Bio-analytical method validation and its importance in pharma research - A review article

Bioanalytical method based on a variety of physico-chemical and biological techniques such as chromatography, immunoassay and mass spectrometry, must be validated prior to and during use to give confidence in the results generated. It is the process used to establish that a quantitative analytical method is suitable for biomedical applications. Bioanalytical method validation includes all of the procedures that demonstrate that a particular method used for quantitative measurement of analytes in a given biological matrix, such as blood, plasma, serum, or urine is reliable and reproducible for the intended use. The present manuscript focuses on the consistent evaluation of the key bioanalytical validation parameters is discussed: accuracy, precision, sensitivity, selectivity, standard curve, limits of quantification, range, recovery and stability. These validation parameters are described, together with an example of validation methodology applied in the case of chromatographic methods used in bioanalysis, taking in account to the recent Food and Drug Administration (FDA) guidelines and EMA guid

To assess awareness regarding rational drug therapy and fixed dose combinations amongst interns and II MBBS students in tertiary care teaching hospital in Maharashtra, India

Background: The present study was designed to assess awareness regarding rational drug therapy and fixed dose combinations (FDC) amongst interns and II MBBS students in a tertiary-care teaching hospital in Maharashtra, India.Methods: This cross-sectional, questionnaire-based study containing MCQ and analytical questions on rational drug therapy, fixed dose combinations and role of Pharmacist in dispensing correct drug to the patients was carried out in both interns (n=80) and II MBBS students (n=100). The completed questionnaires were then collected and analysed statistically for responses.Results: Mean average score obtained by II MBBS students (score - 36.66marks) was significantly better than interns (score- 20marks) which probably may be due to pharmacology teaching they were undergoing. II MBBS students were found to be better informed as compared to the interns (p0.05). However, on question related to justification of FDC, interns were found to be better informed as compared to the II MBBS students (p<0.05). On single question pertaining to role of pharmacist, interns were found to be better informed than II MBBS students possibly due to their better understanding of patient-pharmacist relationship.Conclusions: Our study highlights the significance regarding knowledge of rational drug therapy and fixed dose combination (both rational and irrational), both rational and irrational, amongst both interns and II MBBS students while identifying the possible areas of interventions to make them rational clinicians

Sustainable synthesis and precise characterisation of bio-based star polycaprolactone synthesised with a metal catalyst and with lipase

Bio-based building blocks and sustainable synthesis pathways were used to synthesise star-shaped polymers composed of a D-sorbitol core and polycaprolactone arms by ring opening polymerisation (ROP). The use of volatile organic solvents was avoided and less energy intense reaction conditions were achieved by performing the ROP in the bulk or in a green solvent, supercritical CO2 (scCO2). Two catalysts were tested: conventional tin(II) 2-ethylhexanoate (Sn(Oct)2) which is a Food and Drug Administration (FDA) approved metal catalyst and an enzyme, Novozym 435 (Lipase B from Candida Antarctica immobilised on a solid support). The influence of the reaction medium and of the nature of the catalyst on the molecular weight, the dispersity and the architecture of the PCL stars was investigated. The star polymers were characterised by 1H and 31P nuclear magnetic resonance (1H and 31P NMR) spectroscopy, size exclusion chromatography – multi-angle light scattering (SEC-MALS) and matrix-assisted laser desorption and ionisation-time of flight (MALDI-TOF) mass spectrometry. The use of scCO2 enabled the reduction of the reaction temperature of Sn(Oct)2 catalysed star D-sorbitol-polycaprolactone polymerisations from 140 to 95 °C. In addition, star polymers were successfully synthesised by enzyme catalysis in the bulk or in scCO2 at 60 °C; lower temperatures that could provide significant energy savings on a commercial scale. Thecatalyst was shown to have a pronounced influence on the architecture of the PCL stars. Regular star polymers were obtained in the presence of Sn(Oct)2 whereas Novozym 435 gave access to miktoarmtype star PCL. Finally, the influence of the number and length of the arms on the thermal properties of the star polymers was investigated by differential scanning calorimetry (DSC)

Use of CR-39 films for nuclear radiation shielding efficacy evaluation of lining materials for combat vehicles

