.In this review, these bioanalytical methods are summarized, and the advantages and disadvantages of each are discussed. We provide insights into the applicability and limitations of these analytical methods in the application of nanoliposomes measurement in vivo, and highlight the recent development of instrumental analysis techniques. The review is devoted to providing a comprehensive overview of the investigation of nanoliposomes design and associated fate in vivo, promoting the development of bioanalytical techniques for nanoliposomes measurement, and understanding the pharmacokinetic behavior, effectiveness and potential toxicity of nanoliposomes in vivo.

Recent advances in screening of enzymes inhibitors based on capillary electrophoresis

Mengxia Cheng, Zilin Chen

2018, 8(4): 226-233.

Abstract(123) PDF(0)

Abstract:
Capillary electrophoresis with many advantages plays an important role in pharmaceutical analysis and drug screening. This review gives an overview on the recent advances in the developments and applications of capillary electrophoresis in the field of enzyme inhibitor screening. The period covers 2013 to 2017. Both the pre-capillary enzyme assays and in-capillary enzyme assays which include electrophoretically mediated microanalysis (EMMA) and immobilized enzyme microreactor (IMER) are summarized in this article.

Unusual retention behavior of omeprazole and its chiral impurities B and E on the amylose tris (3-chloro-5-methylphenylcarbamate) chiral stationary phase in polar organic mode

Rosella Ferretti, Leo Zanitti, Adriano Casulli, Roberto Cirilli

2018, 8(4): 234-239.

Abstract(60) PDF(1)

Abstract:
Recent reports have demonstrated that the new commercially available immobilized-type chiral stationary phases (CSPs) containing amylose tris(3-chloro-5-methylphenylcarbamate) (ACMPC) as a selector exhibit not only an exceptionally high enantioselectivity in high-performance liquid chromatography (HPLC) but they are also applicable to a wide range of chiral analytes. Herein, we report the results obtained in the HPLC analysis of omeprazole and its impurities B and E on the ACMPC-based Chiralpak IG-3 CSP (CSP) under polar organic conditions. A systematic evaluation of the retention characteristics of the selected benzimidazole chiral probes was carried out by changing the composition of the mobile phase and the column temperature. It is worth emphasizing that the high affinity of both enantiomers of all analytes recorded in pure methanol mode dramatically decreased incorporating small volumes of either basic or acid additives in the mobile phase. Unspecified sites of the IG-3 CSP presumably involved in strong and non-stereoselective H-bonding contacts with chiral analytes are assumed responsible for the unproductive retention process.

Screening potential mitochondria-targeting compounds from traditional Chinese medicines using a mitochondria-based centrifugal ultrafiltration/liquid chromatography/mass spectrometry method

Xing-Xin Yang, Yu-Zhen Zhou, Feng Xu, Jie Yu, Gegentana, Ming-Ying Shang, Xuan Wang, Shao-Qing Cai

2018, 8(4): 240-249.

Abstract(192) PDF(5)

Abstract:
Mitochondria regulate numerous crucial cell processes, including energy production, apoptotic cell death, oxidative stress, calcium homeostasis and lipid metabolism. Here, we applied an efficient mitochondria-based centrifugal ultrafiltration/liquid chromatography/mass spectrometry (LC/MS) method,also known as screening method for mitochondria-targeted bioactive constituents (SM-MBC). This method allowed searching natural mitochondria-targeting compounds from traditional Chinese medicines(TCMs), including Puerariae Radix (PR) and Chuanxiong Radix (CR). A total of 23 active compounds were successfully discovered from the two TCMs extracts. Among these 23 hit compounds, 17 were identified by LC/MS, 12 of which were novel mitochondria-targeting compounds. Among these, 6 active compounds were analyzed in vitro for pharmacological tests and found able to affect mitochondrial functions. We also investigated the effects of the hit compounds on HepG2 cell proliferation and on loss of cardiomyocyte viability induced by hypoxia/reoxygenation injury. The results obtained are useful for in-depth understanding of mechanisms underlying TCMs therapeutic effects at mitochondria level and for developing novel potential drugs using TCMs as lead compounds. Finally, we showed that SM-MBC was an efficient protocol for the rapid screening of mitochondria-targeting constituents from complex samples such as PR and CR extracts.

Simultaneous determination of steroid drugs in the ointment via magnetic solid phase extraction followed by HPLC-UV

Yadollah Yamini, Meysam Safari, Maryam Shamsayei

2018, 8(4): 250-257.

Abstract(76) PDF(1)

