Determination of gymnemagenin in rat plasma using high‐performance liquid chromatography–tandem mass spectrometry: application to pharmacokinetics after oral administration of Gymnema sylvestre extract

A sensitive and rapid high‐performance liquid chromatography–tandem mass spectrometry (HPLC‐MS/MS) method has been developed and validated for the determination of gymnemagenin (GMG), a triterpene sapogenin from Gymnema sylvestre, in rat plasma using withaferin A as the internal standard (IS). Plasma samples were simply extracted using liquid–liquid extraction with tetra‐butyl methyl ether. Chromatographic separation was performed on Luna C₁₈ column using gradient elution of water and methanol (with 0.1% formic acid and 0.3% ammonia) at a flow rate of 0.8 mL/min. GMG and IS were eluted at 4.64 and 4.36 min, ionized in negative and positive mode, respectively, and quantitatively estimated using multiple reaction monitoring (MRM) mode. Two MRM transitions were selected at m/z 505.70 → 455.5 and m/z 471.50 → 281.3 for GMG and IS, respectively. The assay was linear over the concentration range of 5.280–300.920 ng/mL. The mean plasma extraction recoveries for GMG and IS were found to be 80.92 ± 8.70 and 55.63 ± 0.76%, respectively. The method was successfully applied for the determination of pharmacokinetic parameters of GMG after oral administration of G. sylvestre extract. Copyright © 2012 John Wiley & Sons, Ltd.     

Study on the subgel-phase formation using an asymmetric phospholipid bilayer membrane by high-pressure fluorometry

The myristoylpalmitoylphosphatidylcholine (MPPC) bilayer membrane shows a complicated temperature-pressure phase diagram. The large portion of the lamellar gel (L(β)'), ripple gel (P(β)'), and pressure-induced gel (L(β)I) phases exist as metastable phases due to the extremely stable subgel (L(c)) phase. The stable L(c) phase enables us to examine the properties of the L(c) phase. The phases of the MPPC bilayers under atmospheric and high pressures were studied by small-angle neutron scattering (SANS) and fluorescence spectroscopy using a polarity-sensitive fluorescent probe Prodan. The SANS measurements clearly demonstrated the existence of the metastable L(β)I phase with the smallest lamellar repeat distance. From a second-derivative analysis of the fluorescence data, the line shape for the L(c) phase under high pressure was characterized by a broad peak with a minimum of ca. 460 nm. The line shapes and the minimum intensity wavelength (λ″(min)) values changed with pressure, indicating that the L(c) phase has highly pressure-sensible structure. The λ″(min) values of the L(c) phase spectra were split into ca. 430 and 500 nm in the L(β)I phase region, which corresponds to the formation of a interdigitated subgel L(c) (L(c)I) phase. Moreover, the phase transitions related to the L(c) phase were reversible transitions under high pressure. Taking into account the fluorescence behavior of Prodan for the L(c) phase, we concluded that the structure of the L(c) phase is highly probably a staggered structure, which can transform into the L(c)I phase easily.     

Growth,structural, optical and mechanical studies on acid mixed glycine metal salt (GABN) crystal as potential NLO material

Transparent crystals of α-glycine with ammonium nitrate and barium nitrate (GABN) have been grown from aqueous solution by slow evaporation technique at room temperature. Crystals of size 11 × 7 × 4 mm³ have been obtained in about 3–4 weeks time. The solubility of GABN has been determined in water. The grown crystal belongs to orthorhombic system with cell parameters a = 7.317 A.U, b = 12.154 A.U and c = 5.468 A.U with a unit cell volume 486.35 (A.U)³. The presence of chemical components/groups has been identified by CHN, EDAX and NMR analysis. Comparative IR and Raman studies indicate a molecule with a lack of centre of symmetry. A wide transparency window useful for optoelectronic applications is indicated by the UV Studies. Using a Nd-YAG laser (1064 nm), the optical second harmonic generation (SHG) conversion efficiency of GABN is found to be 1.406 times of that of standard KDP. On exposure to light the GABN crystals are found to exhibit negative photoconductivity. I–V characteristics, SEM studies, dielectrics studies, and Vickers micro hardness measurement have been carried out.     

