Study on the mechanism of biochar loaded typical microalgae Chlorella removal of cadmium.

Coconut shell activated carbon (Csac) is one of the most widely used materials to remove cadmium (Cd) from contaminated water. A large diversity of microorganisms exists in various aquatic systems and may aid Cd removal by Csac. In this study, we explored the reactions of Csac with microalgae (Chlorella) in Cd-containing media. The results of scanning electron microscope (SEM) imaging, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), superconducting pulse-Fourier transform nuclear magnetic resonance (pulse-FT NMR) and X-ray photoelectron spectroscopy (XPS) indicated that Chlorella could adhere in the micropores of Csac formed Csac@Chlorella composite adsorbent loading Chlorella. Furthermore, the composite adsorbent surface had abundant functional groups such -COOH, -OH and C-O-C, which served as active sites during the adsorption process. Compared with Csac, Csac@Chlorella had an enhanced Cd adsorption capacity evidently. The results showed that pH 8, 0.2 g Csac, OD680 of 0.1 for Chlorella were optimal conditions for maximum Cd adsorption capacity within one hour contact time. Furthermore, the Cd adsorption process was well described by the pseudo-second-order and Langmuir adsorption isotherm models. The models revealed that the adsorption process was mainly based on chemical adsorption of a single molecular layer, accompanied by electrostatic attraction, complexation and intracellular adsorption, amongst other parameters. Collectively, the findings illustrate that the microalgae (Chlorella)-Csac-Cd interaction is complex and will thus have immense interest to a broad range of biological, environmental, and geoscience communities.

Chemical constituents of Kopsia officinalis and their antagonizing high glucose-evoked podocyte injury activity.

Four new indole alkaloids (1-4) and twenty known compounds (5-24) were isolated from the leaves and stems, and fruits of Kopsia officinalis. Their structures were confirmed by means of spectroscopic methods. All these isolates were evaluated for their antagonizing high glucose-evoked podocyte injury activity for the first time, and compounds 5-8 showed potent activity with EC50 values of 3.0-12.0 µM.

Application of magnetic N-doped carbon nanotubes in solid-phase extraction of trace bisphenols from fruit juices.

Magnetic N-doped carbon nanotubes were firstly applied as adsorbent in food analysis for pre-concentration of bisphenols in fruit juices followed by ultra-high performance liquid chromatography-tandem mass spectrometry determination. The magnetic nanoparticles were characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy and vibrating sample magnetometer. The adsorption conditions were further optimized by response surface methodology. Under optimal conditions, the method provided good linearity with correlation coefficient (r ≥ 0.9979), excellent intermediate precisions (2.71-5.91%, n = 3), low limits of detection (LODs) ranging from 0.43 to 2.47 ng L-1, and satisfying recoveries of three juice samples (between 90.6% and 101%).

An Efficient Method for the Preparative Isolation and Purification of Flavonoids from Leaves of Crataegus pinnatifida by HSCCC and Pre-HPLC.

In this work, flavonoid fraction from the leaves of Crataegus pinnatifida was separated into its seven main constituents using a combination of HSCCC coupled with pre-HPLC. In the first step, the total flavonoid extract was subjected to HSCCC with a two-solvent system of chloroform/methanol/water/n-butanol (4:3:2:1.5, v/v), yielding four pure compounds, namely (-)-epicatechin (1), quercetin-3-O-(2,6-di-α-l-rhamnopyranosyl)-ß-d-galactopyranoside (2), 4''-O-glucosylvitexin (3) and 2''-O-rhamnosylvitexin (4) as well as a mixture of three further flavonoids. An extrusion mode was used to rapidly separate quercetin-3-O-(2,6-di-α-l-rhamnopyranosyl)-ß-d-galactopyranoside with a big KD-value. In the second step, the mixture that resulted from HSCCC was separated by pre-HPLC, resulting in three pure compounds including: vitexin (5), hyperoside (6) and isoquercitrin (7). The purities of the isolated compounds were established to be over 98%, as determined by HPLC. The structures of these seven flavonoids were elucidated by ESI-MS and NMR spectroscopic analyses.

Three novel indole alkaloids from Kopsia officinalis.

Three new indole alkaloids, named kopsioffines A-C (1-3), possessing relatively novel ten-membered lactam ring, and one known compound (11,12-demethoxy-16-deoxypauciflorine, 4) were isolated from the leaves and stems of Kopsia officinalis. Their structures were elucidated by means of spectroscopic methods. The absolute configuration of 1 was determined by calculated electronic circular dichroism data. The hypothetical biosynthetic pathway of 1 was postulated. All these isolates were evaluated for their inhibitory effects on α-glucosidase. None of them showed activity with IC50 far beyond 50µM.

