One-Pot Process for the Production of Ginsenoside Rd by Coupling Enzyme-Assisted Extraction with Selective Enzymolysis.

One-pot process for the production of ginsenoside Rd by coupling enzyme-assisted extraction with selective enzymolysis was explored in this paper. Several detection methods including HPLC-MS were used to identify and quantify the products in the enzymolysis solution of pectinase. Results showed that ginsenoside Rd was the main component in enzymolysis solution, pectinase specifically hydrolyzes protopanaxadiol (PPD)-type ginsenoside and was a selective enzyme to convert ginsenoside Rb1 to Rd in a way. In addition the influencing factors on the yield of ginsenoside Rb1 and Rd were optimized using L9(34) orthogonal design data. The enzymolysis conditions for the higher yield of Rd were 52.5 °C, pH 6 and 1 h with a yield of 0.8314 from 50 mg drug material. The controllable transformation hypothesis of the PPD-type ginsenoside was also explored from the perspective of the molecular steric hindrance. Pectinase could be used as an efficient enzyme for one-pot producing ginsenoside Rd.

A Novel Green Extraction Technique for Extracting Flavonoids from Folium nelumbinis by Changing Osmosis Pressure.

A new green and sustainable extraction technique, namely osmosis extraction (OE), was developed for efficient extracting flavonoids from Folium nelumbinis by changing the osmotic pressure. The antioxidant activities of the extracted flavonoids were also evaluated. Ethanol and ammonium sulfate were selected for the OE system because they are environmentally friendly. The maximum flavonoids concentration in the top phase was obtained with an ethanol volume fraction of 42.0% and the salt mass of 1.9 g. The kinetic behavior of the extraction process showed that OE had higher efficiencies especially coupled with ultrasonication due to the accompanying and serious morphological changes of Folium nelumbinis cells observed by digital microscope and nano-computed tomography (nano-CT). Results of morphological and anatomical features showed that the higher intracellular chemical potential made the cell expand and even led to bursting. The results also showed that the extraction efficiency of flavonoids with high antioxidant activities was higher than that of the traditional method. The interface effect enhanced the extraction during the salting-out extraction and osmosis was the main factor that improved the extraction efficiency.

Salting-out extraction of ginsenosides from the enzymatic hydrolysates of Panax quinquefolium based on ethanol/sodium carbonate system.

BACKGROUND: Salting-out extraction (SOE) had been developed as a special branch of aqueous two-phase system recently. So far as we know, few reports involved in extracting ginsenosides with SOE because of the lower recovery caused by the unique solubility and surface activity of ginsenosides. A new SOE method for rapid pretreatment of ginsenosides from the enzymatic hydrolysates of Panax quinquefolium was established in this article. METHODS: The SOE system comprising ethanol and sodium carbonate was selected to extract ginsenosides from the enzymatic hydrolysates of Panax quinquefolium, and HPLC was applied to analyze the ginsenosides. RESULTS: The optimized extraction conditions were as follows: the aqueous two-phase extraction system comprising ethanol, sodium carbonate, ethanol concentration of 41.51%, and the mass percent of sodium carbonate of 7.9% in the extraction system under the experimental condition. Extraction time had minor influence on extraction efficiency of ginsenosides. The results also showed that the extraction efficiencies of three ginsenosides were all more than 90.0% only in a single step. CONCLUSION: The proposed method had been successfully applied to determine ginsenosides in enzymatic hydrolysate and demonstrated as a powerful technique for separating and purifying ginsenosides in complex samples.

Covalent Organic Framework as a Heterogeneous Ligand for the Regioselective Oxidative Heck Reaction.

A simple imine-based covalent organic framework (COF) as heterogeneous ligand for PdII-promoted Heck reaction is reported. Good regioselectivity for a wide range of electronically unbiased olefins is obtained (linear/branched >100:1 in most cases). Related tests and density functional theory calculations are used to explore the reason underlying the high selectivity. This research opens a route for COF as an intriguing platform to control regioselectivity catalysis.

The Mn-catalyzed paired electrochemical facile oxychlorination of styrenes via the oxygen reduction reaction.

Reported herein is the electrochemical engendering of chlorine radicals by a manganese catalyst with a controllable pattern, and inexpensive MgCl2 as the chlorine source. In combination with the oxygen reduction reaction, chloroacetophenones were synthesized with abundant styrene as the feedstock in good to excellent yields.

Facile preparation of hybrid porous polyanilines for highly efficient Cr(vi) removal.

In the present work, leucoemeraldine-based hybrid porous polyanilines (LHPPs) have been synthesized by the Friedel-Crafts reaction of leucoemeraldine and octavinylsilsesquioxane (OVS) for Cr(vi) removal. The resulting LHPPs were characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy and N2 adsorption-desorption. The findings indiated that the LHPPs were amorphous, with apparent surface areas (S BET) in the range of 147 to 388 m2 g-1 and total volumes in the range of 0.13 to 0.44 cm3 g-1. Cr(vi) removal experiments displayed that the LHPPs exhibited highly efficient Cr(vi) removal performance. The maximum Cr(vi) removal capacity of LHPP-1 was 990.1 mg g-1 at 308 K and pH 1, which is higher than those of other reported polyaniline-based adsorbents. The adsorption process was a spontaneous, endothermic and chemical adsorption process. The adsorption behavior agreed well with Langmuir models and pseudo second-order equations. X-ray photoelectron spectroscopy and Fourier transformed infrared (FTIR) spectroscopy analysis revealed that the highly efficient Cr(vi) removal performance can be mainly attributed to the existence of numerous amine and imine groups on the surface of the LHPPs; these can function as adsorption active sites for Cr(vi) removal through electrostatic adsorption and reduction to Cr(iii) under acidic conditions. Moreover, the LHPPs exhibited excellent adsorption selectivity for Cr(vi) despite the presence of other metal ions (K+, Cu2+, Mn2+) and anions (NO3 -, SO4 2-). Therefore, the LHPPs have potential applications for Cr(vi) removal in industrial wastewater.

