Determination of isoflavones in red clover by capillary electrophoresis with electrochemical detection

Capillary electrophoresis with electrochemical detection (CE-ED) was employed to analyze isoflavones in red clover (Trifolium pratense). The effects of potential of working electrode, pH and concentration of running buffer, separation voltage and injection time on CE-ED were investigated. Operated in a wall-jet configuration, a 300 microm diameter carbon-disk electrode was used as the working electrode, which exhibits a good response at +0.85 V (versus saturated calomel electrode) for the analytes. The analytes could be separated in a 50 mmol/l borate buffer (pH 9.5) within 25 min. The response was linear over three orders of magnitude with detection limit (S/N=3) ranging from 2x10(-5) mg/ml to 5x10(-5) mg/ml for the analytes. This method has been used for the determination of daidzein, genistein and biochanin A in red clover with satisfactory results.     

Antioxidant activity of propolis: role of caffeic acid phenethyl ester and galangin

Propolis, a natural product produced by the honeybee, has been used for thousands of years in folk medicine for several purposes. The extract contains amino acids, phenolic acids, phenolic acid esters, flavonoids, cinnamic acid, terpenes and caffeic acid. It possesses several biological activities such as antiinflammatory, immunostimulatory, antiviral and antibacterial. The exact mode of physiological or biochemical mechanisms responsible for the medical effects, however, is yet to be determined. In this work, we have investigated the antioxidant activity of a propolis extract deprived of caffeic acid phenethyl ester (CAPE). In addition, the activity of CAPE and galangin was also examined. Propolis extract (with and without CAPE) and its active components showed a dose-dependent free radical scavenging effect, a significant inhibition of xanthine oxidase activity, and an antilipoperoxidative capacity. Propolis extract with CAPE was more active than propolis extract without CAPE. CAPE, used alone, exhibited a strong antioxidant activity, higher than galangin. The experimental evidence, therefore, suggests that CAPE plays an important role in the antioxidant activity of propolis.     

Determination of formaldehyde in particle boards using headspace gas chromatography

Summary Formaldehyde in particle board was analyzed by gas chromatography (GC) using instruments equipped with headspace injector and flame-ionization detector. The application of the method to the determination of formaldehyde desorbing from urea-formaldehyde and melamine-urea-formaldehyde resins used in manufacturing particle board is discussed. In the 47 samples analyzed, the concentration ranged between 10.34–56.29 mg of formaldehyde/100 g of particle board.     

Effect of a propolis extract and caffeic acid phenethyl ester on formation of aberrant crypt foci and tumors in the rat colon

We have studied the effect of propolis and its main active ingredient caffeic acid phenetyl ester (CAPE) on formation of aberrant crypt foci (ACF) and tumors in the rat colon in vivo. CAPE (50 mg/kg i.p.) reduced the formation of ACF and tumor induced by azoxymethane, while propolis ethanolic extract was without effect. These results suggest a potential anti-carcinogenesis of CAPE but not propolis.     

气相色谱法检测湖南掺杂油茶籽油

采用气相色谱法,对自行提取的16个湖南油茶籽样品、湖南本地的20家油茶籽油生产企业生产的油茶籽油进行脂肪酸组成测定,并对不同比例的大豆油、花生油、玉米油、葵花油、菜籽油、米糠油、棕榈油和油茶籽油组成的二元体系的样品进行了脂肪酸组成分析。通过分析脂肪酸组成的变化,建立了应用气相色谱法快速、精准地检测油茶籽油中掺杂大豆油、花生油、玉米油、葵花油、菜籽油、米糠油、棕榈油含量的油茶籽油掺假判定方法。     

The role of the phenethyl ester of caffeic acid (CAPE) in the inhibition of rat lung cyclooxygenase activity by propolis

