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[A study of quality standards for fuyanke granule].

OBJECTIVE: To establish the quality standards for fuyanke(FYK) granule. METHODS: The phellodendron Chinese schneid, polygonum cuspidatum, sieb. et Zucc and glycyrrihza uralensis fisch in FYK granule were identified by thin-layer chromatography(TLC). The contents of berberine were determined by thin-layer chromatographic scanning(TLCs). RESULTS: The average recovery rate was 97.86%, and the relative standard deviation 1.96%. CONCLUSION: The method is simple, accurate and reliable.

Berberine↗

[Studies on the quality control of shangke wangshui].

Shangke Wangshui is a new Chinese traditional patent medicine. Its main ingredients Coptis Chinsis Franch, Phellodendron amurense Rupr. and Gardenia jasminoides Ellis. were identified by TLC and PC. The content of active component berberine in Shangke Wangshui was determined by TLC-scanner. This mothod is simple, quick and highly reproducible and can be as a quality control standards for this preparation.

Berberine↗

[Quantitative analysis of urban forest structure: a case study on Shenyang arboretum].

The spatial features and attribute data of urban forests in Shenyang arboretum were acquired by using aerial photographs and field investigation. After systemic and quantitative analysis of the species composition and spatial distribution pattern of urban forest community based on geographic information system (GIS), the following results were achieved: 1) the vegetation in the arboretum was rich and in a good condition. Phellodendron amurense, Robinia pseudoacacia, and Ulmus punita were the main species according to their abundant individuals and relative dominance. The spatial distribution pattern of this vegetation indicated that it was in a growing level and in the best state for ecological benefits; 2) the tree species relative dominance based on vegetation quantity had no distinct relationship with the species abundance, and the species having abundant individuals might have a low relative dominance; and 3) the curve displayed in the relationship diagram between tree individuals and tree height showed ascending and protruding. With the increment of tree height class, the individuals were unchanged nearly at the beginning, but when the height was more than 12 m, the individuals reduced distinctly, and the curve displayed a quickly declined trend. The relationship between tree individuals and tree diameter at the breast height (DBH) showed the same result.

City Planning↗

Screening of indigenous plants from Japan for modulating effects on transformation of the aryl hydrocarbon receptor.

The aryl hydrocarbon receptor (AhR) is a ligand-activated transcription factor with which halogenated and polycyclic aromatic hydrocarbons such as dioxins and benzo[a]pyrene interact as ligands. Since such compounds cause various toxicological effects, including cancer, through the transformation of AhR, it is important to determine influence of modulating factors. It has been reported that certain plant components such as flavonoids and indoles can affect AhR transformation. In this study, to obtain clues to novel ligands of AhR, 191 species of indigenous plants were collected in Japan, and their 50% methanolic extracts (total 368 plant parts) were tested for modulating effects on AhR transformation in a cell-free system using a rat hepatic cytosolic fraction. Among tested extracts at a concentration of 1 mg dry weight of plant/mL, 174 of 368 extracts suppressed 1 nM 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD)-induced AhR transformation to 50% or less, while 9 extracts per se induced AhR transformation equivalent to more than 20% of that induced by 1 nM TCDD. Mallotus japonicus (Thunb.) Muell. (leaf) and Trichosanthes rostrata Kitamura (fruit and fruit skin) strongly suppressed 1 nM TCDD-induced AhR transformation, while Phellodendron amurense Ruprecht (seed) per se strongly induced AhR transformation. These results suggest that a large variety of plants in Japan contain various compounds modulating, mainly suppressing, AhR transformation.

Animals↗

[Berberine-electrochemical detector for the determination of berberine-type alkaloids in various Chinese patent medicines by flow injection analysis].

A description is given for the preparation of flow through sensor and of the incorporation of the sensor into a flow injection analysis system. The parameters affecting the measurement are discussed. An accurate, convenient and rapid method is proposed for the determination of berberine-type alkaloids in various Chinese patent medicines (Coptis chinensis Franch., Phellodendron chinesis Schneid., xianglian wan, zuojin wan, ermiao wan and sanmiao wan). The slope is 54-60 mV/decade over the concentration range of 10(-3)-3 x 10(-6) mol/L berberine at pH 2-9.5. Direct potentiometry determination of berberine in various samples showed an average recovery of 99.5-103.5% and a relative standard deviation of 1.3-3.5% at a sampling rate of 120/h.

Berberine↗

[Quality standards for qingwei huanglian pills].

