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Showing papers in "Journal of analytical and bioanalytical techniques in 2017"


Journal ArticleDOI
TL;DR: Many important aspects of molecular docking in terms of its approaches, types, applications and challenges are briefly discussed in this article.
Abstract: Molecular docking is a kind of bioinformatic modelling which involves the interaction of two or more molecules to give the stable adduct. Depending upon binding properties of ligand and target, it predicts the three-dimensional structure of any complex. Molecular docking generates different possible adduct structures that are ranked and grouped together using scoring function in the software. Docking simulations predict optimized docked conformer based upon total energy of the system. In spite of all potential approaches, ligand chemistry (tautomerism and ionization), receptor flexibility (single conformation of rigid receptor) and scoring function (differentiate true binding mode) still remained the challenge. Many important aspects of molecular docking in terms of its approaches, types, applications and challenges are briefly discussed in this article.

106 citations


Journal ArticleDOI
Dan Jin, Shengxi Jin, Yang Yu, Colin Lee, Jie Chen 
TL;DR: Cannabis classification using a full spectrum of compounds will more closely meet the practical needs of cannabis applications in clinical research, insdustrial production, and patients’ self-production in Canada and will contribute to the standardization of commercially-available cannabis cultivars in support of a continuously growing market.
Abstract: For over a century, research on cannabis has been hampered by its legal status as a narcotic. The recent legalization of cannabis for medical purposes in North America requires rigorous standardization of its phytochemical composition in the interest of consumer safety and medicinal efficacy. To utilize medicinal cannabis as a predictable medicine, it is crucial to classify hundreds of cultivars with respect to dozens of therapeutic cannabinoids and terpenes, as opposed to the current industrial or forensic classifications that only consider the primary cannabinoids tetrahydrocannabinol (THC) and cannabidiol (CBD). We have recently developed and validated analytical methods using high-pressure liquid chromatography (HPLC-DAD) to quantify cannabinoids and gas chromatography with mass spectroscopy (GC-MS) to quantify terpenes in cannabis raw material currently marketed in Canada. We classified 32 cannabis samples from two licensed producers into four clusters based on the content of 10 cannabinoids and 14 terpenes. The classification results were confirmed by cluster analysis and principal component analysis in tandem, which were distinct from those using only THC and CBD. Cannabis classification using a full spectrum of compounds will more closely meet the practical needs of cannabis applications in clinical research, insdustrial production, and patients’ self-production in Canada. As such, this holistic classification methodology will contribute to the standardization of commercially-available cannabis cultivars in support of a continuously growing market.

35 citations


Journal ArticleDOI
TL;DR: In this paper, the level of common cations, anions, heavy metals and physical parameters in drinking water supply system in konso and its surrounding area, Southwestern of Ethiopia were determined.
Abstract: To improve water quality, there should be a mechanism of keeping safe water source from chemical contaminants in an effective and protective way through the application of regular check up and with interventions by taking exact measure periodically before it is supplied for usage. The intention of this research work is to determine the level of common cations, anions, heavy metals and physical parameters in drinking water supply system in konso and its surrounding area, Southwestern of Ethiopia. Water samples were collected from 23 different locations in the area where there is hand pump or motorized supply system that are used for drinking purpose. Collected samples were analyzed for physicochemical parameters including total alkalinity, Temperature, pH, Electrical Conductivity, Total dissolved solids, Turbidity, Alkalinity, Total hardness and Total suspended solid. Common cations (Li+, K+, Na+,Ca2+ and Mg2+), Common anions (NO3−, SO42−, PO42−, F− and Cl−) and Heavy metals (Pd, Ni, Mn, Pb, Co, Zn, Cu) were analyzed. The obtained results were compared with some national and international standards or guidelines for drinking water. Accordingly, the results obtained show that most of the physical and some common ions and heavy metals were within the accepted range of the guideline recommended by WHO. In addition to this, some parameters are at alarming state as compared to the WHO standards for drinking purposes, thereby suggesting the need for treatment and precautionary measures for use of the particular ground water.

22 citations


Journal ArticleDOI
TL;DR: A fast and simple microfluidic ZipChip CE-MS method to measure quality attributes of monoclonal antibody protein directly from cell culture supernatant and a good correlation of the levels of N-glycosylation attributes between ZipChipCE-MS of crude samples and RPLCMS analysis following Protein A (ProA) purification step has been demonstrated.
Abstract: Rapid and sensitive product quality analysis is important for real-time monitoring during biopharmaceutical development and manufacturing. However, low level of protein concentration and complex cell culture matrix pose challenges for product quality characterization at early stages of cell line selection and process development. Here, we describe a fast and simple microfluidic ZipChip CE-MS method to measure quality attributes of monoclonal antibody protein directly from cell culture supernatant. Cell culture supernatant samples were characterized with charge-based separation using microfluidic capillary electrophoresis coupled to a high-resolution mass spectrometer. Under sample reducing conditions, multiple protein glycosylation attributes were determined on the heavy chain, whereas titer information was obtained from comparison of light chain signal intensity following sample spiking-in with heavy labeled mAb. Therefore, the protein expression and product quality can be monitored using the same method with a single microfluidic device. A total volume of ten to fifty microliter of cell culture supernatant is needed, whereas analysis time is within three minutes per sample. In addition, comparison of new method with traditional RP-LC-MS method using a set of time-course bioreactor cell culture samples has been performed. A good correlation of the levels of N-glycosylation attributes between ZipChip CE-MS of crude samples and RPLCMS analysis following Protein A (ProA) purification step has been demonstrated.

