A New Thioamide Derivative for Separation and Preconcentration of Multi Elements in Aquatic Environment by Cloud Point Extraction

2-(pyridine-2-yl)-N-p-chlorohydrazinecarbothioamide (HCPTS) was synthesized, characterized and successfully applied for the preconcentration of Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II) in water, blood, and urine samples prior to graphite furnace atomic absorption determination (GFAAS);Hg was determined by cold vapor technique. Under the optimum experimental conditions (i.e. pH = 8, 10–4 M of HCPTS, 0.05% w/v of Triton X-114), calibration graphs were linear in the range of 0.02 to 200 ng?mL–1 for Co(II), Cd(II), Pb(II) and Ni(II);0.03 to 200 ng?mL–1 for Cu(II);0.07 to 200 ng?mL–1 for Fe(II) and Zn(II) and 0.02 to 150 ng?mL–1 for Hg(II). The enrichment factors were 43, 51, 41, 46, 54, 40, 45 and 52 for Cu(II), Ni(II),Zn (II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The limit of detection were found to be 0.019, 0.094, 0.0514, 0.052, 0.0165, 0.047, 0.068 and 0.041 ng?mL–1 for Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The developed method was applied to the determination of these metal ions in water, blood and urine samples with satisfactory results.

Selective Pre-concentration and Solid Phase Extraction of Mercury（Ⅱ） from Natural Water by Silica Gel-loaded （E）-N-（1-Thien-2＇-ylethylidene）-1,2-phenylenediamine Phase

Silica gel-loaded （E）-N-（1-thien-2＇-ylethylidene）-1,2-phenylenediamine （TEPDA） phase was synthesized based on physical adsorption approaches. The stability of a chemically modified TEPDA especially in concentrated hydrochloric acid that was then used as a recycling and preconcentration reagent allowed the further uses of silica gel-loaded immobilized TEPDA phase. The application of this silica gel-loaded phase to sorption of a series of metal ions was performed by using different controlling factors such as the pH of the metal ion solution and the equilibration shaking time by the static technique. This difference was interpreted on the basis of selectivity incorporated in these sulfur containing silica gel-loaded TEPDA phases. Hg（Ⅱ） was found to exhibit the highest affinity towards extraction by these silica gel-loaded TEPDA phases. The pronounced selectivity was also confirmed by the determined distribution coefficients （Kd） of all the metal ions, showing the highest value reported for mercury（Ⅱ） extraction by the silica gel immobilized TEPDA phase. The potential applications of the silica gel immobilized TEPDA phase to selective extraction of mercury（Ⅱ） from aqueous solution were successfully accomplished and preconcentration of low concentration of Hg（Ⅱ） （30 pg·mL^-1） from natural tap water with a preconcentration factor of 200 for Hg（Ⅱ） off-line analysis was conducted by cold vapor atomic absorption analysis.

金樱子提取液对NO_2^-清除作用的体外实验研究

金樱子提取液在模拟胃液的pH酸性条件下对NO-2具有很强的清除作用。用0.1%柠檬酸作提取剂，在固液比为1:3、温度60℃，提取时间为1h所得的金樱子提取液对NO-2有87%以上的清除率；浸出液中的VC、还原糖、黄酮等对NO-2的清除有重要作用；浸出液在低pH值（pH2～3）下对NO-2清除作用强烈，随pH值升高，清除能力急剧下降。

THE EXTRACTED COMPLEX FORMED BY MONO (2-ETHYLHEXYL)-2-ETHYLHEXYL PHOSPHATE WITH DIVALENT Mn

In order to clarify the mechanism and the complex formed in the extraction of divalent Mn by alkylphosphonic acid monoester, the solid complex has been prepared by mono (2-ethylhexyl)-2-ethylhexyl phosphate, HEH(EH)P, HA with divalent Mn. The elemental analysis, magnetic susceptibility and thermogravimetry have been determined for the solid complex of HEH(EH)P-Mn(II) and the infrared spectrum has been carried out in comparison to the extractant HEH(EH)P. The extracted compound has also been studied by electronic and electron spin resonance spectroscopy in octane solvent and solid state at room temperature. On the basis of the measurements, it is concluded that the structure of the solid polymeric species MnA_2 is in a tetrahedral arrangement.