A New Microextraction Technique for the Assay of Alkaloids in Chinese Compound Formula-Based Polyether Sulfone Membrane Fiber Decorated by TiO2 Nanoparticles.

A new nanocomposite membrane was used to clean up impurities from complex samples and the obvious synergy was obtained in this paper. The nanocomposite membrane was prepared by dispersing TiO2 nanoparticles in chloroform and filled in the pores and lumen of polyether sulfone membrane fiber. The novel microextraction method showed the ideal selective extraction effect for alkaloids in the formulae composed of Rhizoma coptidis and the excellent clean-up efficiency compared with the single membrane method. The optimum extraction conditions were as follows: chloroform as accepted phase; the number of nanocomposite membrane fiber bars, 7; extraction time, 30 min; pH of the sample solution, 10.55; desorption solvent, methanol. The limit of detection for the described alkaloids was estimated at 0.122 µg mL-1. The recovery of the four alkaloids in complex samples ranged from 93.24% to 97.94% with relative standard deviation of <4.99 (n = 5). The validated method had been successfully applied to study the transfer rate of alkaloids in the producing process of Qihuang capsule and the ideal transfer rate of alkaloids was obtained in this paper.

Analysis of five alkaloids using surfactant-coated multi-walled carbon nanotubes as the pseudostationary phase in nonaqueous capillary electrophoresis.

In this paper, surfactant-coated multi-walled carbon nanotubes (SC-MWNTs) have been proposed as a novel pseudostationary phase (PSP) to enhance the separation of isoquinoline alkaloids in nonaqueous capillary electrophoresis (NACE). Several parameters affecting NACE separation were studied including the MWNT concentration, the electrolyte concentration, pH* and the separation voltage. In comparison to conventional NACE, the addition of an MWNT dispersion using surfactant solutions in the electrolyte produced an important enhancement in the resolution due to the π-π interactions between the analytes and the surface of the carbon nanotubes. Using SC-MWNTs (6µgmL(-1)) as a PSP in the background electrolyte (BGE) (i.e., 20mM sodium acetate in methanol-acetonitrile (80:20, v/v)) provided the complete separation of five alkaloids. Finally, the developed method has been successfully applied to the detection and quantification of the tested compounds of Rhizoma Coptidis.

[Application of digital earth technology in research of traditional Chinese medicine resources].

This paper describes the digital earth technology and its core technology-"3S" integration technology. The advance and promotion of the "3S" technology provide more favorable means and technical support for Chinese medicine resources survey, evaluation and appropriate zoning. Grid is a mature and popular technology that can connect all kinds of information resources. The author sums up the application of digital earth technology in the research of traditional Chinese medicine resources in recent years, and proposes the new method and technical route of investigation in traditional Chinese medicine resources, traditional Chinese medicine zoning and suitability assessment by combining the digital earth technology and grid.

[The first and second cluster analysis of dual index grade sequence of IR fingerprint spectra of Guifudihuang pill and Jinkuishenqi pill samples and their quality evaluation].

In the present paper a method for identifying and evaluating traditional Chinese medicine (TCM) Jinkuishenqi pill and Guifudihuang pill samples is proposed. Mathematical statistics was applied to analyze the dual index sequences of infrared fingerprint spectra of components extracted from Jinkuishenqi pill and Guifudihuang pill samples with water, then the grade sequences were determined and the first and second clusters were performed based on these grade sequences. As a results, the most similar sample groups of different samples were also obtained. The Jinkuishenqi pill and Guifudihuang pill samples can be distinguished accurately with the most similar sample groups. The method put forward is new and effective to identify and evaluate combinational TCM quantitatively.

[Determination of alkaloids from Coptis chinensis Franch. and Phellodendron amurense Rupr. Decocted together in baitouweng decocta by high performance capillary electrophoresis].

A rapid and accurate method for determining alkaloids from Coptis chinensis Franch, and Phellodendron amurense Rupr, decocted together in Baitouweng decocta was established. Experiments were carried out on a self-assembled capillary electrophoresis system. The experimental conditions were as follows: 75 microns i.d. x 50 cm fused silica capillary, 0.05 mol/L Na2B4O7-CH3OH (85:15, V/V) as buffer, applied voltage 14 kV and detection wavelength 232 nm. In addition, the concentration of ethanol in the extraction solvent was optimized. Experimental results showed that ethanol-water (30:70, V/V) was the ideal solvent to extract the main effective ingredients from Coptis chinensis Franch. and Phellodendron amurense Rupr. decocted together in Baitouweng decocta. Berberine and palmatine had good linearities in the range of 15.0 mg/L-65.0 mg/L and 12.5 mg/L-50.0 mg/L respectively, and their average recoveries were 95.5%-104% (RSD 2.7%-6.9%) and 92.1%-103% (RSD 4.5%-6.7%) respectively.