96 research outputs found
Validated HPTLC Method for Quantification of Luteolin and Apigenin in Premna mucronata Roxb., Verbenaceae
Full text linkA simple, rapid, and precise high-performance thin-layer chromatographic method was developed for quantitative estimation of luteolin and apigenin in Premna mucronata Roxb., family Verbenaceae. Separation was performed on silica gel 60 F254 HPTLC plates using toluene : ethyl acetate : formic acid (6 : 4 : 0.3) as mobile phase for elution of markers from extract. The determination was carried out in fluorescence mode using densitometric absorbance-reflection mode at 366 nm for both luteolin and apigenin. The methanolic extract of Premna mucronata was found to contain 10.2 mg/g % luteolin and 0.165 mg/g % of apigenin. The method was validated in terms of linearity, LOD and LOQ, accuracy, precision, and specificity. The calibration curve was found to be linear between 200 and 1000 ng/band for luteolin and 50 and 250 ng/band for apigenin. For luteolin and apigenin, the limit of detection was found to be 42.6 ng/band and 7.97 ng/band while the limit of quantitation was found to be 129.08 ng/band and 24.155 ng/band, respectively. This developed validated method is capable of quantifying and resolving luteolin and apigenin and can be applicable for routine analysis of extract and plant as a whole
Multi-omic features of oesophageal adenocarcinoma in patients treated with preoperative neoadjuvant therapy
Full text linkOesophageal adenocarcinoma is a poor prognosis cancer and the molecular features underpinning response to treatment remain unclear. We investigate whole genome, transcriptomic and methylation data from 115 oesophageal adenocarcinoma patients mostly from the DOCTOR phase II clinical trial (Australian New Zealand Clinical Trials Registry-ACTRN12609000665235), with exploratory analysis pre-specified in the study protocol of the trial. We report genomic features associated with poorer overall survival, such as the APOBEC mutational and RS3-like rearrangement signatures. We also show that positron emission tomography non-responders have more sub-clonal genomic copy number alterations. Transcriptomic analysis categorises patients into four immune clusters correlated with survival. The immune suppressed cluster is associated with worse survival, enriched with myeloid-derived cells, and an epithelial-mesenchymal transition signature. The immune hot cluster is associated with better survival, enriched with lymphocytes, myeloid-derived cells, and an immune signature including CCL5, CD8A, and NKG7. The immune clusters highlight patients who may respond to immunotherapy and thus may guide future clinical trials.Marjan M. Naeini, Felicity Newell, LaurenG. Aoude, Vanessa F. Bonazzi, Kalpana Patel, Guy Lampe, Lambros T. Koufariotis, Vanessa Lakis, Venkateswar Addala, Olga Kondrashova, Rebecca L. Johnston, Sowmya Sharma, Sandra Brosda, Oliver Holmes, Conrad Leonard, Scott Wood, Qinying Xu, Janine Thomas, Euan Walpole, G. Tao Mai, Stephen P. Ackland, Jarad Martin, Matthew Burge, Robert Finch, Christos S. Karapetis, Jenny Shannon, Louise Nott, Robert Bohmer, Kate Wilson, Elizabeth Barnes, John R. Zalcberg, B. Mark Smithers, John Simes, Timothy Price, Val Gebski, Katia Nones, David I. Watson, John V. Pearson, Andrew P. Barbour, Nicola Waddel
The Effectiveness of Different Revision Approaches in Science on Achievement and Retention of Learners Having Different Learning Styles
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Assessment of nutritional status of gynecological cancer cases in India and comparison of subjective and objective nutrition assessment parameters
No full textAim: To assess the nutritional status of gynecological cancer patients using scored Patient Generated Subjective Global Assessment (PG-SGA) then compare it with the body mass index (BMI), hemoglobin, serum albumin, and approximate percentage weight lost in last 1 month so as to find any one parameter that can be used in place of the comprehensive assessment tool. Materials and Methods: Sixty gynecological cancer patients were assessed for their nutritional status using BMI, serum albumin, hemoglobin, percentage weight lost in last 1 month, and scored PG-SGA. Correlation, sensitivity, specificity, and predictive values of the former four parameters compared to scored PG-SGA were calculated. Results: 88.33% of cases were at risk of or had some degree of malnutrition according to scored PG-SGA. Serum albumin level ≤ 2 g/dl had highest specificity and positive predictive value at 1, whereas percentage weight lost in last month had better overall sensitivity, specificity, and positive and negative predictive values of 0.5833, 0.9444, 0.875, and 0.7727, respectively. The Pearson′s correlation coefficient between scored PG-SGA and percentage weight lost in last 1 month was 0.784, highest among all the parameters. Conclusion: 88.33% of gynecologic cancer cases had some degree of malnutrition or were at risk of malnutrition. Approximate percentage weight lost in last 1 month, that is, ≥ 5% may be used in place of the comprehensive scored PG-SGA to triage the patients in case the latter is not used for some reason. Severe hypoalbuminemia ≤ 2 g/dl is an indicator of severe malnutrition in gynecologic cancer cases