20 citations


Journal ArticleDOI
TL;DR: In this paper, the photocatalytic properties of Titania-silica nanocomposite xerogels were described and the molar ratio of TEOS:TTIP:MtOH:DIW at 1: 1:6:14 respectively and the catalysts used were HCl and NH4OH.
Abstract: The use of titania-silica materials in photocatalytic processes has been proposed as an alternative to the conventional TiO2 catalysts, in order to facilitate the separation of products after the reaction. However, despite the large number of research in this field, the mechanism governing the photocatalytic activity of the mixed TiO2/SiO2 oxides is not clear. Titania-Silica nanocomposite xerogels were prepared by sol-gel method. This work has been used to describe the synthesis and the photocatalytic properties of TiO2-SiO2 nanocomposite xerogel. The nanocomposite xerogels were prepared by keeping the molar ratio of TEOS:TTIP:MtOH:DIW at 1: 1:6:14 respectively and the catalysts used were HCl and NH4OH. After the preparation xerogels were characterized by FTIR, XRD, UV and LLS. All these techniques show the amorphous nature of Titania-silica xerogel.

18 citations


Journal ArticleDOI
TL;DR: A good correlation between adenosine values measured by FAP and LC-MS/MS in whole blood and between LCMS/ MS and HPLC in plasma is found and mean adenosines concentration was higher in patients whatever the method used.
Abstract: Background: Adenosine is a nucleoside that impacts the cardiovascular system during cardiovascular or inflammatory diseases. The rapid determination of adenosine in blood may be useful in emergency medicine especially in syncope diagnose or septic shock. We compare its measurement in blood using fixed potential amperometry (FPA), with usual methods: mass spectrometry (LC-MS/MS) or high performance liquid chromatography (HPLC). Methods: Twenty healthy subjects (14 men and 6 women) and ten patients suffering from vasovagal syncope (VVS, 6 women and 4 men) were included. Blood samples were collected by vein puncture for plasma adenosine assay and in the same time using finger puncture for direct FAP measurement and on blotting paper for LC-MS/MS. Results: Mean plasma adenosine concentration was 26% higher using HPLC compared with LC-MSMS; p<0.01. In whole blood, adenosine concentration was 35% higher using FPA compared with LC-MS/MS. We found a good correlation between adenosine values measured by FAP and LC-MS/MS in whole blood and between LCMS/ MS and HPLC in plasma. Mean adenosine concentration was higher in patients whatever the method used. Conclusion: Adenosine measurement to the patient’s bed, using FPA may be useful in some cases where high adenosine is associated with pejorative outcome.

18 citations


Journal ArticleDOI
TL;DR: Continuous monitoring BA is useful in monitoring some abnormal physiological status such as T1D outpatients with very high BG or ketone bodies, as well as some adverse or abnormal physiological conditions such as diabetic ketoacidosis, low body mass index or a special daily activity.
Abstract: Although breath acetone (BA) has been identified as a breath biomarker for some abnormal metabolic status, such as diabetic ketoacidosis, diabetes under insulin treatments, on a ketogenic diet, heart congestion failure, and post intense exercises, many intra-individual biological parameters also influence the breath acetone concentration. Therefore, it would be insightful to study longitudinal variations of breath acetone concentration in given individuals that have no baseline effect resulting from individual physiological heterogeneity. We carried out a daily-based continuous monitoring of BA, blood glucose (BG), and blood ketone (BK) in 20 type 1 diabetic (T1D) outpatients and 5 healthy volunteers over a period of 30 days. 600 breath samples from the T1D outpatients and the healthy subjects were collected and tested. BA was measured using a cavity ringdown BA analyzer. Simultaneous BG and BK levels were also measured using a standard BG/ketone meter. Our findings include: (1) The T1D subjects have elevated mean BA concentrations as compared to the controls. (2) There exists a positive correlation (R=0.57, P<0.05) between the individual mean BA concentration and the individual mean BK in the 20 T1D outpatients. (3) Some adverse or abnormal physiological conditions such as diabetic ketoacidosis, low body mass index or a special daily activity (e.g., exercises) can be identified via an abnormal BA concentration. This study suggests that continuous monitoring BA is useful in monitoring some abnormal physiological status such as T1D outpatients with very high BG or ketone bodies.

17 citations


Journal ArticleDOI
TL;DR: In this paper, the authors highlighted the importance of seven heavy metals residual concentration including Cd, Cr, Cu, Fe, Mn, Ni and Zn in milk of Camel, Cattle, Buffalo, Sheep and Goat from various areas of Khyber Pakhtunkhwa (KPK), Pakistan.
Abstract: The determination of the seven elements was performed by Perkin Elmer Atomic Absorption (AA) spectrophotometer. The present study highlights the importance of seven heavy metals residual concentration including Cd, Cr, Cu, Fe, Mn, Ni and Zn in milk of Camel, Cattle, Buffalo, Sheep and Goat from various areas of Khyber Pakhtunkhwa (KPK), Pakistan. It revealed that milk of camel comprising of high levels of Zn (5.150 ± 0.021 mg/kg), Mn (0.094 ± 0.003 mg/kg) and Fe (1.580 ± 0.530 mg/kg) with a definite correlation. In the milk of buffalo, high concentration of noxious heavy metals including Cu (0.223 ± 0.010 mg/kg) and Cd (0.117 ± 0.086 mg/kg) were found whereas in goat milk, high Ni (1.152 ± 0.045 mg/kg) and Cr (1.152 ± 0.045 mg/kg) was observed and detected. The analysis showed that camel and buffalo have similar high concentration of heavy metals. Overall results showed that milk of cattle shows higher concentration of Zn, Mn and Fe along with Buffalo.