In this study we investigated the effect of an ethanolic extract of propolis, with and without CAPE, and some of its components on cyclooxygenase (COX) activity. Propolis (0.00003-0.03%) significantly and concentration-dependently inhibited COX activity from lung homogenate of saline- or LPS-treated rats. Same results were obtained with CAPE (0.1-100 microM). COX activity from lung homogenate of saline- or LPS-treated rats was also inhibited by galangin (0.1-100 microM), although the inhibition induced by the lowest concentration was not significant. Caffeic, ferulic, cinnamic and chlorogenic acids and pinocembrin, (0.1-100 microM) did not affect COX activity. The inhibition curves showed that CAPE and propolis were equipotent inhibitors, whereas galangin was significantly (P<0.001) less potent than propolis and CAPE. In order to better investigate the role of CAPE, we tested the action of an ethanolic extract of propolis (0.00003-0.03%) without CAPE. This extract significantly and concentration-dependently inhibited COX activity from lung homogenate of saline- or LPS-treated rats, however, it resulted to be approximately 10 times less potent than the extract containing CAPE. The analysis of the inhibition curves of the extract with and without CAPE showed a significant (P<0.001) difference. These results suggest that both CAPE and galangin contribute to the overall activity of propolis, CAPE being more effective.     

TLC法测定几种植物中熊果酸的含量

采用薄层扫描法对车前草、夏枯草、山茱萸中熊果酸的含量进行了测定, 其TLC测定条件为用环己烷-氯仿-乙酸乙酯(20 5 8) 作展开剂; 用10%H2SO4乙酸溶液作显色剂。测定结果表明: 3种植物中, 以夏枯草的熊果酸含量最高, 达0 812 %, 车前草的熊果酸含量最低, 为0 516 %, 前者是后者的1 57倍。该方法简便、快速、准确、可靠, 回收率高达96 1 %。     

等离子光谱法同时测定土壤中微量铬、铅、镍、铜和锌

用电感耦合等离子光谱法,测定了土壤中微量镍、铜、铬、铅和锌的含量,结果表明:相对标准偏差为1.78%~3.12%,回收率为97.3%~103.8%。该方法简便,易操作,数据重复性好,加标回收率高。重点讨论了样品前处理方法对测定结果的影响。     

Determination of ligustilide in the brains of freely moving rats using microdialysis coupled with ultra performance liquid chromatography/mass spectrometry

In this paper, microdialysis combined with ultra performance liquid chromatography/mass spectrometry (UPLC-MS) was applied for the determination of ligustilide in freely moving rats' brain. The extracellular unbound ligustilide could be detected in rat brain within the first time interval (0-20 min) after nasal administration but not after oral administration. This result showed that ligustilide could quickly enter the brain after nasal administration; which implied that ligustilide may have a rapid onset of action. This work demonstrated the potential application of microdialysis combined with UPLC-MS in pharmacokinetic studies. Furthermore, the advantage that fewer animals used in the microdialysis experiment was confirmed.     

广西不同产地八角茴香果中莽草酸含量测定

采用高效液相色谱法（HPLC）测定广西不同产地八角茴香中莽草酸含量。测定结果表明：武呜太平镇样点的八角茴香样品莽草酸含量最高（11．57％）,玉林六万林场的样品含量最低（6．28％）,同一品种不同产地的八角茴香中莽草酸的含量有显著差异且含量均在6．2％以上。     

Distribution of sulphur fractions in lysimeters previously treated with sulphuric acid,NPK fertilizer and a combination of acid and fertilizer

The retention of applied ³⁵S was studied in a lysimeter experiment, in which the lysimeters, consisting of soil columns with intact field and groundlayer vegetation, had previously been treated with either sulphuric acid, NPK or a combination of sulphuric acid and NPK.³⁵S was applied as Na₂³⁵SO₄ to all lysimeters in an amount corresponding to 2 kg S ha^?1, 3 months before the termination of the experiment. Of the applied ³⁵S, 4.7 ± 1.6% (the error term showing the standard error of the mean) was leached from the lysimeters; ³⁵SO₄^2?, was preferentially sorbed in the upper part of the B horizon, >61% being sorbed in the B horizon as a whole. The influence of previous treatments was seen in SO₄^2? content in the B horizon and also in the SO₄^2? concentrations in the leachates from the lysimeters. Sorption of ³⁵SO₄^2? was enhanced by the acid treatment in the A₀ and A₁/A₂ horizons. Ratios between water-extractable SO₄^2? and KCl-extractable SO₄^2? varied from 0.88 in the A₁/A₂ horizon to 0.46 in the lower part of the B horizon, indicating a preferential sorption of less available SO₄^2? fractions in that part of the soil.Significant positive correlations between soil organic carbon and various sulphur fractions, both labelled and unlabelled, indicated the importance of biological S transformations in the A₀ and A₁/A₂ horizons.Positive correlations between KCl-extractable Al and KCl-extractable SO₄^2? were found in the B horizon. Equilibrium calculations suggested that the SO₄^2? activity and Al³⁺ activity in leachates from control and acidified lysimeters were within the stability fields of basaluminite (Al₄(OH)₁₀SO₄), activities in leachates from the latter group of lysimeters, also being close to jurbanite (Al(OH)SO₄).     