Abstract:
The copper-coated iron oxide nanoparticles with core-shell were produced by deposition of a Cu shell on Fe3O4 NPs through reduction of Cu2+ ions in solution using NaBH4. Subsequently, the organosulfur compound, bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid (b-TMP-DTPA), was used to form self-assembled monolayer in order to modify sorbent's surface via covalent bonding between Cu and thiol (-SH) terminal groups. The prepared magnetic nanoparticles were characterized by using Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscope (TEM), vibrating sample magnetometer (VSM) and thermo gravimetric analysis (TGA). Then, the application of this new sorbent was investigated to extract the steroid drugs in ointment samples with the aid of ultrasound.An external magnetic field was applied to collect the magnetic nanoparticles (MNPs). The extracted analytes were desorbed using acetonitrile. The obtained extraction solution was analyzed by HPLC-UV. The main affecting factors on the extraction efficiency including pH, sonication time, amount of sorbent, salt concentration, and desorption conditions were optimized in detail. Under the optimum conditions, good linearity was obtained in the range of 2.5-250.0 μg/ L with reasonable linearity (R2 > 0.99) and the limits of detection (LODs) ranged between 0.5 and 1.0 μg/L (based on S/N = 3). Repeatability (intra-day precision) based on five replicates and preconcentration factors were calculated to be 3.6%-4.7% and 87116,respectively.Relative recoveries in ointment samples at two spiked levels of the target analytes were obtained in the range of 90.0%-103.2%. The results illustrated that the Fe3O4@Cu@ b-TMP-DTPA NPs have the capability of extraction of steroid drugs from ointment samples.

Extracellular synthesis of silver nanoparticles by Pseudomonas sp. THG-LS1.4 and their antimicrobial application

Hina Singh, Juan Du, Priyanka Singh, Tae Hoo Yi

2018, 8(4): 258-264.

Abstract(207) PDF(1)

Abstract:
Silver nanoparticles (AgNPs) are known to have bacteriostatic and bactericidal effects. The present study highlights the extracellular synthesis of AgNPs and its antibacterial properties. The AgNPs were synthesized using Pseudomonas sp. THG-LS1.4 strain which had been isolated from soil. The AgNPs werecharacterized by field emission-transmission electron microscopy (FE-TEM), X-ray diffraction (XRD),Fourier transform-infrared (FT-IR) spectroscopy, and particle size distribution (DLS). The AgNPs displayed maximum absorbance at 412 nm and were irregular in shape ranging from 10 to 40 nm. The XRD spectroscopy results demonstrated the crystalline nature of nanoparticles. The AgNPs showed antimicrobial activity against Bacillus cereus, Staphylococcus aureus, Candida tropicalis, Vibrio parahaemolyticus,Escherichia coli and Pseudomonas aeruginosa. Furthermore, the AgNPs were also evaluated for their increased antibacterial activities with various antibiotics against Escherichia coli, Pseudomonas aeruginosa and Salmonella enterica. Additionally, AgNPs showd biofilm inhibition activity. The biosynthesized AgNPs were found to be a potent agent against tested pathogens. More importantly, we highlight the applications of AgNPs as an antimicrobial agent.

Duplex microRNAs assay based on target-triggered universal reporter hybridization

Yinan Wang, Yue Sun, Choiwan Lau, Jianzhong Lu

2018, 8(4): 265-270.

Abstract(81) PDF(1)

Abstract:
In this paper, we designed and evaluated a duplex detection strategy for microRNAs (miRNAs) using universal probe-based target-triggered double hybridization and fluorescent microsphere-based assay system (xMAP array). In the absence of target miRNA, reporter DNA cannot hybridize stably with the immobilized capture DNA due to its low melting temperature. Only after adding target miRNA, can reporter probe hybridize with capture probe to form a stable three-component complex. This targettriggered stable hybridization makes this method possible for highly selective and sensitive detection of multiple miRNAs. We exemplified a quantitative detection of duplex miRNAs with a limit of detection of 40 pM. The xMAP array platform holds the potential of extending this approach to simultaneous detection of up to 100 miRNA targets. Considering the simplicity, rapidity and multiplexing, this work promised a potential detection of multiple miRNA biomarkers for early disease diagnosis and prognosis.

Quantitation of tadalafil in human plasma using a sensitive and rapid LC-MS/MS method for a bioequivalence study

Abhaysingh Bhadoriya, Bhavesh Dasandi, Dharmesh Parmar, Priyanka A. Shah, Pranav S. Shrivastav

2018, 8(4): 271-276.

Abstract(85) PDF(1)

Abstract:
A highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of tadalafil (TAD) in human plasma. TAD and its deuterated internal standard (IS), tadalafil-d3, were extracted from 200 μL plasma using Phenomenex Strata-X-C 33 μ extraction cartridges.Chromatographic analysis was carried out on Synergi? Hydro-RP C18 (100mm × 4.6 mm, 4 μm) column with a mobile phase consisting of methanol and 10mM ammonium formate, pH 4.0 (90:10, v/v),delivered at a flow rate of 0.9 mL/min. Quantitation of the protonated analyte was done on a triple quadrupole mass spectrometer using multiple reaction monitoring via electrospray ionization. The precursor to product ions transitions monitored for TAD and TAD-d3 were m/z 390.3 → 268.2 and m/z 393.1 → 271.2, respectively. The calibration curve was linear over the concentration range of 0.50-500 ng/mL with correlation coefficient, r2 ≥ 0.9994. Acceptable intra-batch and inter-batch precision (≤3.7%) and accuracy (97.8% to 104.1%) were obtained at five concentration levels. The recovery of TAD from spiked plasma was highly precise and quantitative (98.95% to 100.61%). Further, the effect of endogenous matrix components was minimal. TAD was found to be stable under different storage conditions in human plasma and also in whole blood samples. The validated method was successfully used to determine TAD plasma concentration in a bioequivalence study with 20 mg TAD tablets in 24 healthy volunteers. Method performance was evaluated by reanalyzing 115 study samples.

2018 Vol. 8, No. 4