邻苯二甲酸二(2-丙基庚)酯分子印迹固相萃取剂的制备及其应用

以邻苯二甲酸二辛酯（ DOP）为虚拟模板分子，α-甲基丙烯酸（ MAA）为功能单体，乙二醇二甲基丙烯酸酯（ EDMA）为交联剂，采用沉淀聚合法制备了对邻苯二甲酸二（2-丙基庚）酯（ DPHP）具有高选择性的分子印迹聚合物（ MIP）。用紫外分光光度法探索了不同功能单体与模板分子的结合能力，与功能单体丙烯酸（ AA）相比，MAA 与DOP的结合能力更强，其最佳结合的物质的量比为6：1。考察 MIP 对 DOP、DPHP、邻苯二甲酸二甲酯（ DMP）、邻苯二甲酸二丁酯（ DBP）的选择吸附性能，发现该聚合物对 DPHP具有更高的选择吸附性。以制备的聚合物为固相萃取填料，结合 HPLC分析，考察了淋洗剂与洗脱剂的种类和用量对 DPHP 回收率的影响。将 DPHP 甲醇溶液加载至萃取柱后用1 mL甲醇-水（1：9，v/v）淋洗，5 mL甲醇-乙酸（9：1，v/v）洗脱，DPHP在分子印迹固相萃取（ MI-SPE）柱上的回收率达到96.8％，而在非印迹固相萃取（ NISPE）柱上的回收率仅为52.9％。将建立的 MISPE-HPLC方法应用于测定兔口服 DPHP后不同时间点兔血清中 DPHP的浓度，发现其血药浓度的最大值为5.88μg/mL，达峰值时间为4 h，DPHP加标回收率为90.0％~92.0％，相对标准偏差小于5％。

Antioxidant and Antigenotoxic Activity of Bioactive Extracts from Corn Tassel

This study is designed to evaluate antioxidant and antigenotoxic activities of corn tassel extracts（CTTs）. The major bioactive components of CTTs include flavonoid, saponin and polysaccharide. The antioxidant properties of the three bioactive components of CTTs were investigated by Ferric Reducing Antioxidant Property（FRAP） and 1, 1-diphenyl-2-picrylhydrazyl（DPPH） assays. The activities of the extracts were determined by assessing the inhibition of mutagenicity of the direct-acting mutagen fenaminosulf, sodium azide, and indirect-acting mutagen 2-aminofluorene using the Ames test（strains TA98 and TA100）. The results showed that the extraction rates of flavonoid, saponin, and polysaccharide from the dried corn tassels were 1.67%, 2.41% and 4.76% respectively. DPPH and FRAP assay strongly demonstrated that CTTs had antioxidant properties. CTTs at doses of 625, 1250 and 2500 μg per plate reduced 2-aminofluorene mutagenicity by 12.52%, 28.76% and 36.49% in Salmonella typhimurium TA98 strain assay respectively and by 10.98%, 25.27% and 37.83%, at the same doses in Salmonella typhimurium TA100 assay system, respectively. 3-[4, 5-dimethylthiazol-2-yl]-2, 5-diphenyltetrazolium bromide（MTT） assay showed that the different concentrations of CTTs inhibited the proliferation of MGC80-3 cells in a dose-dependent manner（P0.01）. It is concluded that these integrated approaches to antioxidant and antigenotoxicity assessment may be useful to study corn tassel as a natural herbal material.

Effect of Marsdenia tenacissima extract on G2/M cell cycle arrest by upregulating 14-3-3σ and downregulating c-myc in vitro and in vivo

Objective: Marsdenia tenacissima extract(MTE) is a traditional Chinese herbal medicine with anti-cancer activity. In some previous studies, different mechanism actions of the anti-cancer effect of MTE have been revealed. In this study, we first observed that MTE exhibited G2/M cell cycle arrest on two different human breast cancer cell lines, MDA-MB-231 and MCF-7 by mediating 14-3-3σ and c-myc.Methods: The effect of MTE on G2/M cell cycle arrest was evaluated in MDA-MB-231 and MCF-7 cell lines. MTT assay was done for evaluation of cell viability. Flow cytometry was employed for cell cycle analysis. Western blotting analysis and immunohistochemistry were performed to analyze the expression of G2/M cell cycle-related key protein in cells and tissue samples. Animal studies have been conducted to elucidate the anti-tumor effect of MTE.Results: Cell cycle is the backbone for developing cancer. Cell cycle proteins play a major role in the progression of cell cycle and cell proliferation. However, some key protein directly or indirectly modulate the action of cell cycle protein that highly affect cell cycle regulation. In order to investigate cellular proliferation of cancer, we observed that MTE induced the upregulation of 14-3-3σ and downregulation of c-myc,and then reduced the expression of G2/M cell cycle associated key protein, leading to the inhibition of cellular entry into mitosis phase. We also confirmed that MTE exerted a significant antitumor effect on the MDA-MB-231 xenograft model in vivo.Conclusion: G2/M cell cycle arrest occurred by the action of MTE, mediated by the upregulation of 14-3-3σ as well as downregulation of c-myc in MDA-MB-231 and MCF-7 cell lines.