16 citations


Journal ArticleDOI
TL;DR: The development of a point-of-care (POC) analyzer that can rapidly measure both illicit and treatment drugs in patient saliva, ideally in the physician’s office, and with a degree of accuracy similar to chromatography is described.
Abstract: Buprenorphine is becoming the medication of choice to help patients withdraw from opioid addiction. However, treatment is compromised by the inability of physicians to assess patient usage during scheduled examinations. Here we describe the development of a point-of-care (POC) analyzer that can rapidly measure both illicit and treatment drugs in patient saliva, ideally in the physician's office, and with a degree of accuracy similar to chromatography. The analyzer employs a relatively simple supported liquid extraction to isolate the drugs from the saliva and surface-enhanced Raman spectroscopy (SERS) to detect the drugs. The SERS-based POC analyzer was used to identify buprenorphine and opioids in saliva samples by matching library spectra to samples collected from 7 veterans. The total analysis time, including sample preparation, was ~25 minutes. Buprenorphine concentration was estimated between 0 and 3 μg/mL. While no other prescription opioids were detected in any samples, heroin was identified in one sample; Δ-9 tetrahydrocannabinol (THC) was detected in 3 samples; and acetaminophen, caffeine, and nicotine were detected in several samples, none of which interfered with the measurements. The analysis was in very good agreement with urinalysis, correctly identifying the presence or absence of buprenorphine and THC in 13 of 14 measurements.

11 citations


Journal ArticleDOI
TL;DR: In this paper, an analytical methodology for quantification of 18 water soluble vitamers and secreted or biological forms in breast milk was presented. But the analytical approach has not been validated according to the EMA guidelines.
Abstract: With this report we present development, validation and application of an analytical methodology for the quantification of 18 water soluble vitamers and secreted or biological forms in breast milk. On a relatively low amount of breast milk (200 µL), we applied isotope dilution-based sample preparation based on a combination of enzymatic treatment and protein precipitation using acidic methanol enriched with stable isotope labelled internal standards. Compounds separation was achieved by reversed-phase liquid chromatography and detection performed by tandem mass spectrometry in positive electrospray ionization mode. To perform the quantification of 18 water soluble vitamers, procured pooled breast milk was used to build matrixmatched calibration curves, as labelled internal standards were not available for each vitamer. The analytical approach has been validated according to the EMA guidelines. The overall performance of the method was considered adequate, with 0.3- 28.3% and 0.9-32.6% intra and inter-day precision respectively and averaged accuracy reaching 92.2-107.5%. In addition, performed freeze/thaw stability studies showed the potential degradation of some vitamers. We therefore recommend particular attention in sample collection with rather having dedicated aliquots with small volumes. The feasibility of this analytical approach has been evaluated by quantifying various breast milk samples that were procured from an external supplier. The main forms found in breast milk were thiamine monophosphate for B1, flavin adenine nucleotide for B2, nicotinamide for B3, pyridoxal for B6 and 5-methyl tetrahydrofolic acid for B9. In addition, we newly reported nudifloramide as B3 form present in breast milk. With this analytical approach, it will give more confidence to provide a comprehensive assessment of the presence of water soluble vitamins in breast milk. This will enable the accurate evaluation of the nutritional requirements of infants.

10 citations


Journal ArticleDOI
TL;DR: In this article, the same brand's sunscreens with sun protection factor (SPF) of 8, 15, 30, and 50 were tested under identical experimental conditions, and the results showed that the UV absorbance and the transmittance of the sun screens are associated with the SPF value.
Abstract: Sunscreens are used to absorb or block harmful sunlight especially ultra violet (UV) radiation. An UV-vis spectrometer was employed to measure absorbance of sunscreen products. The same brand’s sunscreens with sun protection factor (SPF) of 8, 15, 30, and 50 were tested under identical experimental conditions. The results show that the UV absorbance and the transmittance of the sunscreens are associated with the SPF value. The maximum absorbance of the sunscreens measured between 280 to 320 nm (UVB region) is linearly proportional to the SPF value with a correlation coefficient of 0.998 using the same brand’s sunscreens. Thus, the absorbance can be used to evaluate the efficiency of a sunscreen that absorbs or blocks UVB radiation. Several commercial sunscreens of different brands but with the same SPF 30 were compared. The results confirmed that, although different brand sunscreens with the same SPF varied slightly in UV absorbance, they all offer adequate protection against UVB radiation. The utilization of UV-Vis spectroscopy is found to be particularly effective for determination of sunblock efficiency.

Journal ArticleDOI
TL;DR: In the present study, the extreme experimental conditions that offer worst result but still acceptable and likely to occur were predicted from the robustness test effects and the system suitability test (SST) limits were determined.
Abstract: A chromatographic method newly optimized to identify and assay four antihypertensive drugs in tablet dosage forms was complemented by a robustness test. The best system suitability criteria for numerous responses were evaluated on the basis of the robustness test results. Generally speaking, it is difficult to achieve a total satisfactory solution. Situations may also become ambiguous if the system suitability limits for few responses of a robust method are violated. In this context, it becomes crucial to redefine these limits based on the robustness test results. In the present study, the extreme experimental (worst-case) conditions that offer worst result but still acceptable and likely to occur were predicted from the robustness test effects. Eventually, replicated experiments were executed in such worst conditions and the system suitability test (SST) limits were determined.

