Detection of tobacco smoke deposition by hyperpolarized krypton-83 MRI

Despite the importance of the tobacco smoke particulate matter in the lungs to the etiology of pulmonary disease in cigarette smokers, little is currently known about the spatial distribution of particle deposition or the persistence of the resulting deposits in humans, and no satisfactory technique currently exists to directly observe tobacco smoke condensate in airways. In this proof-of-principle work, hyperpolarized (hp) 83Kr MRI and NMR spectroscopy are introduced as probes for tobacco smoke deposition in porous media. A reduction in the hp-83Kr longitudinal (T1) relaxation of up to 95% under near-ambient humidity, pressure and temperature conditions was observed when the krypton gas was brought into contact with surfaces that had been exposed to cigarette smoke. This smoke-induced acceleration of the 83Kr self-relaxation was observed for model glass surfaces that, in some experiments, were coated with bovine lung surfactant extract. However, a similar effect was not observed with hp-(129)Xe indicating that the 83Kr sensitivity to smoke deposition was not caused by paramagnetic species but rather by quadrupolar relaxation due to high adsorption affinity for the smoke deposits. The 83Kr T1 differences between smoke-treated and untreated surfaces were sufficient to produce a strong contrast in variable flip angle FLASH hp-83Kr MRI, suggesting that hp-83Kr may be a promising contrast agent for in vivo pulmonary MRI.     

Electron holography of biological samples

In this paper, we summarise the development of off-axis electron holography on biological samples starting in 1986 with the first results on ferritin from the group of Tonomura. In the middle of the 1990s strong interest was evoked, but then stagnation took place because the results obtained at that stage did not reach the contrast and the resolution achieved by conventional electron microscopy.

To date, there exist only a few (12) publications on electron holography of biological objects, thus this topic is quite small and concise. The reason for this could be that holography is mostly established in materials science by physicists. Therefore, applications for off-axis holography were powerfully pushed forward in the area of imaging, e.g. electric or magnetic micro- and nanofields. Unstained biological systems investigated by means of off-axis electron holography up to now are ferritin, tobacco mosaic virus, a bacterial flagellum, T5 bacteriophage virus, hexagonal packed intermediate layer of bacteria and the Semliki Forest virus. New results of the authors on collagen fibres and surface layer of bacteria, the so-called S-layer 2D crystal lattice are presented in this review. For the sake of completeness, we will shortly discuss in-line holography of biological samples and off-axis holography of materials related to biological systems, such as biomaterial composites or magnetotactic bacteria.     

Analysis of phenolic acids and flavonoids in leaves of Lycium barbarum from different habitats by ultra‐high‐performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry

The leaves of Lycium barbarum (LLB) have been utilized as crude drugs and functional tea for human health in China and Southeast Asia for thousands of years. To control its quality, a rapid and sensitive ultra‐high‐performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry method was established and validated for the first time for simultaneous determination of 10 phenolic acids and flavonoids (including neochlorogenic acid , protocatechuic aldehyde, p‐hydroxybenzoic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, p‐coumaric acid, ferulic acid, rutin and kaempferol‐3‐O‐rutinoside) in LLB. The separation was performed on an Acquity UPLC C₁₈ chromatographic column (100 × 2.1 mm internal diameter, 1.7 μm particle size) with 0.1% formic acid in water (A)–acetonitrile (B) as the mobile phase under gradient elution. Multiple reaction monitoring mode was adopted to simultaneously monitor the target components. The developed method was fully validated in terms of linearity (r² ≥ 0.9860), precision (RSD ≤ 6.58%), repeatability (RSD ≤ 6.60%), stability (RSD ≤ 6.17%), recovery (95.56–108.06%, RSD ≤ 4.64%) and limit of detection (0.021–0.664 ng/mL) and limit of quantitation (0.069–2.210 ng/mL), and then successfully applied to evaluate the quality of 64 batches of LLB collected from 41 producing areas in four different provinces of China. The results showed that the LLB, especially collected from Inner Mongolia regions, were rich in the phenolic acids and flavonoids. Rutin, kaempferol‐3‐O‐rutinoside and chlorogenic acid are the predominant compounds contained in LLB. The above findings will provide helpful information for the effective utilization of LLB.     

Preparation and Characterization of Bhant Leaves‐derived Nitrogen‐doped Carbon and its Use as an Electrocatalyst for Detecting Ketoconazole

In this study, the electrocatalytic characteristics of nitrogen‐doped carbon (NDC) prepared from Clerodendrum Infortunatum L leaves on a glassy carbon electrode (GCE) surface was evaluated with regards to its ability to detect the electroactive drug ketoconazole (KCZ). The NDC was prepared by carrying out a simple pyrolysis of dry powder of the leaves at 850 °C. The prepared NDC was characterized using field‐emission scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, X‐ray photoelectron spectroscopy and Brunauer‐Emmett‐Teller analysis, and was then used as an electrode material. The performance of the electrochemical KCZ sensor with the NDC‐modified glassy carbon electrode (NDC/GCE) was found to be optimal when using PBS buffer at pH 3 and a concentration of 0.1 mg/ml of NDC in the conjugate with Nafion polymer. Under these conditions, the NDC/GCE displayed a KCZ detection limit of 3 μM and a linear dependence of its response on KCZ concentration over a wide range of KCZ concentrations from 47 μM to 752 μM (R²=0.9742). These results confirmed the potential of NDC as an electrocatalyst.     