Inhibitory effect of a propolis on Di-n-Propyl Disulfide or n-Hexyl salycilate-induced skin irritation,oxidative stress and inflammatory responses in mice

PurposeThermal imaging has been utilised, both preclinically and clinically, as a tool for assessing inflammation. Psoriasis is a chronic inflammatory skin disease characterised by hyperkeratosis, dermal inflammatory infiltrate and increased angiogenesis. The aim of the present study was to assess the usefulness of thermography in psoriatic lesion regression after topical treatment with bee propolis, recognised as potent antioxidants and anti-inflammatory agents.MethodsWe monitored the inflammation process induced by irritants such as n-Hexyl salycilate (HXS) or Di-n-Propyl Disulfide (PPD) by histopatological assessment of the skin, thermographic scanning, total number of inflammatory cells in the peritoneal cavity, differential analysis of cells in the peritoneal cavity, macrophage spreading index, haematological and biochemical parameters, frequencies of micronucleated reticulocytes, lipid peroxidation and glutathione assay in the skin.ResultsTopically applied ethanolic extract of propolis (EEP) with HXS or PPD reduced the lipid peroxidation in the skin and total number of inflammatory cells in the skin and peritoneal cavity, functional activity of macrophages, the number of micronuclei in mouse peripheral blood reticulocytes and enzymatic activity of ALP and AST.ConclusionThese results demonstrate that topical application of EEP may improve psoriatic-like skin lesions by suppressing functional activity of macrophages and ROS production. Taken together, it is suggested that EEP can safely be utilised in the prevention of psoriasis-related inflammatory changes without causing any toxic effect.     

Determination of oxymatrine and its active metabolite matrine in human plasma after administration of oxymatrine oral solution by high-performance liquid chromatography coupled with mass spectrometry

A rapid, sensitive and selective high-performance liquid chromatography mass spectrometric method has been developed and validated for the simultaneous determination of oxymatrine and its active metabolite matrine in human plasma after administration of oxymatrine oral solution. Analytes were extracted from the plasma by liquid-liquid extraction with chloroform. The chromatographic separation was accomplished on a Venusil C₁₈ column (150 mm × 4.6 mm, 5 μm) protected by a C₁₈ guard column (4.0 mm × 2.0 nm; Phenomenex, Torrance, CA, USA). Analytes were detected on a single quadruple mass spectrometer by selected ion monitoring mode via electrospray ionization source. The assay had a lower limit of quantification of 1.5 ng · mL^− 1 for oxymatrine and 3 ng·mL^− 1 for matrine in plasma. The calibration curves were linear in the measured range. The overall precision and accuracy for all concentrations of quality controls and standards were within ± 15%. The proposed method enabled unambiguous identification and quantification of oxymatrine and its active metabolite matrine in vivo. The results provided a meaningful basis for evaluating the clinical applications of the oxymatrine oral solution.     