Journal ArticleDOI
TL;DR: A new NHS-aryl azido heterobifunctional cross-linker based on an “introverted” carboxylic acid has been used to bring about successful intermolecular cross-linking of Lysozyme using bioinformatics software StavroX 3.6.0.1.
Abstract: A new NHS-aryl azido heterobifunctional cross-linker based on an “introverted” carboxylic acid has been used to bring about successful intermolecular cross-linking. As a ‘proof-of-concept’ Lysozyme was incubated with the crosslinker, then photolysed (366 nm, 6 W UV lamp), subjected to SDS-PAGE, excision of the ‘dimer’, trypsin digested and analyzed by ESI-MS and StavroX 3.6.0.1. Previous studies on crosslinking of Lysozyme (SI-I and SIII) using homobifunctional cross-linkers, either no cross-linking was observed or only two crosslinks were detected in the case of BS3, a smaller cross-linker. The heterobifunctional cross-linker described here leads to many more crosslinks, which have been identified by using mass spectrometry (ESI-MS) and StavroX 3.6.0.1, a bioinformatics software, especially suited for identifying intermolecular crosslinking.

Journal ArticleDOI
TL;DR: In this paper, a screen-printed electrode based on a graphite and polyurethane composite (SPGPU) was used in the determination of epinephrine (EP) in cerebral synthetic fluid (CSF) sample.
Abstract: A screen-printed electrode based on a graphite and polyurethane composite (SPGPU) was used in the determination of epinephrine (EP) in cerebral synthetic fluid (CSF) sample. Both Differential Pulse Voltammetry (DPV) and Square Wave Voltammetry (SWV) were used to investigate the suitability of sensor for determination of EP. Under the optimum conditions, the analyte oxidation signal was observed at 0.17 and 0.080 V for DPV and SWV, respectively (vs. pseudo-Ag¦AgCl) in phosphate buffer (pH=7.4). A linear region between 0.10 and 1.0 µmol L-1 was observed in DPV, with detection limit of 6.2 × 10-7 mol L-1 (R=0.997). In SWV two linear ranges were observed, the first one between 0.10 and 0.80 µmol L-1 and the second from 1.0 to 8.0 µmol L-1 with limit of detection 9.5 × 10-8 and 6.0 × 10-7 mol L-1 (R=0.998) respectively. Recoveries of 99 to 100% were observed using the sensor for determination of epinephrine in the CSF. Interference tests showed that uric and ascorbic acids as well as dopamine increase the current of epinephrine, with acceptable levels for UA. The use of a standard addition of EP in the CSF solution containing the ascorbic acid allowed minimizing such interference.

Journal ArticleDOI
TL;DR: The results suggest that Alchornea cordifolia is relatively non-toxic but has the propensity to induce hepatic injury at high doses.
Abstract: The ethanolic leaf extract of Alchornea cordifolia (Schum. and Thonn.) Mull. Arg (Euphorbiaceae), a widely used traditional medicinal plant was assessed for possible sub-acute toxicity in Swiss albino rats. The rats were randomly distributed into five groups of four animals each. The groups were respectively administered 125, 250, 500 and 750 mg/kg body weight ethanolic leaf extract of Alchornea cordifolia intra peritoneally daily for (two weeks) 14 days. Normal saline was administered to the control group according to their body weights. The experimental animals were observed for another 14 days before the termination of the experiment. The weight of the animals was recorded daily throughout the duration of the study. The number of deaths in any group was recorded. All the surviving animals were sacrificed after 28 days. Blood samples were collected for biochemical and haematological analysis. Selected organs of the animals i.e., liver and kidney of both the dead and sacrificed animals were removed and stored in 10% formal saline ready for histopathological analysis. Administration of Alchornea cordifolia (0.125- 0.75 g/kg, po daily) for two weeks (14 days) did not affect significantly the relative organ weights, blood chemistry and renal function. Histology of liver and kidney at dose levels up to 0.5 g/kg was normal and similarto vehicletreated controls. However, liver sections of mice treated with 0.75 g/kg Alchornea cordifolia ethanolic leaf extract showed cloudy swelling of hepatocytes with vascular degeneration. These results suggest that Alchornea cordifolia is relatively non-toxic but has the propensity to induce hepatic injury at high doses.

Journal ArticleDOI
TL;DR: The need of a robust, sensitive HPLC method for the quantitation of 6-thioguaninenucleotides and 6-methylmercaptopurine is indispensable to relate levels of these metabolites with emergence of signs of toxicity in patients undergoing treatment with 6-mercaptipurine (6-MP), paving the road to accurate dose calculations and thus providing a cost-effective treatment approach.
Abstract: The need of a robust, sensitive HPLC method for the quantitation of 6-thioguaninenucleotides (6-TG) and 6-methylmercaptopurine (6-MMP) is indispensable to relate levels of these metabolites with emergence of signs of toxicity in patients undergoing treatment with 6-mercaptopurine (6-MP), paving the road to accurate dose calculations and thus providing a cost-effective treatment approach. Previously reported methods were either laborious, required special types of C18 columns, or had long run times. A Design of Experiments (DoE) approach targeting the shortest run time with greatest selectivity was adopted using a user friendly HPLC method development simulation software (DryLab®). Analytes eluted within 10 min, at 3.8, 4.2, 5.6 and 7.5 min for 6-TG, 6-MP, 6-MMP and Dithiothreitol (DTT) respectively. Excellent recovery percentages of 90.9 ± 14.4, 87.8 ± 6.7 and 92.1 ± 9.08, respectively were obtained. The method proved its validity and robustness according to the International Conference on Harmonization (ICH) guidelines. The LOD of 6-MP, 6-TG and 6-MMP were 6, 9 and 24 pmol/8 × 108 RBCs, respectively. Twenty-Two Acute Lymphocytic Leukemia (ALL) children recruited from 57357 Cancer Hospital (Cairo, Egypt) had their 6-MP metabolites measured using the developed method. A strong negative correlation was manifested between TG and RBCs count and hemoglobin (p=0.009 and 0.002 respectively). WBC and neutrophils showed a negative correlation to TG at Continuation 1 phase of treatment, confirming the association of TG with myelotoxicity. The significant correlation between MMP and alanine aminotransferase (ALT) and aspartate aminotransferase (AST) (p=0.030, 0.004) explained its potential hepatotoxicity.