Quantitative solid phase microextraction – Gas chromatography mass spectrometry analysis of five megastigmatrienone isomers in aged wine

Megastigmatrienone is a key flavor compound in tobacco. It has also been detected in wine, where it may contribute to a tobacco/incense aroma, but its importance and concentration in wines had never previously been evaluated.     

A green protocol for efficient discovery of novel natural compounds: Characterization of new ginsenosides from the stems and leaves of Panax ginseng as a case study

Exploration of new natural compounds is of vital significance for drug discovery and development. The conventional approaches by systematic phytochemical isolation are low-efficiency and consume masses of organic solvent. This study presents an integrated strategy that combines offline comprehensive two-dimensional liquid chromatography, hybrid linear ion-trap/Orbitrap mass spectrometry, and NMR analysis (2D LC/LTQ-Orbitrap-MS/NMR), aimed to establish a green protocol for the efficient discovery of new natural molecules. A comprehensive chemical analysis of the total ginsenosides of stems and leaves of Panax ginseng (SLP), a cardiovascular disease medicine, was performed following this strategy. An offline 2D LC system was constructed with an orthogonality of 0.79 and a practical peak capacity of 11,000. The much greener UHPLC separation and LTQ-Orbitrap-MS detection by data-dependent high-energy C-trap dissociation (HCD)/dynamic exclusion were employed for separation and characterization of ginsenosides from thirteen fractionated SLP samples. Consequently, a total of 646 ginsenosides were characterized, and 427 have not been isolated from the genus of Panax L. The ginsenosides identified from SLP exhibited distinct sapogenin diversity and molecular isomerism. NMR analysis was finally employed to verify and offer complementary structural information to MS-oriented characterization. The established 2D LC/LTQ-Orbitrap-MS/NMR approach outperforms the conventional approaches in respect of significantly improved efficiency, much less use of drug materials and organic solvent. The integrated strategy enables a deep investigation on the therapeutic basis of an herbal medicine, and facilitates new compounds discovery in an efficient and environmentally friendly manner as well.     

Olive-Derived Triterpenes Suppress SARS COV-2 Main Protease: A Promising Scaffold for Future Therapeutics

SARS CoV-2 pandemic is still considered a global health disaster, and newly emerged variants keep growing. A number of promising vaccines have been recently developed as a protective measure; however, cost-effective treatments are also of great importance to support this critical situation. Previously, betulinic acid has shown promising antiviral activity against SARS CoV via targeting its main protease. Herein, we investigated the inhibitory potential of this compound together with three other triterpene congeners (i.e., ursolic acid, maslinic acid, and betulin) derived from olive leaves against the viral main protease (M^pro) of the currently widespread SARS CoV-2. Interestingly, betulinic, ursolic, and maslinic acids showed significant inhibitory activity (IC₅₀ = 3.22–14.55 µM), while betulin was far less active (IC₅₀ = 89.67 µM). A comprehensive in-silico analysis (i.e., ensemble docking, molecular dynamic simulation, and binding-free energy calculation) was then performed to describe the binding mode of these compounds with the enzyme catalytic active site and determine the main essential structural features required for their inhibitory activity. Results presented in this communication indicated that this class of compounds could be considered as a promising lead scaffold for developing cost-effective anti-SARS CoV-2 therapeutics.     

Phytochemical analysis of non-polar solvent extracts of the Wisteria sinensis leaves

A comparative study on the phytochemical composition of the n-hexane and chloroform extracts from Wisteria sinensis leaves collected in June and October is described. Continuous extraction in Soxhlet apparatus, as well as ultrasound-assisted technique, was used for the preparation of the extracts. All the extracts were analysed by GC/MS method. As a result, α-tocopherol was identified as the main component (56%) of the extracts from October leaves, whereas, β-sitosterol was identified as the main compound (47%) in the extracts from the June leaves. Additionally, pure α-tocopherol was isolated from n-hexane extract of the October leaves using column chromatography. A total of 6.25 mg of α-tocopherol was isolated from 1 g of dried leaves. The presence of the vitamin E in extracts from W. sinensis leaves is described here for the first time.     

Sequential preconcentration by coupling of field amplified sample injection with pseudo isotachophoresis–acid stacking for analysis of alkaloids in capillary electrophoresis

A novel on-column sequential preconcentration method based on the combination of field-amplified sample injection induced by acetonitrile and pseudo isotachophoresis (ITP)–acid stacking is developed for simply but efficiently concentrating alkaloid cations in a high-salt sample matrix in capillary electrophoresis. Acetonitrile (70%) added to a sample solution with a high-salt sample matrix not only induces field-amplified sample stacking by decreasing conductivity but also acts as a termination reagent in the succeeding pseudo ITP. After sample injection had been completed, a plug of H⁺ was injected electrokinetically and a neutralization reaction between H⁺ and tartrate from the buffer solution produced a low conductivity zone, in which the injected analyte cations were further concentrated. With the sequential preconcentration method, a 3 orders of magnitude detection sensitivity (1,400-fold) increase could be observed compared with the conventional electrokinetic injection method, without compromising separation efficiency and peak shape, and detection limits of 0.1 ng/mL for myosmine and 0.3 ng/mL for anabasine with the conditions selected were achieved. The calibration curves demonstrated good linearity in the concentration ranges 1.3–600 ng/mL for myosmine and 4.9–900 ng/mL for anabasine, respectively. The proposed method has been used to analyze successfully trace alkaloids in cigarette samples. Figure Sequential preconcentration processes: a sample injection; b introduction of HCl; c capillary zone electrophoresis separation. A ⁻ tartrate, white circles acetonitrile, black circles Na⁺, sample zone, myosmine, anabasine