In the paper systematic studies on quality standards for Qingwei Huanglian Pills are reported, along with the TLC identification of Gardenia jasminoides, Scutellaria baicalensis and Anemarrhena asphodeloides and the quantitative determination of berberine in Coptis chinensis and Phellodendron chinese by TLC densitometric method. To simplify the operation, the same solvent was used for both the identification and determination. The quantitative method is simple, sensitive, reproducible and accurate. The recovery of berberine is 99.48%. The coefficient of variation is 1.42%.

Berberine↗

Stir bar sorptive extraction for the analysis of wine cork taint.

A magnetic stir bar with a polydimethylsiloxane coating was used to absorb 2,4,6-trichloroanisole, 2,3,4,5-tetrachloroanisole, pentachloroanisole and their respective phenols from synthetic and real wine samples. The stir bar sorptive extraction method was optimised to obtain the best extraction conditions in terms of temperature, time, pH and NaCl addition. The stir bar was desorbed in a thermal desorption system coupled to a gas chromatograph-mass spectrometer. The method proposed showed good linearity over the concentration range tested and correlation coefficients ranged from 0.96 to 0.99 for all the analytes. The reproducibility and repeatability of the method was estimated between 1.29 and 4.02%. With no a pre-concentration step and with a much reduced analysis time, all the analyzed compounds showed detection and quantification limits that were lower than those observed with other methods found in the bibliography. Except for pentachlorophenol due to its poor absorptivity in polydimethysiloxane, in red wines, LOD ranged between 7.56 and 61.56 pg/l, and LOQ ranged between 17.21 and 205.11 pg/l; while in white wines, the LOD ranged between 5.82 and 30.50 pg/l and LOQ ranged between 19.41 and 101.61 pg/l. These concentrations were always lower than their respective olfactory thresholds values.

Gas Chromatography-Mass Spectrometry↗

Development of solid-phase extraction and solid-phase microextraction methods for the determination of chlorophenols in cork macerate and wine samples.

Tri-, tetra- and pentachlorophenol (TCP, TeCP and PCP) can be considered the precursors in the formation of corresponding chloroanisoles, known to be powerful odorants in corks and wine. Determining the presence of these chlorophenolic compounds in cork soaking solutions (ethanol/water mixtures, 12% (v/v) ethanol used for cork quality control testing), or in wine can be achieved by acetylation/gas chromatography electron-capture detection. In order to reach the required sensitivity, a previous preconcentration step is necessary. Solid-phase extraction (SPE) and headspace solid-phase microextraction (HS-SPME) have given good results for the preconcentration of TCP, TeCP and PCP in such matrices. The use of Oasis HLB cartridges gives acceptable recoveries for the three compounds when different volumes (50-250 mL) of cork macerate with concentrations ranging from 20 to 150 ng/L are processed. Preconcentration based on HS-SPME has also been optimised with a 100 microm polydimethylsiloxane fibre and in situ derivatization. The HS-SPME method allows chlorophenols in a cork soaking solution and in wine to be determined with a limit of detection of 1 ng/L for each compound (in cork macerate) and a repeatability of around 0.5%-5% (n=8) for a concentration level of 30 ng/L.

Chlorophenols↗

Optimisation of a headspace solid-phase microextraction method for the direct determination of chloroanisoles related to cork taint in red wine.

One of the most critical problems in the enological industry is associated with cork taint. The main compounds responsible for this off-flavour are some chloroanisoles: 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TECA) and pentachloroanisole (PCA). Headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-electron capture detection has been used for the direct determination of these chloroanisoles in wine samples. After the evaluation of some parameters (desorption conditions and salt addition) that affect extraction efficiency, a screening study of six types of fibres and five extraction temperatures was performed. Then, a Doehlert matrix including the exposure time, temperature and Vs (sample volume)/Vt (total volume) ratio as experimental factors was proposed. According to the results of this design and the kinetic profiles evaluated, an analytical procedure based on HS-SPME was optimised and validated. This method can be used for the simultaneous determination at the low ng/l level of all chloroanisoles involved in cork taint, and not only TCA, which is the only compound found in the literature when SPME is proposed as the analytical technique.

Anisoles↗

Sorption behaviour of bifenthrin on cork.