西伯利亚杏仁粕营养物质测定与其氨基酸组成评价

为了探究西伯利亚杏仁粕的营养成分及其特点,以西伯利亚杏仁粕为试材,分别采用溶剂法、灼烧法、凯氏定氮法等方法对杏仁粕营养成分的含量与组成进行了测定与分析;采用氨基酸自动分析仪测定了杏仁粕中氨基酸的组成,并应用氨基酸比值系数法,以WHO/FAO氨基酸参考模式为评价标准,对其必需氨基酸的组成进行了评价。测定结果表明:西伯利亚杏仁粕中蛋白质的含量为648.00 mg·g^-1,粗脂肪含量为54.00 mg·g^-1,粗纤维含量为3.20 mg·g^-1,灰分含量为44.00 mg·g^-1。西伯利亚杏仁粕中含有17种氨基酸,氨基酸总含量为65.86%;西伯利亚杏仁粕中8种人体必需氨基酸的总含量为20.59%,其中谷氨酸含量最高,为8.70%,其必需氨基酸与非必需氨基酸的含量比为0.45;其药用氨基酸含量高达41.79%。杏仁粕中还含有丰富的Cu、Zn、Fe、Mn、K、Ca、Mg、P等微量元素和多种维生素,其中维生素E和维生素B2的含量分别为1.39×10-2与0.38×10-3 mg·g^-1。其必需氨基酸的构成比例基本符合食品法典委员会(WHO/FAO)的标准,其氨基酸的比值系数评分(SRC)为76.51。研究结果表明:西伯利亚杏仁粕营养丰富,所含人体必需氨基酸的种类齐全,且配比均衡,是有利于人体氨基酸营养平衡的优质食品原料。     

山杏叶桦木酸、齐墩果酸和熊果酸的研究

我国山杏资源十分丰富,是绿化荒山的优良树种。采用HydersirBDSC18色谱柱（150×4．6mm,5μm）,流动相体积比为90：10的0．3‰硫酸甲醇溶液一3‰硫酸水溶液,检测波长210nm,建立了山杏叶中三萜酸测定的高效液相色谱法。结果表明：桦木酸、齐墩果酸与熊果酸的浓度在30～2000μg／mL（r桦=0．9971,r齐=0．9986,r熊=0．9978）范围内与色谱峰面积呈良好线性关系;平均加标回收率分别为99．9％、101．1％和98．9％。以山杏叶为材料,采用高效液相色谱法和紫外可见分光光度法分别对山杏叶中的三萜酸成分进行分析,结果表明,山杏叶富含三萜酸,落叶期山杏叶中总三萜酸（17078#g／g）、桦木酸（1842μg／g）、齐墩果酸（2536μg／g）和熊果酸（5706μg／g）含量均高于非落叶期。本研究首次建立了山杏叶中桦木酸、齐墩果酸和熊果酸同时测定的反向高效液相色谱法（HPLC）,发现落叶期山杏叶富含三萜酸,为山杏叶综合开发利用提供了基础数据。     

Determination of formic-acid and acetic acid concentrations formed during hydrothermal treatment of birch wood and its relation to colour, strength and hardness

Formation of benzyl esters from acetic and formic acids during heat treatment of birch at 160–200°C has been studied by gas chromatography. High concentrations of formic and acetic acids formed by the wood itself during hydrothermal treatment were found. The concentrations of acids increased with both treatment time and temperature. The maximum formic- and acetic acid concentrations found at 180°C and after 4 h of treatment performed in this work were 1.1 and 7.2%, based on dry-weight wood, respectively. The treated wood material was characterised by mechanical testing [bending tests perpendicular to the grain, modulus of rupture, modulus of elasticity, Brinell hardness, impact bending and colour measurements (CIE colour space)]. The experiments, where high concentration of acids was formed, showed severe losses in mass and mechanical strength. Indications of possible enhanced mechanical properties for the treated, compared with untreated birch wood were found around 180–200°C at short treatment times. This paper discusses possible degradation reactions coupled with the colour and mechanical properties in relation to acid formation, and suggestions for process optimisations.     

Development and application of a capillary electrophoresis method for the determination of ellagic acid in E. globulus wood and in filtrates from E. globulus kraft pulp

A capillary zone electrophoresis (CZE) method for simple and rapid determination of ellagic acid (EA) in Eucalyptus globulus wood and in the filtrate from unbleached kraft pulp has been developed. This is the first application of CZE for the detection of EA in industrial streams from cellulosic pulp production. The EA determinations in wood extractives and in pulp filtrates were succeeded only after sample acidification. This new CZE analytical procedure allowed reliable determinations of EA in E. globulus wood (1.1 ± 0.6 g kg^?1 of dry wood) and in the filtrates from unbleached kraft pulp (98 ± 0.7 mg L^?1). Gas chromatography–mass spectrometry was used as a reference method for the quantification of EA in industrial samples.