All materials provide, to a lesser or greater extent, shielding against nuclear radiations. Armoured fighting vehicles (AFVs) have steel as the structural material, which appears to be a reasonably good gamma and neutron shield material but a shield of pure iron would not be equally effective against whole range of neutron energies as it has a few resonances in electron volt range, and it reduces energy of fast neutrons to lower energy neutrons. These neutrons will be absorbed through radiative capture and emit gamma radiations. Thus it is essential that an effective shield should contain a large amount of moderating material, hydrogen being preferred with low atomic number materials (B, C, Li) and lead (Pb) to ensure that the neutrons do not diffuse at intermediate energies in the shield as well as gamma attenuation will also take place. In order to have a suitable shield material for armoured vehicles which serves as neutron and gamma radiation attenuator, polyethylene polymer with fillers lining materials are preferred. These materials were evaluated against gamma and fast neutrons using radioactive sources for suitability to fitment into combat vehicle as per the requirement of protection factor values. The detector for gamma radiation was used as Nal(Tl) while for neutron, CR-39 film was used.Use of CR-39 films for nuclear radiation shielding efficacy evaluation of lining materials for combat vehicles Deepak Gopalani1*, A S Jodha1, M K Das1, R K Singh2 and G L Baheti1 1Defence Laboratory, Jodhpur-342 011, Rajasthan, India 2Defence Material & Store Research & Developement Establishment, Kanpur-208 013, Uttar Pradesh, India E-mail : [email protected] Laboratory, Jodhpur-342 011, Rajasthan, India 2Defence Material & Store Research & Developement Establishment, Kanpur-208 013, Uttar Pradesh, Indi

Efficiency of Energy Conversion in Thermoelectric Nanojunctions

Using first-principles approaches, this study investigated the efficiency of energy conversion in nanojunctions, described by the thermoelectric figure of merit $ZT$. We obtained the qualitative and quantitative descriptions for the dependence of $ZT$ on temperatures and lengths. A characteristic temperature: $T_{0}= \sqrt{\beta/\gamma(l)}$ was observed. When $T\ll T_{0}$, $ZT\propto T^{2}$. When $T\gg T_{0}$, $ZT$ tends to a saturation value. The dependence of $ZT$ on the wire length for the metallic atomic chains is opposite to that for the insulating molecules: for aluminum atomic (conducting) wires, the saturation value of $ZT$ increases as the length increases; while for alkanethiol (insulating) chains, the saturation value of $ZT$ decreases as the length increases. $ZT$ can also be enhanced by choosing low-elasticity bridging materials or creating poor thermal contacts in nanojunctions. The results of this study may be of interest to research attempting to increase the efficiency of energy conversion in nano thermoelectric devices.Comment: 2 figure

Formulation and evaluation of a face serum containing fenugreek extract

Background: Wrinkles on the face and aging of the skin are an undesirable effect of photodamage and ultraviolet radiation. Serum has a quick absorption and ability to penetrate deep layers of the skin, as well as a non-oily finish and a deep formula with a very high amount of active ingredients. Methods: In this study, we have formulated and evaluated a face serum containing combination of aqueous extract of fenugreek seed and lemon oil. Results: Facial serum was tested for its pH, physical appearance, viscosity, microbial testing, cyclic temperature test, etc. The results of the stability study show that there was no change in visual acuity, homogeneity. Conclusions: Serum containing Fenugreek extract have been able to cure bacterial infections and inflammations of facial skin, and other signs also moistens the skin without any side effects making skin soft, smooth and supple

Effect of Thermoelectric Cooling in Nanoscale Junctions

We propose a thermoelectric cooling device based on an atomic-sized junction. Using first-principles approaches, we investigate the working conditions and the coefficient of performance (COP) of an atomic-scale electronic refrigerator where the effects of phonon's thermal current and local heating are included. It is observed that the functioning of the thermoelectric nano-refrigerator is restricted to a narrow range of driving voltages. Compared with the bulk thermoelectric system with the overwhelmingly irreversible Joule heating, the 4-Al atomic refrigerator has a higher efficiency than a bulk thermoelectric refrigerator with the same $ZT$ due to suppressed local heating via the quasi-ballistic electron transport and small driving voltages. Quantum nature due to the size minimization offered by atomic-level control of properties facilitates electron cooling beyond the expectation of the conventional thermoelectric device theory.Comment: 8 figure

Clean synthesis of linear and star amphiphilic poly(ε-caprolactone)-block-poly(ethyl ethylene phosphonate) block copolymers: assessing self-assembly and surface activity

International audienc

Molecular design and control of fullerene-based bi-thermoelectric materials

Molecular junctions are a versatile test bed for investigating nanoscale thermoelectricity and contribute to the design of new cost-effective environmentally friendly organic thermoelectric materials. It was suggested that transport resonances associated with discrete molecular levels could play a key role in thermoelectric performance, but no direct experimental evidence has been reported. Here we study single-molecule junctions of the endohedral fullerene Sc3N@C8 connected to gold electrodes using a scanning tunnelling microscope. We find that the magnitude and sign of the thermopower depend strongly on the orientation of the molecule and on applied pressure. Our calculations show that Sc3N inside the fullerene cage creates a sharp resonance near the Fermi level, whose energetic location, and hence the thermopower, can be tuned by applying pressure. These results reveal that Sc3N@C80 is a bi-thermoelectric material, exhibiting both positive and negative thermopower, and provide an unambiguous demonstration of the importance of transport resonances in molecular junctions