Biphentrin, a known pyrethroid, was studied, aiming its removal from aqueous solutions by granulated cork sorption. Batch experiments, either for equilibrium or for kinetics, with two granulated cork sizes were performed and results were compared with those obtained with of activated carbon sorption. Langmuir and Freundlich adsorption isotherms were obtained both showing high linear correlations. Bifenthrin desorption was evaluated for cork and results varied with the granule size of sorbent. The results obtained in this work indicate that cork wastes may be used as a cheap natural sorbent for bifenthrin or similar compounds removal from wastewaters.

Adsorption↗

Determination of odour-causing volatile organic compounds in cork stoppers by multiple headspace solid-phase microextraction.

Multiple headspace solid-phase microextraction (MHS-SPME) coupled with gas chromatography-mass spectrometry has been applied in order to determine 2,4,6-trichloroanisole (2,4,6-TCA), guaiacol, 1-octen-3-ol and 1-octen-3-one in three samples of cork stoppers. These compounds are responsible for cork taint in wine and can modify the organoleptic properties of bottled wine. Variables such as temperature, addition of water, extraction time, and amount of cork were studied. The extractions were performed with a 50/30 microm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) fibre for 45 min at 100 degrees C using 20 mg of cork. For calibration, 50 microL of VOC aqueous solutions were used and the extraction were carried out for 45 min at 75 degrees C. The limits of detection of the method expressed as ng of VOC per g of cork were 0.3 for 2,4,6-TCA, 7.5 for guaiacol, 1.7 for 1-octen-3-one and 1.9 for 1-octen-3-ol. Relative standard deviation of replicate samples was less than 10%. Significant losses of analytes were observed when the samples were ground at room temperature. Finally, a recovery study was performed and the MHS-SPME results were validated using Soxhlet extraction results.

Anisoles↗

Determination of 2,4,6-trichloroanisole and guaiacol in cork stoppers by pressurised fluid extraction and gas chromatography-mass spectrometry.

This paper describes the development of an analytical method consisting of pressurised fluid extraction (PFE) and gas chromatography-mass spectrometry (GC-MS) using experimental designs to determine two volatile compounds in naturally-tainted cork stoppers. The target analytes, 2,4,6-trichloroanisole (2,4,6-TCA) and guaiacol, are involved in the cork taint of wine. First, a Plackett-Burman experimental design was carried out in order to determine the significant experimental parameters affecting the PFE process, and then a central composite design was used to optimise these significant parameters. Once the method had been optimised, the influence of the number of extraction cycles was studied. The method was applied to determine the concentration of 2,4,6-TCA and guaiacol in three cork samples, and the results were compared with the ones obtained by multiple headspace-solid-phase microextraction (MHS-SPME) and by Soxhlet extraction.

Anisoles↗

Quantification of chloroanisoles in cork using headspace solid-phase microextraction and gas chromatography with electron capture detection.

Chloroanisoles can migrate from the cork stopper in wine bottles to the wine and give it a musty taint so it is important to find a method by which they can be determined. The aim of this paper is to develop a method for quantifying 2,4-dichloroanisole, 2,6-dichloroanisole, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole and 2,3,4,5,6-pentachloroanisole in cork using headspace solid-phase microextraction and gas chromatography with electron capture detection. After we had prepared the cork standards that were so essential to the work we optimised the parameters that most influence headspace solid-phase microextraction: fibre coating, vial volume, cork, kind and volume of solvent to help the extraction, extraction temperature and time, ionic strength and stirring. The method quantifies the total amount of chloroanisoles in cork stoppers (natural, agglomerated, agglomerated with disks and sparkling wine stoppers), at suitable concentrations so that the capacity of these compounds to give wine a musty taint can be evaluated. The quantification limits are: 2,6-dichloroanisole (8.6 ng/g), 2,4,6-trichloroanisole (0.8 ng/g), 2,4-dichloroanisole (3.5 ng/g), 2,3,4,6-tetrachloroanisole (0.6 ng/g), 2,3,4,5,6-pentachloroanisole (0.8 ng/g). The other quality parameters are: recoveries (90.3-105.8%), repeatability (4-13% (RSD expressed)) and intermediate precision (5-14% (RSD expressed)).

Anisoles↗

Non-destructive method to determine halophenols and haloanisoles in cork stoppers by headspace sorptive extraction.