Can low-power electromagnetic radiation disrupt hydrogen bonds in dsDNA?

Microwave radiation resonant with the natural phonon frequencies of double-stranded DNA (dsDNA) is shown to couple strongly to the breather modes of dsDNA under certain conditions. The excitation of the disruptive breather modes is controlled to a great extent by energy dissipation to its aqueous environment. For sufficiently high power—much higher than expected under ambient conditions—the breather solutions become unstable. Our analysis discounts the disruptive effect of low frequency, low power radiation on dsDNA. The authors hope to stimulate experiments via their analysis. The resulting data will dictate the future evolution of their models. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 2740–2747, 2006     

Synthesis of 2-Tert-butylimino-3-hepta-O-benzoyl-β-D-lactosylimino-4-S-benzyl-6-arylimino-2,3-dihydro-1,3,5-thiadiazines

A new series of synthesis of 2-tert-butylimino-3-hepta-O-benzoyl-β-D-lactosylimino-4-S-benzyl-6-arylimino-2,3-dihydro-1,3,5-thiadiazines (hydrochloride) were synthesized by the interaction of 1-aryl-5-hepta-O-benzoyl-β-D-lactosyl-2-S-benzyl-2,4-isodithiobiurets with tert-butyl isocyanodichloride. The identities of these newly synthesized N-lactosides have been established on the basis of usual chemical transformations and infrared, ¹H NMR, and mass spectral analysis.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource(s): Full experimental and spectral details.]     

Structural, optical and electrical studies on amino acid based new GBC crystals having non linear optical response

Transparent crystals of α-glycine with barium nitrate and calcium nitrate (GBC) have been grown from aqueous solution by slow evaporation technique at room temperature. Crystals of size 22 × 25 × 4 mm³ have been obtained in 3-4 weeks time. The solubility of GBC has been determined in water. The grown crystal belongs to orthorhombic system with cell parameters a = 12.7321 A.U, b = 13.7752 A.U and c = 8.6002 A.U with unit cell volume of 1508.36 (A.U)³. Comparative IR and Raman studies indicate a molecule with a lack of center of symmetry. A wide transparency window useful for optoelectronic applications is indicated by the UV Studies. Using Nd:YAG laser (1064 nm), the optical second harmonic generation (SHG) conversion efficiency of GBC is found to be 0.702 times than that of standard KDP. On exposure to light the GBC crystals exhibit positive photoconductivity. I-V characteristics, dielectrics studies, electrical and Vickers micro hardness measurement have been carried out. The GBC crystal exhibits more mechanical strength compared to the reported GSN crystals.     

A smart coating established with encapsulation of Zinc Molybdate centred nanocontainer for active corrosion protection of mild steel: release kinetics of corrosion inhibitor

In the current work smart coating of corrosion inhibitive nanocontainer was developed based on the encapsulation of ultrasonically synthesized Zinc Molybdate (ZM) nanoparticles. The ZM nanoparticles were doped ultrasonically with the layers of Myristic acid (MA), Polyaniline layer (PANI), benzotriazole layer and polyacrylic acid layer respectively to prepare layer by layer assembled nanocontainer. Results of XRD, PSD, FTIR, zeta potential and TEM analysis proves the successful formation of the layered structure of ZM nanocontainer particles. The release rate of benzotriazole at various experimental pH values was estimated using UV–vis spectroscopy. Different semi-empirical models were examined to predict the release mechanism of the benzotriazole. The corrosion inhibitive performance of ZM nanocontainers has been evaluated by incorporating 1wt % ZM nanocontainer in the epoxy based coating formulations and assessing by DC polarization measurement and Bode plots. The results from corrosion potential and Bode plots suggest the successful use of ZM nanocontainer in the multifunctional anticorrosion coating formulations.     