Journal ArticleDOI
TL;DR: Using benzo-18-crown-6 ether (B18C6), extraction experiments of cadmium picrate (CdPic2) into various diluents were performed at 298 K as mentioned in this paper, where three kinds of extraction constants, KCd/CdL, Kex± and Kex, four kinds of distribution constants, KD,j (=[j]org/[j]), with j=Pic−, CdLPic2, CdLLPic+ and CdL2+ and two kinds of ion-pair formation constants, K
Abstract: Using benzo-18-crown-6 ether (B18C6), extraction experiments of cadmium picrate (CdPic2) into various diluents were performed at 298 K. Thereby, three kinds of extraction constants, KCd/CdL, Kex± and Kex, four kinds of distribution constants, KD,j (=[j]org/[j]), with j=Pic−, CdLPic2, CdLPic+ and CdL2+ and two kinds of ion-pair formation constants, K1,org {=Kex±/KCd/CdL(KD,Pic)2} and K2,org (=Kex/Kex±), for L=B18C6 were determined. Here, KCd/CdL, Kex± and Kex were defined as [CdL2+]org/[Cd2+][L]org, [CdLPic+]org[Pic−]org/P and [CdLPic2]org/P, respectively, with P=[Cd2+][L]org[Pic−]2 and the subscript “org” denotes an organic phase. Based on these equilibrium constants, distribution properties of the species j between the water (w) and org phases and reactivity of CdL2+ or CdLPic+ in the org phases were compared. Additionally, some Pb2+ selectivity coefficients, kpotPbCd(=KCd/CdL/KPb/PbL), against Cd2+ with L=18-crown-6 ether at the nitrobenzene/w, 1,2-dichloroethane/w, o-dichlorobenzene/w and dichloromethane/w interfaces.

Journal ArticleDOI
TL;DR: The results showed that the breath acetone, BG, and BHB in the T1D rat group were significantly different from those in the healthy group (P<0.05), and the accuracy of diabetes screening using Breath acetone was analyzed using the receiver operating characteristic (ROC) analysis method and results showed the accuracy is low when the area under ROC curve (AUC) is <0.6425.
Abstract: We investigate correlations of breath acetone with blood glucose (BG) and blood beta-hydroxybutyrate (BHB) in a rat model of 126 streptozotocin-induced Type 1 diabetic (T1D) and 32 healthy rats, and evaluate the role of breath acetone analysis as a non-invasive alternative in diabetes screening and management. We conducted breath acetone analysis using a T1D rat model under various conditions, including fasting and insulin-treated. Breath acetone concentrations were measured using a cavity ringdown breath acetone analyzer, LaserBreath-001. The results showed that the breath acetone, BG, and BHB in the T1D rat group were significantly different from those in the healthy group (P<0.05). Significant positive relationships between breath acetone and blood BHB existed in both T1D and healthy groups, as well as in a group of T1D rats under fasting condition and insulin treatment. When the BG concentrations were grouped as follows: 16.5-24.4, 24.5-27.7, and 27.8-41.7 mmol/L, a moderate negative correlation between breath acetone and BG was observed in the T1D group. Furthermore, the accuracy of diabetes screening using breath acetone was analyzed using the receiver operating characteristic (ROC) analysis method and results showed that the accuracy is low when the area under ROC curve (AUC) is <0.6425.

Journal ArticleDOI
TL;DR: In this article, 17 Organochlorine Pesticides (OCPs) were evaluated in 14 surface sediment samples from a dam lake in Northwestern Turkey using GC-Mass system; HP (Hewlett Packard) 6890 series gas chromatograph coupled with HP 5973 mass spectrometer was used.
Abstract: Seventeen Organochlorine Pesticides (OCPs) were evaluated in 14 surface sediment samples from a dam lake in Northwestern Turkey. As analytical tool GC-Mass system; HP (Hewlett Packard) 6890 series gas chromatograph coupled with HP 5973 mass spectrometer was used. The HP 5MS capillary column had 30 m length with 0.32 mm internal diameter. A 0.25 mm film thickness cross-linked with stationary phase of 5% Phenyl methyl siloxane and Ultra-pure Helium gas was used as mobile phase. Ultrasonic bath extraction method was applied and cleaned up process were carried up with anhydrous Na2SO4 and Florisil column. Total pesticides concentrations were ranged from=0.237-2.39 mg/kg for dry weA„±ght. Percent total organic carbon (TOC) were observed between 1 and 3%. Average total OCP concentrations was 58.00 ± 45.44 mg/kg. The total concentrations of OCPs in sediment samples ranged from 12.9 to 169.9 mg/kg, with a mean value of 58.00 mg/kg. Although organochlorine pesticides have been banned in Turkey still the residues can be seen in sediment samples indicating the use of prohibited pesticides in the country. Comparison of organochlorine pesticides concentrations in sediment samples with other lakes in Turkey implies the higher concentration therefore higher usage of synthetic chemicals.

