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Quantitative Analysis of Nutrient Minerals in Malagasy Rice Species by EDXRF and Dietary Intake Assessment EDXRF定量分析马达加斯加稻营养矿物质及日粮摄取量
Pub Date : 2019-10-23 DOI: 10.11648/J.AJAC.20190705.12
Herinirina Nomenjanahary Ravoson, M. Harinoely, N. N. Andriamahenina, Natolotriniavo Nomena Fitiavana Andrianirinamanantsoa, Elise Octavie Rasoazanany, Lucienne Voahangilalao Rakotozafy, R. Raboanary
The elemental analysis of rice samples sold in local market in Antananarivo are carried out at Institut National des Sciences et Techniques Nucleaires-Madagascar (INSTN-Madagascar) using Energy Dispersive X-Ray Fluorescence (EDXRF) spectrometer. The study aims to assess the nutritional and mineral elements contents of rice which is the staple dietary food for Malagasy people. The Malagasy rice is divided into three species according to its color: red, pink and white rice. Essential major elements namely sodium (Na), magnesium (Mg), phosphorus (P), chloride (Cl), potassium (K), calcium (Ca) and trace elements such as chromium (Cr), manganese (Mn), iron (Fe), copper (Cu), zinc (Zn), selenium (Se) and iodine (I) are quantitatively determined. The accuracy of the instrumental method and analytical procedures are checked by using the Reference Material IPE 135 (Rice sample) from the Wageningen Evaluating Programmes for Analytical Laboratory (WEPAL) in Netherland. The experimental values are in good agreement with the certified values because of a coefficient of determination R² of 0.999 and a recovery rate %R between 87% and 114%. The comparison of the elemental content of the studied rice samples with the Recommended Dietary Allowance (RDA) reveals that Red rice foods have sufficient capacity to provide adult male consumers with P, Mn, Mg, Fe, Cu and Zn. Certainly insufficient daily intake of Mg (55%), Fe (58%), Cu (89%) and Zn (79%) could be met by ingestion of vegetables and meats that are served as a side dish.
利用能量色散x射线荧光光谱仪对塔那那利佛当地市场销售的大米样品进行了元素分析,该分析是在马达加斯加国家核科学技术研究所进行的。该研究旨在评估大米的营养和矿物质元素含量,大米是马达加斯加人的主食。马达加斯加米根据颜色分为三种:红米、粉米和白米。定量测定必需的主元素即钠(Na)、镁(Mg)、磷(P)、氯(Cl)、钾(K)、钙(Ca)和微量元素如铬(Cr)、锰(Mn)、铁(Fe)、铜(Cu)、锌(Zn)、硒(Se)和碘(I)。仪器方法和分析程序的准确性通过使用来自荷兰瓦赫宁根分析实验室评估计划(WEPAL)的参考物质IPE 135(水稻样品)进行检查。测定系数R²为0.999,回收率%R在87% ~ 114%之间,实验值与鉴定值吻合较好。研究样品的元素含量与推荐膳食摄取量(RDA)的比较表明,红米食品有足够的能力为成年男性消费者提供P、Mn、Mg、Fe、Cu和Zn。当然每日摄入不足的镁(55%),铁(58%),铜(89%)和锌(79%)可以通过摄入蔬菜和肉类作为配菜来满足。
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引用次数: 2
Nutritional and Anti-nutritional Composition of Ximenia americana Fruit 美洲西米尼亚果实营养与抗营养成分研究
Pub Date : 2019-09-06 DOI: 10.11648/J.AJAC.20190704.13
A. Muhammad, Sayudi Yahaya Haruna, A. U. Birnin-Yauri, A. Muhammad, C. M. Elinge
In this work the nutritional and anti-nutritional composition of Ximenia americana fruit is investigate using standard analytical methods. The results of proximate analysis of the fruit on dry weight basis shows that it contains, Crude protein (7.26%), Crude lipid (13.0%), ash (10.5%), and moisture (64%Wet Weight), The pulp contains appreciable concentration of ascorbic acid (21.12 mg/100g). The mineral analysis, revealed that the pulp is rich in potassium (690mg/100g), magnesium (10.67mg/100g) phosphorus (4.48mg/100g), Calcium (0.65mg/100g) and sodium (45mg/100g). The analysis further revealed high content of Tannins (74.8mg/100g) and phytate (29.43mg/100g). This shows that the sample can serve as good source of mineral to both human and livestock.
