DEVELOPMENT AND VALIDATION OF A HPTLC METHOD FOR SIMULTANEOUS DENSITOMETRIC ANALYSIS OF GLYCYRRHETIC ACID AND SOLASODINE IN HERBAL DRUG FORMULATION

Objective: To develop and validate a simple, precise, selective, and accurate high-performance thin layer chromatographic method for simultaneous densitometric analysis of glycyrrhetic acid and solasodine in the polyherbal formulation.Methods: The method was developed using HPTLC silica gel GF254precoated aluminium plate as the stationary phase and Chloroform: Methanol (9:1 v/v) as the mobile phase. Quantization of glycyrrhetic acid was achieved by determining the area under the curve at 267 nm using CAMAG TLC Scanner and CATS 3 software. Since the structure of solasodine lacks conjugated double bond, it does not give any fluorescence either in the absorbance mode or reflectance mode hence solasodine was derivatized using 0.5%anisaldehyde sulphuric acids which gave a bluish spot as seen on TLC plate. These spots were scanned at 546 nm wavelength using CAMAG TLC Scanner and CATS 3 software.Results: The retention factor for glycyrrhetic acid and solasodine were found to be 0.52±0.01, 0.40±0.01% w/w respectively. The developed HPTLC method was validated using parameters described in International Conference on Harmonization (ICH) guideline. The proposed method showed good linearity in the range of 400-2000 ng spot-1 for glycyrrhetic acid as well as for solasodine. The content of glycyrrhetic acid and solasodine in marketed polyherbal formulation were found to be 0.67%±0.8 and 0.10±0.35%w/w respectively.Conclusion: The developed method can be used as quality control tool for the routine analysis of glycyrrhetic acid and solasodine in polyherbal formulation

Automatable analytical workflow for characterization of fatty acids in animal-based matrix by GC×GC-TOFMS

peer reviewe

Acute electrocardiographic changes during smoking: An observational study

Objective To study the temporal relationship of smoking with electrophysiological changes. Design Prospective observational study. Setting Tertiary cardiac center. Participants Male smokers with atypical chest pain were screened with a treadmill exercise test (TMT). A total of 31 such patients aged 49.8±10.5 years, in whom TMT was either negative or mildly positive were included. Heart rate variability (HRV) parameters of smokers were compared to those of 15 healthy non-smoking participants. Interventions All patients underwent a 24 h Holter monitoring to assess ECG changes during smoking periods. Results Heart rate increased acutely during smoking. Mean heart rate increased from 83.8±13.7 bpm 10 min before smoking, to 90.5±16.4 bpm during smoking, (p <0.0001) and returned to baseline after 30 min. Smoking was also associated with increased ectopic beats (mean of 5.3/h prior to smoking to 9.8/h during smoking to 11.3/h during the hour after smoking; p <0.001). Three patients (9.7%) had significant ST–T changes after smoking. HRV index significantly decreased in smokers (15.2±5.3) as compared to non-smoking controls participants (19.4±3.6; p=0.02), but the other spectral HRV parameters were comparable. Conclusions Heart rate and ectopic beats increase acutely following smoking. Ischaemic ST–T changes were also detected during smoking. Spectral parameters of HRV analysis of smokers remained in normal limits, but more importantly geometrical parameter—HRV index—showed significant abnormality

Improving analytical and annotation robustness in small molecule metabolomics using GCxGC-HRTOFMS

editorial reviewedThis presentation focus on the enhanced annotation and detectability capacity provided by high resolution information contained in multidimensional chromatography data. The presentation will focus on the combination of untargeted screening of small metabolites and small lipids in human blood serum samples from different form of colorectal cancers

SIMULTANEOUS MULTIPLE SPME FIBERS SAMPLING TO MAXIMIZE THE SAMPLE POTENTIAL

editorial reviewe

Advanced characterization and extraction of complex bio-based matrices using GC×GC-TOFMS

peer reviewe

Multiple et extraction SPME et simultanée pour maximiser le potentiel d'un échantillon

peer reviewe

Fishery and reproductive biology of Sardinella longiceps Valenciennes, 1847 landed along Veraval coast of Gujarat

The present study on the biology of Sardinella longiceps was carried out at the Veraval coast of Gujarat. The observed length of species was in the range of 145 to 236 mm and weighing from 37.54 to 122.35 gm. The highest mean length of 206 ± 9 mm was observed in the month of December

Comprehensive Insight into Colorectal Cancer Metabolites and Lipids for Human Serum: A Proof-of-Concept Study.

peer reviewedColorectal cancer (CRC) ranks as the third most frequently diagnosed cancer and the second leading cause of cancer-related deaths. The current endoscopic-based or stool-based diagnostic techniques are either highly invasive or lack sufficient sensitivity. Thus, there is a need for less invasive and more sensitive screening approaches. We, therefore, conducted a study on 64 human serum samples representing three different groups (adenocarcinoma, adenoma, and control) using cutting-edge GC×GC-LR/HR-TOFMS (comprehensive two-dimensional gas chromatography coupled with low/high-resolution time-of-flight mass spectrometry). We analyzed samples with two different specifically tailored sample preparation approaches for lipidomics (fatty acids) (25 μL serum) and metabolomics (50 μL serum). In-depth chemometric screening with supervised and unsupervised approaches and metabolic pathway analysis were applied to both datasets. A lipidomics study revealed that specific PUFA (ω-3) molecules are inversely associated with increased odds of CRC, while some PUFA (ω-6) analytes show a positive correlation. The metabolomics approach revealed downregulation of amino acids (alanine, glutamate, methionine, threonine, tyrosine, and valine) and myo-inositol in CRC, while 3-hydroxybutyrate levels were increased. This unique study provides comprehensive insight into molecular-level changes associated with CRC and allows for a comparison of the efficiency of two different analytical approaches for CRC screening using same serum samples and single instrumentation