Journal ArticleDOI
TL;DR: Results indicate that functional DcIspF and D cIspH enzymes, which may play a pivotal role in the biosynthesis of diterpenoid in I. rubescens, are identified.
Abstract: Isodon rubescens, an important medical plant, contains various terpenoids. This plant’s active compounds are primarily oridonin with antitumor properties. As the precursor for oridonin biosynthesis, are synthesized by MEP pathway. On the basis of our earlier studies, we isolated and cloned two important genes catalyzing diterpenoid biosynthesis in the MEP pathway. 2-C-methyl-D-erythritol 2,4-cyclodiphosphate synthase and 4-hydroxy-3- methylbut-2-enyl diphosphate reductase are the fifth enzymes and the last step key enzyme for the methylerythritol phosphate (MEP) pathway, respectively, which is important for the regulation of isoprenoid biosynthesis. Sequence analysis revealed that DcIspF (accession no. KT948057) was 966 bp, contains a gene open reading frame (ORF) of 708 bp belonging to the MECDP-synthase superfamily and DcIspH (accession no KT948058) contains a 1389 bp ORF encoding a predicted 462 amino acid polypeptides as a member of the lytB_ispH superfamily. The deduced DcIspF and DcIspH amino acid sequences shared high similarity with DcIspF and DcIspH of other plant respectively, each of them exhibiting an N-terminal transit peptide and conserved amino acid sites. Quantitative real-time PCR analysis showed that the expression of DcIspF was considerably higher in leaves, the lowest in callus. These results indicate that we have identified functional DcIspF and DcIspH enzymes, which may play a pivotal role in the biosynthesis of diterpenoid in I. rubescens.

Journal ArticleDOI
TL;DR: A highly sophisticated and sensitive LC-MS/MS method has been developed and validated and can be significantly utilized for developing full pharmacokinetic profiling in individuals.
Abstract: Sensitive LC-MS/MS (Liquid Chromatography Tandem Mass Spectrometric) Method for the Simultaneous Determination of Alogliptin and Voglibose in human plasma. A highly sophisticated and sensitive LC-MS/MS method has been developed and validated for the Alogliptin and Voglibose simultaneous determination in human plasma. Alogliptin D3 and Miglitol were used as IS (Internal standard). Protein precipitation extraction was followed for the analytes and IS. Chromatography conditions included an isocratic mobile phase composing of 5 mM Ammonium formate: Acetonitrile in the ratio 50:50 v/v. The column used was Welchrom XB C18, with specifications of 50 × 4.6 mm, 5 μm, at a flow rate of 0.70 ml/min. The retention time of Alogliptin, Voglibose, Alogliptin D3 and Miglitol occurred at ~1.03, 0.8, 0.8 and 0.81 min respectively and the total chromatographic run time was 3.0 min. Alogliptin and Voglibose achieved a linear response function in human plasma at 5.09-509 ng/mL and 2.03-203 ng/mL respectively. Alogliptin and Voglibose achieved an intra and inter-day accuracy and precision in the range of 0.94- 4.35 and 0.91-3.89%; 1.41-10.8 and 1.90-7.75% respectively. The method was strictly validated according to the ICH guidelines. The results obtained from this study can be significantly utilized for developing full pharmacokinetic profiling in individuals.

Journal ArticleDOI
TL;DR: Trimethylphosphonium-substituted polyfluorenes (PTMPHFs) were synthesized using the Kumada catalyst-transfer polycondensation procedure, and their recognition properties towards various biomolecules were examined.
Abstract: Trimethylphosphonium-substituted polyfluorenes (PTMPHFs) with controlled molecular weights were synthesized using the Kumada catalyst-transfer polycondensation procedure, and their recognition properties towards various biomolecules were examined. Upon the formation of polyelectrolyte complexes with single stranded DNA (particularly polyadenine and polycytosine), the UV-vis absorption of PTMPHF was red-shifted and its fluo-rescence was quenched.

Journal ArticleDOI
TL;DR: In this paper, a method without a pre-analytical conditioning step was proposed to find out the reason for the decrease in propylene glycol levels in tobacco, and to propose a method that minimizes this loss.
Abstract: Humectants, especially glycerol and propylene glycol, are tobacco additives that are used to facilitate several processes in the production of tobacco products and to maintain the moisture content. Humectants in tobacco are usually detected by gas chromatography with flame ionization detection after a pre-analytical conditioning procedure. During this conditioning step, significant decreases of especially propylene glycol levels were observed. The goal of the present study is to find out the reason for this decrease, and to propose a method that minimizes this loss. Therefore, detailed studies were performed directed to this problem, which revealed that evaporation is the most likely source of this loss. Based on our findings, we propose a method without a pre-analytical conditioning step. Using the present method, in 10 different brands of commercially available cigarettes it was checked whether the measured concentrations of the humectants correspond with the declared concentrations as supplied by the manufacturers. The analysis showed that the measured levels were in general much lower than the specified amounts, possibly due to evaporation during processing tobacco to cigarettes. Therefore, it was suggested that the manufacturers should also specify the final amounts of humectants in cigarettes after the manufacturing process.

Journal ArticleDOI
TL;DR: In this paper, the removal of Methyl violet from aqueous solutions using the double perovskites BaSr2NbO5.5 are reported, where the oxides were prepared using solid state reaction in which the raw materials were mixed initially by either acetone or water.
Abstract: The removals of Methyl violet from aqueous solutions using the double perovskites BaSr2NbO5.5 are reported. The oxides were prepared using solid state reaction in which the raw materials were mixed initially by either acetone or water. The X-ray diffraction measurements demonstrated that the preparation methods have influenced the cell volume, crystal size and surface area of the oxides. As consequence, the adsorption properties were also affected. The study showed that the prepared oxides have a cubic structure with crystallite size is less than 82 nm. However, the crystallite size of the oxide obtained by wet method (W) is higher than that of the oxide obtained by dry method (D). Consequently, the amounts of the dye adsorbed by BaSr2NbO5.5 (D) were higher than those adsorbed by BaSr2NbO5.5 (W). The maximum removal capacities of Methyl violet are found to be 8.71 and 9.39 mg/g using BaSr2NbO5.5 (W) and BaSr2NbO5.5(D) respectively. The removals of the dye have positive relationship with pH, temperature, the specific surface area and the mass of the oxide.