Organic biogeochemical study of deeper southeastern Bengal Basin sediments in West Bengal, India
No full textThe Bengal Basin is a fluvio-deltaic basin spanning Bangladesh and part of east and northeast India. The evolution of the peripheral foreland basin has been studied, but published literature on depositional conditions, source and maturity of organic matter in the deeper sediments of the Indian section of the basin is rare, despite the fact that natural gas is often encountered during hydrocarbon exploration. Our research assesses the depositional environment and source of the organic matter (OM) in the Pleistocene-Miocene sediments from five wells drilled by Oil and Natural Gas Corporation Limited in the southeastern Bengal Basin, West Bengal, India and aims to understand its maturity and potential to yield natural gas. The total organic carbon/nitrogen ratio and stable isotope (δ13C and δ15N) signature indicate primarily aquatic and C3 terrestrial plant sources of the OM and deposition under tidal flat and marshy environments. The n-alkane and isoprenoid alkane distribution are consistent with an autochthonous source of OM and terrestrial oxic-suboxic shallow-water depositional setting. The Rock-Eval parameters, such as maximal pyrolysis temperature, hydrogen and oxygen indices, indicate the immature nature of Type III and Type IV kerogen. The presence of methanogenic archaea, as indicated by phylogenetic analysis, in two Miocene sediment samples from one well indicates an active microbial activity in Type III immature OM, derived from C3 marsh vegetation and deposited under oxic shallow-water conditions. Our research describes the presence of methanogenic archaea for the first time in Miocene Bengal Basin sediments and is one of the few reports of their presence in deep (> 4000 m) horizons.Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public.Sanitary Engineerin
Validation and Experimental Design Assisted Robustness Testing of RPLC Method for the Simultaneous Analysis of Brinzolamide and Brimonidine Tartrate in an Ophthalmic Dosage Form
No full textHPLC and HPTLC methods for simultaneous quantification of Metformin hydrochloride, Vildagliptin and Dapagliflozin propanediol with comparative evaluation by greenness and whiteness assessment tools
No full textThe combination of Vildagliptin, Dapagliflozin propanediol monohydrate and Metformin hydrochloride has been approved by Central Drug Standard Control Organization in March 2023 for conducting Phase III trial for treatment of diabetes mellitus. None of the chromatographic methods are reported for the proposed combination. In context to this, the proposed work aims to develop and validate two chromatographic methods, high HPLC and HPTLC for simultaneous estimation of the said combination followed by validation in accordance to ICH Q2(R2). For HPLC, linearity range were, 300–700, 30–70 and 3–7 µg/ml for Metformin hydrochloride, Vildagliptin and Dapagliflozin propanediol respectively. Good resolution was obtained with the final mobile phase, Acetonitrile: 10 mM potassium dihydrogen phosphate buffer pH 6.5 set with TEA (75:25 %v/v). The flow rate was 1 ml/min and detection wavelength was 214 nm. Rt of Metformin hydrochloride, Vildagliptin and Dapagliflozin propanediol was 2.262, 3.956 and 11.411 min respectively. For HPTLC the linearity range set was 1000–5000, 5000–9000 and 1000–5000 ng/band for Metformin hydrochloride, Vildagliptin and Dapagliflozin propanediol respectively. Separation of all drugs was observed using optimized mobile phase, Toluene: Ethyl acetate: 3% Ammonium acetate: Triethylamine(4: 4: 3: 0.1). Rf for Metformin hydrochloride, Vildagliptin and Dapagliflozin propanediol was 0.19, 0.48 and 0.61 respectively at 214 nm. % Relative Standard Deviation for validation parameters of both methods were found to be <2, which indicates that the methods were validated properly as per guideline. The proposed methods were specific, reliable, precise and can be applicable in routine analysis. Analytical Eco-Scale, Analytical GREEnness metric, and complex Green Analytical Procedure Index were the three methods used to assess the greenness. Furthermore, the quality (R), ecological effect (G), and economic feasibility (B) of the new technique were assessed by RGBfast tool for whiteness assessment and the applicability evaluated by the BAGI metric tool for performance verification