Effect of Native Reservoir State and Oilfield Operations on Clay Mineral Surface Chemistry

An understanding of clay mineral surface chemistry is becoming critical as deeper levels of control of reservoir rock wettability via fluid–solid interactions are sought. Reservoir rock is composed of many minerals that contact the crude oil and control the wetting state of the rock. Clay minerals are one of the minerals present in reservoir rock, with a high surface area and cation exchange capacity. This is a first-of-its-kind study that presents zeta potential measurements and insights into the surface charge development process of clay minerals (chlorite, illite, kaolinite, and montmorillonite) in a native reservoir environment. Presented in this study as well is the effect of fluid salinity, composition, and oilfield operations on clay mineral surface charge development. Experimental results show that the surface charge of clay minerals is controlled by electrostatic and electrophilic interactions as well as the electrical double layer. Results from this study showed that clay minerals are negatively charged in formation brines as well as in deionized water, except in the case of chlorite, which is positively charged in formation water. In addition, a negative surface charge results from oilfield operations, except for operations at a high alkaline pH range of 10–13. Furthermore, a reduction in the concentrations of Na, Mg, Ca, and bicarbonate ions does not reverse the surface charge of the clay minerals; however, an increase in sulfate ion concentration does. Established in this study as well, is a good correlation between the zeta potential value of the clay minerals and contact angle, as an increase in fluid salinity results in a reduction of the negative charge magnitude and an increase in contact angle from 63 to 102 degree in the case of chlorite. Lastly, findings from this study provide vital information that would enhance the understanding of the role of clay minerals in the improvement of oil recovery.     

A Modified Contact Angle Measurement Process to Suppress Oil Drop Spreading and Improve Precision

Static contact angle measurement is a widely applied method for wettability assessment. Despite its convenience, it suffers from errors induced by contact angle hysteresis, material heterogeneity, and other factors. This paper discusses the oil drop spreading phenomenon that was frequently observed during contact angle measurements. Experimental tests showed that this phenomenon is closely related to surfactants in the surrounding phase, the remaining oil on the rock surface, and oil inside the surrounding phase. A modified contact angle measurement process was proposed. In the modified method, deionized water was used as the surrounding phase, and a rock surface cleaning step was added. Subsequent measurements showed a very low chance of oil drop spreading and improved precision. A further comparison study showed that, when the surrounding phase was deionized water, the measured contact angle values tended to be closer to intermediate-wet conditions compared to the values measured in clean surfactant solutions. This difference became more significant when the surface was strongly water-wet or strongly oil-wet. As a result, the developed process has two prerequisites: that the in-situ contact angle values inside surfactant solutions are not required, and that the wettability alteration induced by the surfactant solution is irreversible.     

Physico-Chemical and Antimicrobial Efficacy of Encapsulated Dhavana Oil: Evaluation of Release and Stability Profile from Base Matrices

Essential oils (EOs) are naturally occurring volatile aromatic compounds extracted from different parts of plants. They are made up of components like terpenes, phenols, etc., and are chemically unstable and susceptible to oxidative deterioration, leading to reduced shelf-life and overall degradation of the product. Encapsulation of EOs in a matrix can prevent degradation of the active ingredient and improve the shelf-life. In this paper, we report encapsulation of Dhavana oil (Artemisia pellen) in a modified starch matrix using a spray-drying technique. Physico-chemical properties of neat and encapsulated Dhavana oil were studied. We selected two powder bases: CaCO₃ and TALC and, loaded neat and encapsulated Dhavana oil in it, studied their stability and interaction with the base matrices at 3 °C, 22 °C and 45 °C up to 2 months under closed conditions and one week at 22 °C and 45 °C under open condition. Thermal degradation pattern was studied for neat and encapsulated Dhavana oil and modified starch. Release of primary active component of neat and encapsulated Dhavana oil from the base matrices was evaluated with GCMS. Stability study and release mechanism were elucidated to understand the release pattern in different base powders under similar conditions. Retention of hydroxydhavanone was found to be better in TALC than CaCO₃, and therefore, the former can be considered a suitable base matrix for developing a stable powder formulation with an optimum release of the oil. Dhavana oil is known for its anti-microbial activity, and hence, neat and encapsulated Dhavana oil was tested on different bacterial and fungal strains. The encapsulated oil depicted good anti-microbial efficacy against various bacterial and fungal strains, which is a step forward for developing anti-microbial formulations. Thus, the reported work will provide helpful information on cosmetic formulation and, therefore, be useful for perfumery, food, and cosmetic industries.