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TL;DR: In this article, the biochemical composition of Sargassum muticum was evaluated by using classic colorimetric methods based on chemical analysis and Fourier Transform Infra-Red spectrometry (FTIR), and was used as a rapid and safe method that could bring advantages in screening studies and a more comprehensive management and use of seaweed products.
Abstract: Proliferation of the introduced brown macro alga Sargassum muticum is known as a natural and hard to control phenomenon occurring along the Atlantic coasts. The phenomenon causes serious troubles for local ecosystems including the alteration of ecosystem structure, the reduction in indigenous biodiversity and economic losses (tourism, aquaculture). However, despite the serious troubles caused by S. muticum, this species contains highly remarkable bioactive metabolites. This macro alga is at present under-exploited and the valorization of its metabolites to give a positive value to this seaweed could be a solution of ecosystemic service. Biorefinery process could be one solution to valorize S. muticum. Comprehensive knowledge concerning the biochemical composition of S. muticum and the impact of environmental factors, particularly seasons, on its composition is a prerequisite before its valorization. In this study, the biochemical composition of S. muticum was evaluated by using classic colorimetric methods based on chemical analysis and Fourier Transform Infra-Red spectrometry (FTIR), and was used as a rapid and safe method that could bring advantages in screening studies and a more comprehensive management and use of seaweed products. Our results are globally in accordance, notably for phenolic compounds, showing the relevance of the use of infrared spectrometry. Moreover, based on the absorption bands of some specific and valuable compounds shown by FTIR, there was a seasonal variation in the polysaccharides, i.e., uronic acids and sulphated compounds, together with phenolic contents of S. muticum.

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TL;DR: In this article, the effects of four functional monomers, namely acrylamide (AA), atropic acid (AT), methacrylic acid (MAA), and 4-vinylpyridine (4-VP), on the performance of a histamine (HIS) potentiometric sensor were examined by 1H nuclear magnetic resonance (NMR) spectroscopic methods.
Abstract: For the development of a histamine (HIS) potentiometric sensor based on molecularly imprinted polymers (MIPs), the effects of four functional monomers, namely acrylamide (AA), atropic acid (AT), methacrylic acid (MAA), and 4-vinylpyridine (4-VP), from which the MIP was synthesized, on the performance of the HIS sensor were examined by potentiometric and 1H nuclear magnetic resonance (NMR) spectroscopic methods. The intermolecular interactions between HIS as a template molecule and a functional monomer were investigated based on the 1H NMR spectra of HIS in distilled water in the presence of each functional monomer. Changes to the chemical shift of each HIS proton indicated that HIS typically formed a HIS-functional monomer complex at a ratio of 1:1 via hydrogen bonding with AA, AT and MAA, and interacted with 4-VP between the imidazole ring and pyridine ring of 4-VP. The potential changes of the four HIS sensors were measured in 0.1×10-3 mol L-1 aqueous solution using Ag/ AgCl as a reference electrode; the order of the magnitudes of the changes was MAA>AA=4-VP>AT. The potential changes of three non-imprinted polymer-modified potentiometric sensors prepared without HIS were smaller than those of the corresponding HIS sensors, except in the case of AT. The potential response and selectivity of the HIS sensor using MAA were better than those of the other three HIS sensors. The 1H NMR spectroscopic and potentiometric results showed that the hydrogen bond between HIS and MAA strongly and effectively influenced the potential response of the HIS sensor.

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TL;DR: In this paper, an attempt was made to standardise one of Dashmula, P. integrifolia and selected batches of marketed formulation using Apigenin and Luteolin as active biological marker for simultaneous quantification and fingerprinting through developed and validated HPTLC techniques.
Abstract: Dashmula are specific ayurvedic combination of ten roots used for various disorders of liver, kidney, uterus. Standardisation of herbals are necessity for efficacy and quality parameter as per WHO guidelines. Therefore, through this original research attempt was made to standardise one of ‘Dashmula’, P. integrifolia and selected batches of marketed formulation using Apigenin and Luteolin as active biological marker for simultaneous quantification and fingerprinting through developed and validated HPTLC techniques. Developed mobile phase Toluene: Ethyl acetate: Formic acid (6:4:0.15) gave Rf (Retention factor) 0.39 and 0.29 for Standard Apigenin and Luteolin respectively at 347 nm iso absorptive wavelength. The ethyl acetate extract of P. integrifolia (PI-ET), ‘Dashmularishtha’: Manufactuer 1; 3 coded batches as DF1, DF2, DF3, Manufacturer 2; 3 coded batches -as BF4, BF5, BF6, ‘Dashmulkadha’: Manufacturer 3; 3 coded batches as KF, KF8, KF9 were found to contain : 12.8% w/w, 0.294 mg/ml%, 0.429 mg/ ml%, 0.314 mg/ml%, 0.077 mg/ml%, 0.071 mg/ml%, 0.145 mg/ml%, 0.176 mg/ml%, 0.242 mg/ml%, 0.098 mg/ml% of Apigenin and 4.7% w/w, 0.542 mg/ml%, 0.365 mg/ml%, 0.569 mg/ml%, 0.343 mg/ml%, 0.311 mg/ml%, 0.607 mg/ ml%, 0.812 mg/ml%, 0.828 mg/ml%, 0.439 mg/ml% of Luteolin respectively. In stem powder of P. integrifolia 19.84 mg/gm% Apigenin and 7.433 mg/gm% Luteolin was calculated. The estimation shows variance in manufacturers and even within batches, but will be quality control parameter. The method was validated for specificity, linearity, accuracy, precision, and robustness. It was found to be linear in range of 40-120 ng/band with regression coefficient 0.9983, 0.9997 for Apigenin and luteolin. Percentage recovery study carried out for extract PI-ET and DF1 with spike of Apigenin and Luteolin at 80, 100 and 120% level, carried out for inter and intraday precision, subjected for one way ANOVA and found F value is below tabulated F(2,6) value 5.14, therefore there is no significance variance of obtained values.