The new solvent-free technique called headspace sorptive extraction (HSSE) was used to determine 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole, 2,4,6-tribromoanisole, pentachloroanisole in cork stoppers, without grinding them, as these may be responsible for the cork taint off-flavour in wine. The best HSSE sorption kinetics for the target analytes were obtained after submitting the spiked corks to 100 degrees C for 1h, followed by a 30 min stabilization time at room temperature. The stir bar was desorbed in a thermal desorption system coupled to a gas chromatograph-mass spectrometer. The method proposed showed good linearity over the concentration range tested, 1-70 ngg(-1), and correlation coefficients ranged from 0.90 to 0.99 for all the analytes. The reproducibility and repeatability of the method were estimated between 4.91 and 12.67%. The effect of the different cork matrixes on the extraction recovery of the target compounds was studied, with the natural corks showing the higher recovery percentage in relation to agglomerate ones.

Anisoles↗

Integrated Fenton's reagent-coagulation/flocculation process for the treatment of cork processing wastewaters.

In the present work two methods were tested for the treatment of cork processing wastewaters. In a first phase, a coagulation/flocculation method was applied using FeCl3 as flocculating agent and Ca(OH)2 as base-precipitant. One cycle of the treatment (1000 ppm of FeCl3) reduced chemical oxygen demand (COD), total polyphenols and aromatic compounds of the effluent by 45, 71 and 58%, respectively. Two cycles of treatment (2x 1000 ppm of FeCl3) increase these reductions until values of 67, 92 and 85%, respectively. In a second phase, an integrated Fenton-coagulation/flocculation process was applied (this second method only requires the addition of H2O2). One cycle of the integrated process (1000 ppm of FeCl3 and 0.5 mol/l of H2O2) reduced the COD, total polyphenols and aromatic compounds of the effluent by 74, 99 and 98%, respectively, which supposes a considerable improvement compared with the first method.

Coagulants↗

Fenton oxidation of cork cooking wastewater--overall kinetic analysis.

In the present work, the possibility of using chemical oxidation through Fenton's reagent for the pre-treatment of cork cooking wastewaters was exploited. Aiming both the selection of the best operating conditions (pH, Fe2+:H2O2 ratio and initial H2O2 concentration) and the evaluation of the overall reaction kinetics, trials were performed in a batch reactor. Operating at pH = 3.2, H2O2 concentration = 10.6 g/L and Fe2+:H2O2 ratio = 1:5 (by weight), about 66.4% of total organic carbon (TOC), 87.3% of chemical oxygen demand (COD) and 70.2% of biochemical oxygen demand (BOD5) were removed and an increase of the BOD5/COD ratio from 0.27 to 0.63 was achieved. In the temperature range 20-50 degrees C, the best performance was obtained at 30 degrees C. The kinetic study was undertaken at different initial TOC concentrations and temperatures. Overall kinetics can be described by a second-order followed by a zero-order rate equation and the apparent kinetic constants at 30 degrees C are k = 2.3 x 10(-4) L/mg min and k0 = 26.0 mg/L min, respectively. The experiments performed at different temperatures confirmed the global kinetic model and allowed to calculate the global activation energy for the second-order reaction (70.7 kJ/mol).

Hot Temperature↗

Purification of cork processing wastewaters by ozone, by activated sludge, and by their two sequential applications.

Wastewaters generated in the cork processing industry were treated in continuous reactors by means of single treatments separately-a chemical ozonation and an activated sludge system-and then by both sequential processes-ozonation followed by aerobic degradation, and aerobic degradation followed by ozonation. The removals obtained in the ozonation alone were 12-54%, 65-81%, and 55-89% for the COD, total phenolics, and absorbance at 254 nm, respectively, while the consumed ozone yield ranged from 40% to 61%, and the biodegradability (BOD(5)/COD) varied from an initial 0.60 to final values between 0.68 and 0.93. The optimum hydraulic retention time and ozone partial pressure were 3 h and 3 kPa, respectively. The stoichiometric ratio was 0.56 g of organic substrate degraded per g of ozone consumed, while the rate constants obtained for the ozone disappearance and for the organic matter degradation were 4490 L g COD(-1) h(-1) and 1970 L g O(3)(-1)h(-1) respectively. The presence of hydrogen peroxide or UV radiation in addition to ozone increased the values of organic matter removal as well as the stoichiometric ratio and the rate constants. The aerobic treatment by the activated sludge system yielded COD removals between 13% and 37% for hydraulic retention times between 24 and 96 h, and the Contois model gave values of q(max)=0.14 g COD g VSS(-1)h(-1) and K(1)=22.6 g COD g VSS(-1) for the main kinetic parameters. The sequential processes increased the substrate removal efficiencies in comparison with the individual processes. These enhancements were greater in the aerobic degradation-ozonation sequence than in the ozonation-aerobic degradation sequence.

Bioreactors↗