Multivariate optimization for simultaneous determination of aspirin and simvastatin by reverse phase liquid chromatographic method using AQbD approach
No full textThe present study describes the development of a robust method for the separation of aspirin and simvastatin using reverse phase high performance liquid chromatographic method on Kintex reverse phase C18 column (5 μm, 250 mm Ã 4.6 mm) with UV detection at 234 nm. Box-Behnken design was applied for multivariate optimization of the experimental conditions of RP-HPLC for obtaining desired chromatographic resolution with limited number of experiments. Risk assessment was performed to identify the critical method parameters. Three independent parameters; volume of acetonitrile, molarity of buffer and flow rate were used to design mathematical models and study the in depth effects of these independent factors on various responses. The optimized and predicted condition consisted of acetonitrile and potassium dihydrogen orthophosphate buffer pH 2.9 adjusted with orthophosphoric acid (83.89:16.11, v/v) as mobile phase at a flow rate of 0.93 ml/min. Using these optimum conditions, baseline separation of both drugs with good resolution and a run time of less than 6 min was achieved. Perturbation plot revealed that the most important factor affecting the selected responses was volume of acetonitrile. Percent recoveries in terms of accuracy for both drugs at all three levels was found in the range of 99.15â101.86%. The pooled % relative standard deviation values for repeatability and intermediate precision studies was found to be less than 2% for both drugs. Hence, a robust, simple, accurate and reproducible high performance liquid chromatographic method was developed and validated and could be applied for routine quality control testing. Keywords: Aspirin, Simvastatin, Box-Behnken design, HPL
Optimization of HPTLC densitometric method for curcuminoids and polyphenolics in an ayurvedic Emblica officinalis and Curcuma longa based Nishamalaki formulation by Box-Behnken design
No full text719-728The present study focuses on developing a simplified, specific, and accurate high performance thin layer chromatographic (HPTLC) method for the quantitative and qualitative determination of ellagic acid, gallic acid, and curcuminoids (bisdemethoxycurcumin, demethoxycurcumin, and curcumin) in Nishamalaki Ayurvedic formulation. Pre-coated silica gel 60 F254 aluminum-backed plates were used as the stationary phase in the chromatographic technique development, and the optimized mobile phase was toluene: dichloromethane: glacial acetic acid: formic acid (6:4:1.6:0.9% v/v/v/v) with double development in linear ascending mode. The detection wavelength for quantification for ellagic and gallic acid was 280 nm, and curcuminoids (bisdemethoxycurcumin, demethoxycurcumin, and curcumin) were 430 nm. The optimized mobile phase showed optimum separation between peaks for ellagic acid, gallic acid, and curcuminoids (bisdemethoxycurcumin, demethoxycurcumin, and curcumin) at RF of 0.12±0.02, 0.21±0.02, 0.55±0.02, 0.69±0.02 and 0.82±0.02 respectively. Chromatographic conditions were optimized using the Box-Behnken design. Various variables, such as, the volume of formic acid and glacial acetic acid, and chamber saturation time, that are likely to impact RF were identified for further optimization. The volume of glacial acetic acid may be regarded as a critical method parameter, which caused the greatest change in the RF value and was the important factor among the three factors. The linear range was 600-1800 ng/band for all markers (r2 greater than 0.98). The limit of detection (LOD) and quantification (LOQ) measured indicated the method’s sensitivity. For all markers, the recovery percentage reveal acceptable accuracy, and the method was repeatable and reproducible from precision measurements with less than a 2% relative standard deviation. The optimized method was precise, specific, accurate, robust and reproducible for quantifying ellagic acid, gallic acid, and curcuminoids (bisdemethoxycurcumin, demethoxycurcumin, and curcumin) in the quality-control testing of botanical extract along with Nishamalaki ayurvedic formulation
Multivariate optimization for simultaneous determination of aspirin and simvastatin by reverse phase liquid chromatographic method using AQbD approach
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