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TL;DR: In this article, the environmental hazards due to natural radioactivity and human activities in Tuban delta in Yemen were discussed and evaluated using gamma ray spectroscopy, and the results showed that the mean activity concentrations of 238U series (226Ra), 232Th, and 40K were 16.83 ± 2.
Abstract: The knowledge of environmental hazards resulted from natural radioactivity and human activities is very important for monitoring of environmental contamination. In this study, the environmental hazards due to the natural radioactivity and human activities in Tuban delta in Yemen were discussed and evaluated using gamma ray spectroscopy. Thirty soil samples were collected from the study area. The results showed that the mean activity concentrations of 238U series (226Ra), 232Th, and 40K were 16.83 ± 2.3, 24.76 ± 2.3, 646.48 ± 13 Bq kg-1 and 15.22 ± 1.5, 21.99 ± 2.1, 472.58 ± 10 Bq kg-1 for farm soil samples treated with organic and urea fertilizer and farm soil samples treated with urea fertilizer, respectively. The corresponding values were 19.53 ± 1.5, 24.46 ± 3, and 500.76 ± 17 Bq kg-1 for uncultivated soil samples. The activity concentrations of 137Cs showed a significant value in some uncultivated soil samples. Also, physical and chemical properties of some soil samples were discussed and evaluated. A Radiological parameter, an absorbed dose rate in air, and an annual effective dose were calculated and evaluated. The results were compared with those of literature.

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TL;DR: The results suggesting that TNP-470 is a good candidate for transdermal drug delivery, whereas, an optimal dermal formulation would improve drug’s pharmacokinetic properties and toxicity profile by introducing it in a slow release system are suggested.
Abstract: Pathological angiogenesis is a critical component in cancer, in chronic systemic inflammatory diseases such as psoriasis and rheumatoid arthritis, and in ocular diseases. Anti-angiogenic drugs have the ability to prevent, inhibit, and regress newly formed blood vessels. The activity of TNP-470 (chloro acetylcarbamoylfumagillol), a potent anti-angiogenic drug, has been demonstrated in numerous preclinical studies and in eight clinical studies involving more than three hundred patients. Despite its encouraging efficacy, TNP-470 is unstable compound with short plasma half-life, and, as was found clinically it can cause neurotoxicity side-effects at high doses. In light of these limitations, developing a transdermal drug delivery for TNP-470, can offer a novel and promising clinical usage for this drug by improving its bioavailability, controlled dosage and safety profile. In this work, we developed a reliable method for skin permeation studies of TNP-470, using the pig skin in Franz diffusion cells and High-Performance Liquid Chromatography (HPLC) analysis. Additionally, we performed a broad stability and degradation studies of TNP-470 in different mediums and identify optimal stabilizing conditions in acetate buffer pH-4.5, which can be used for transdermal formulation. Our results demonstrated excellent permeability properties of TNP-470 through the pig skin, where 25% from the initial amount was crossed through the skin membrane after 72 hours. Our results suggesting that TNP-470 is a good candidate for transdermal drug delivery, whereas, an optimal dermal formulation would improve drug’s pharmacokinetic properties and toxicity profile by introducing it in a slow release system.

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TL;DR: Two improved versions of a Fluorescence recovery after photobleaching (FRAP) technique using different fluorescent dyes are presented, which allow to correct the fluorescence signal intensity of the protein of interest for different transfection rates of individual cells.
Abstract: Traditionally, studies on protein translation rely on systems, in which cells have been lysed prior determination of levels of the protein of interest. However, these assays do not reflect the protein synthesis in living cells in real time, but analyze protein levels after a given incubation time, leading to limitations in results based on experimental parameters. To overcome this problem, we have previously established a Fluorescence recovery after photobleaching (FRAP)-based technique to monitor protein translation in living cells. For this, the protein of interest fused to green fluorescent protein (GFP) is expressed in cell lines. After bleaching the entire cell, the fluorescent signal of the protein of interest is lost, allowing to capture the signal recovery of newly translated GFPtagged protein over time. Here we present two improved versions of this technique using different fluorescent dyes: tFRAP (translational FRAP). For the first improved version of tFRAP we have inserted a second fluorescent dye, red fluorescent protein (RFP), into the same expression vector that drives expression of the protein of interest fused to GFP driven by a second promoter. For the second improved version of tFRAP we have fused our protein of interest to a photo-switchable dye, Dendra2. Both improved versions allow to correct the fluorescence signal intensity of the protein of interest for different transfection rates of individual cells. These two advanced techniques are new powerful tools for quantifying translation rates in living cells and will be useful in future studies on mRNA translation.