Magnetic metal-organic framework-titanium dioxide nanocomposite as adsorbent in the magnetic solid-phase extraction of fungicides from environmental water samples.

In this work, a core-shell Fe3O4@SiO2@MOF/TiO2 nanocomposite was synthesized and used to as adsorbent for magnetic solid-phase extraction (MSPE) of triazole fungicides from environmental water samples. Five triazole fungicides, namely, triadimenol, hexaconazole, diniconazole, myclobutanil, and tebuconazole, were selected as target analytes for MSPE. These analytes were quantitatively adsorbed on microspheres, and the sorbents were separated from the solution by using a magnet. The analytes were desorbed by methanol and determined through liquid-chromatography coupled with tandem mass spectrometry. The extraction parameters affecting the extraction efficiency were optimized through response surface methodology. The limits of detection and limits of quantification for the selected fungicides were 0.19-1.20ngL(-1) and 0.61-3.62ngL(-1), respectively. The proposed method was applied to determine the concentration of fungicides in actual environmental water samples. The accuracy of the proposed method was evaluated by measuring the recovery of the spiked samples. The satisfying recoveries of the four water samples ranged from 90.2% to 104.2%. Therefore, the magnetic metal-organic framework/TiO2 nanocomposite based MSPE is a potential approach to analyze fungicides in actual water samples.

Melaxillines A and B, monoterpenoid indole alkaloids from Melodinus axillaris.

Two new monoterpenoid indole alkaloids, melaxillines A (1) and B (2), together with four known alkaloids (3-6), were isolated from the roots of Melodinus axillaris. The structures were determined by extensive spectroscopic methods, including 1D and 2D-NMR spectroscopy, high resolution mass spectrometric data, and by comparison to literature data. New compounds 1-2 might be derived from a common precursor (3) by proposing their biogenetic route, and compound 1 represents the first Melodinus alkaloid featuring an ethyl acetate group skeleton at C-18. The anti-inflammatory effects of all the isolated compounds were evaluated by measuring the inhibitory ratios of ß-glucuronidase release in rat polymorphonuclear leukocytes (PMNs) induced by platelet-activating factor. Compounds 1-4 showed significant anti-inflammatory activities with IC50 values ranging from 1.51 to 21.56µM, respectively.

Correlation analysis of urine metabolites and clinical staging in patients with ovarian cancer.

This study is to investigate the correlation between urine metabolites and clinical staging in patients with ovarian cancer. The urina sanguinis from 56 cases of primary epithelial ovarian cancer patients and 15 healthy volunteers was collected and the urine metabolites were extracted. Ultra high performance liquid chromatography/time-of-flight mass spectrometry (UPLC-Q-TOF-MS) analysis was performed. Principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) were used to analyze the mass spectrometry data. Database retrieval and comparison of the screened metabolites were performed and one-way ANOVA and least significant difference (LSD) t test were carried out. PCA analysis of UPLC-Q-TOF-MS results showed that the score plots of samples from healthy people and patients with ovarian cancer at different clinical stages were separated. Further PLS-DA analysis significantly improved the classification results. The R(2)X was 0.757, the R(2)Y was 0.977 and the Q(2)Y was 0.87, indicating that the model stability and predictability were good. Eight metabolites, including N-acetylneuraminic acid-9-phosphate, 5'-methioadenosine, uric acid-3-nucleoside, pseudouridine, L-valine, succinic acid, L-proline and ß-nicotinamide mononucleotide were identified. The contents of these metabolites increased with the development of the disease. There was correlation between urine metabolites and clinical staging in patients with ovarian cancer.

Large-scale separation of alkaloids from Gelsemium elegans by pH-zone-refining counter-current chromatography with a new solvent system screening method.

A rapid and simple solvent system screening method was developed for pH-zone-refining counter-current chromatography (CCC) separation, which was much easier to find a suitable solvent system than the traditional method. Using this method, an optimal solvent system composed of hexane-ethyl acetate-methanol-water (3:7:1:9, v/v) was selected for pH-zone-refining CCC separation of alkaloids from the stems of Gelsemium elegans, where 10mM triethylamine (TEA) was added to the upper organic stationary phase as a retainer and 10mM hydrochloric acid (HCl) to the aqueous mobile phase as an eluter. As a result, six oxindole alkaloids, 420mg 19-xo-gelsenicine, 456mg gelsemine, 723mg koumine, 379mg 11-methoxygelsemamide, 342mg gelsenicine and 318mg humantenine were successfully purified in one step from 4.5g crude extract with the purity of over 95%, respectively. The structures of the oxindole alkaloids were identified by ESI-MS, (1)H NMR and (13)C NMR.