食用菇多糖提取物体外抗氧化性能研究

香菇和鸡腿菇分别经热水浸提,反复醇提、洗涤、真空干燥后得到两种多糖提取物。通过多糖抗食用油脂的氧化作用、利用Fenton反应检测对羟基自由基(.OH)的清除作用、对邻苯三酚自氧化系统产生的超氧阴离子自由基(O2-.)的清除作用以及在模拟胃液条件下清除NO2-的作用,对这两种不同来源的食用真菌多糖的体外抗氧化活性进行了研究。结果表明:两种多糖提取物都具有体外抗氧化性能,香菇多糖提取物的抗活性氧自由基能力和清除NO2-的能力优于鸡腿菇多糖提取物。

Enhanced separation of Pd(Ⅱ)and Pt(Ⅳ)from hydrochloric acid aqueous solution using 2-((2-methoxyethyl)thio)-1H-benzimidazole

Separation of palladium(Pd)and platinum(Pt)by solvent extraction is difficult because of their extremely similar physicochemical properties.Development of new extractants with a high extraction efficiency and excellent separation selectivity is the primary focus for enhancing the separation of Pd and Pt by solvent extraction.In this study,a new extractant,2-((2-methoxyethyl)thio)-1 H-benzimidazole(MOBI),which contains N,S,and O atoms,was synthesized and used to separate Pd(Ⅱ)and Pt(Ⅳ)from a hydrochloric acid aqueous solution.The experimental results revealed that Pd(Ⅱ)and Pt(Ⅳ)were effectively separated under the optimal conditions:MOB I concentration of 0.005 mol·L^(-1),HCl concentration of0.2 mol·L^(-1),organic/aqueous(O/A)phase ratio of 1.0,and contact time of 15 min.The separation coefficient between Pd(Ⅱ)and Pt(Ⅳ)was 1246.40,which indicates that MOBI has a higher selectivity for Pd(Ⅱ)than Pt(Ⅳ).In addition,the mechanism of coordination between Pd(Ⅱ)and MOBI was demonstrated through the slope method,Fourier transform infrared spectroscopy(FTIR),hydrogen-1 nuclear magnetic resonance spectroscopy(^(1)H NMR),and carbon-13 nuclear magnetic resonance spectroscopy(^(13)C NMR).The results revealed that MOBI could coordinate with Pd(Ⅱ)via the N atom in the benzimidazole ring of MOBI molecules to form[Pd(MOBI)_(2)Cl_(2)](O).

Rat cardiomyocyte H9c2(2-1)-based sulforhodamine B assay as a promising in vitro method to assess the biological component of effluent toxicity

The treatment of wastewaters is crucial to maintain the ecological status of receiving waters,and thereby guarantee the protection of aquatic life and human health.Wastewater quality evaluation is conventionally based on physicochemical parameters,but increasing attention has been paid to integrate physicochemical and biological data.Nevertheless,the regulatory use of fish in biological testing methods has been subject to various ethical and cost concerns,and in vitro cell-based assays have thus become an important topic of interest.Hence,the present study intends:(a) to evaluate the efficiency of two different sample pre-concentration techniques (lyophilisation and solid phase extraction) to assess the toxicity of municipal effluents on rat cardiomyoblast H9c2(2-1) cells,and (b) maximizing the use of the effluent sample collected,to estimate the environmental condition of the receiving environment.The gathered results demonstrate that the H9c2(2-1) sulforhodamine B-based assay is an appropriate in vitro method to assess biological effluent toxicity,and the best results were attained by lyophilising the sample as pre-treatment.Due to its response,the H9c2(2-1) cell line might be a possible alternative in vitro model for fish lethal testing to assess the toxicity of municipal effluents.The physicochemical status of the sample suggests a high potential for eutrophication,and iron exceeded the permissible level for wastewater discharge,possibly due to the addition of ferric chloride for wastewater treatment.In general,the levels of carbamazepine and sulfamethoxazole are higher than those reported for other countries,and both surpassed the aquatic protective values for long-term exposure.

Preconcentration/Separation of Some Metal Ions Using Sodium Dodecyl Sulfate Coated Alumina Modified with Bis（5-bromo- 2-hydroxy-benzaldehyde）-2-methyl-1,5-pentane Diimine （BBHBPDI） Prior to Their Flame-AAS Determination

Preconcentration/separation of Co（II）, Fe（III）, Pb（II）, Cr（IIl）, Cu（II） and Cd（II） ions using bis（5-bromo- 2-hydroxy-benzaldehyde）-2-methy1-1,5-pentane diimine （BBHBPDI） on SDS coated alumina has been reported. The influences of the analytical parameters including pH, ligand and SDS amount, type and concentration of eluent and sample volume on metal ions recoveries were investigated. At optimum values of all variables the relative standard deviation are between 2.5-2.7 and preconcentration factor was 375, while recoveries for all understudy metal ions are higher than 95%, determination limits are between 1.5-2.7. The method has been successfully applied to determination of Co（II）, Fe（III）, Pb（II）, Cr（III）, Cu（II） and Cd（II） ions content in some real samples.

黄芪治疗缺血性脑损伤的有效性

目的:对近年来黄芪治疗缺血性脑损伤作以总结,以阐明其在治疗缺血性脑血管病中的有效作用。资料来源:检索数据库Medline1966-01/2005-05有关黄芪的药理作用及其治疗缺血性脑损伤的文章,检索词为“astragulus,cerebralischemiainjury”,限定文章语言种类为英文。同时检索中文医学期刊全文数据库1994-01/2004-12及万方数据库1998-01/2005-11有关黄芪的药理作用及其治疗缺血性脑损伤的文章,检索词为“黄芪,缺血性脑损伤”,限定文章语言种类为中文。资料选择:对资料进行初审,选取包括黄芪与缺血性脑损伤的动物实验和临床研究文章。质量评价主要考察资料的真实性,实施过程是否严密。关于重复实验的多篇文章,选取样本量较大的文章予以纳入。资料提炼:共检索到72篇中文和94篇英文,选取较新的或经典的探讨黄芪的药理作用及其治疗缺血性脑损伤的文章共25篇。排除重复性研究。资料综合:①黄芪具有清除自由基,降低血浆内皮素含量,防止脂质过氧化,改善脑功能的作用。②黄芪能降低兴奋性氨基酸的含量,抑制热休克蛋白70的表达,减轻缺血性脑损伤。③黄芪能提高脑缺血后Bcl-2的水平,拮抗P53和Caspase-3的表达,有效抑制脑缺血引起的神经元凋亡。④黄芪能降低血管通透性,改善脑缺血后血液流变状态,减轻脑缺血损伤。⑤黄芪能抑制脑缺血早期胶质细胞原纤维酸性蛋白过度表达,减轻海马区锥体细胞损伤,保护缺血后脑损伤。结论:黄芪能显著改善脑缺血患者的临床症状,降低致残率,且安全无副作用,有广阔的临床前景。

Screening of Fungi from Chinese Medical Plants for Anti-Human Immunodeficiency Virus Type 1 Activity

In order to Isolate anti-human Immunodeflclency virus （HIV） agents from natural products, 97 ethanollc extracts of 90 fungi were tested for their Inhibitory activity on HIV-1. Most of the extracts tested were relatively non-toxic to human lymphocytic MT-4 cells, but extracts of some fungi exhibited potent antl-HIV activity In an in vitro 3-（4, 5-dlmethyl-2 thlazoyl）-2,5-dlphenyl-2H-tetrazollum bromide assay with a selectivity Index greater than 3. Most fungi were Isolated from Dendrobium sp. and Taxus sp.

基于GEE云平台的福建省10 m分辨率茶园专题空间分布制图

福建省作为中国的产茶大省,快速准确获取茶园的空间分布对福建省农业经济发展和生态环境保护具有重要的决策意义,然而,传统的方法难以保证大范围准确地获取茶园空间分布。本文基于GEE云平台,快速获取覆盖福建省的Sentinel-1雷达影像、Sentinel-2光学影像及地形数据,从中提取光谱特征、纹理特征、地形特征等98个特征,利用递归消除支持向量机算法(SVM_RFE)对特征变量进行筛选,通过支持向量机分类器(SVM)进行茶园提取,首次得到福建省2019年10 m分辨率茶园种植区空间分布图。结果表明:①光谱特征在茶园信息提取中占据重要地位,纹理特征和地形特征次之;②利用SVM_RFE可以有效筛选出最有利于茶园提取的特征子集,有效提高提取精度,总体精度为94.65%,Kappa系数为0.93,茶园的生产者精度为91.64%,用户精度为92.91%;③基于Sentinel-1及Sentinel-2影像获取的福建省2019年茶园种植面积为1913 km^(2),主要分布在安溪县、福鼎市、福安市、武夷山市和寿宁县,其茶园总面积达910 km^(2),约占据全省茶园面积的48%。利用云计算技术可以克服大尺度茶园监测运算能力不足的问题,结合Sentinel-1和Sentinel-2影像能够较准确地提取福建省茶园分布,对南方丘陵山区茶园及其他作物提取具有参考价值,并为政府及有关部门进行茶园管理提供支持。