本文采用标准分析方法对美洲西美尼亚果实的营养成分和抗营养成分进行了研究。果实干重的近似分析结果表明,其含有粗蛋白质(7.26%)、粗脂肪(13.0%)、灰分(10.5%)和水分(湿重64%),果肉中含有一定量的抗坏血酸(21.12 mg/100g)。矿物分析显示,果肉富含钾(690mg/100g)、镁(10.67mg/100g)、磷(4.48mg/100g)、钙(0.65mg/100g)和钠(45mg/100g)。进一步分析显示,单宁(74.8mg/100g)和植酸(29.43mg/100g)的含量较高。这表明该样品可以作为人类和牲畜的良好矿物来源。
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引用次数: 4
Extraction and Analysis of Spectral Properties and ChroMophoric Characterization of Natural Dye Extract from Barks of Terminalia brownii Fresen (Combretaceae) 龙葵树皮天然染料提取物的提取、光谱性质分析及显色性表征
Pub Date : 2019-09-04 DOI: 10.11648/J.AJAC.20190704.12
Maiyo Kimutai Bernard, M. L. Were, Kiprop Kipchumba Ambrose, M. Richard
Terminalia brownii is known for its medicinal properties has been used to treatment and management of malaria, ulcers, diarrhea, coughs, hepatitis etc. In Elgeyo-Marakwet County, and amongst the Marakwet community of Kenya, the plant has been known for its dyeing properties and has been used historically for the dyeing of traditional handbags locally known as “kiondos”. Literature evaluation indicates little is known concerning the dyeing properties of this plant, hence there was need for such work to be done. This coupled with the fact that there has been an attempted shift to natural dyes from their synthetic counterparts which are considered to be poisonous, allergens and in some cases carcinogenic. In this work, two extraction methods namely soxhlet and maceration were compared for their percentage yields with maceration being chosen as a preferred method. The extracts were then separated and identified via UV-VIS, FT-IR and LC-MS. Preliminarily the UV-Vis was used for identification of chromophores present in the dye extracts at maximum absorption (λ max) due to electron transitions from HOMO-LUMO whereas the FT-IR was used to identify the specific vibrational chemical bonds characteristic of the individual functional groups present in the dye extracts. LC-MS in tandem with collision induced dissociation (CID) was used to accurately identify and characterize the chromophoric compounds based on their structures, molecular (product ion) and fragmentation pattern which were then compared with LC-MS data, library and the literature. Several compounds with dyeing properties such as Catechin, Epi-Catechin, Baccatin, Gentianose, Geniposide and Genipin were identified. Gentianose, geniposide baccatin and genipin are being reported for the first time as chromophoric compounds in Terminalia brownii.
黄尾草因其药用价值而闻名,已被用于治疗和管理疟疾、溃疡、腹泻、咳嗽、肝炎等。在Elgeyo-Marakwet县,以及肯尼亚的Marakwet社区,该工厂以其染色性能而闻名,历史上一直用于当地称为“kiondos”的传统手袋的染色。文献评价表明,对该植物的染色特性了解甚少,因此有必要做这样的工作。再加上人们试图从合成染料转向天然染料,这些合成染料被认为是有毒的、过敏原的,在某些情况下还会致癌。在这项工作中,比较了两种提取方法即索氏法和浸渍法的提取率,并选择浸渍法为首选方法。通过UV-VIS、FT-IR和LC-MS对提取物进行分离鉴定。初步采用紫外可见光谱(UV-Vis)鉴定染料提取物中存在的最大吸收(λ max)的发色团,这是由于HOMO-LUMO的电子跃迁,而傅里叶红外光谱(FT-IR)用于鉴定染料提取物中存在的单个官能团的特定振动化学键特征。采用碰撞诱导解离(CID)串联LC-MS技术,根据化合物的结构、分子(产物离子)和断裂模式对其进行准确鉴定和表征,并与LC-MS数据、文库和文献进行比较。鉴定了几种具有染色性能的化合物,如儿茶素、儿茶素、茶素、龙胆糖、京尼平苷和龙胆平。龙胆糖、京尼平苷和龙胆平均为首次报道的发色性化合物。
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引用次数: 1
Physicochemical Characterization and Evaluation of Castor Oil (R. communis) for Hair Biocosmetics 头发生物化妆品用蓖麻油的理化性质及评价
Pub Date : 2019-07-30 DOI: 10.11648/J.AJAC.20190704.11
S. Tessema
This study reports the characterization of oil from Castor (Ricinus Communius L) seed oil. The biocosmetic potential of the castor oil was evaluated for hair through physico-chemical characterization. The various physicochemical parameters (iodine value, pH value, specific gravity, refractive index, peroxide value, etc) were tested in accordance with American standard testing method specifications and compared with argan oil. Accordingly, the parameters tested comply with some journals dealing with cosmetics. Biocosmetic has high potential as a raw material for synthetic cosmetics or blend stock substitution for cosmetics without any modification. The advantage of castor oil over other oils (sunflower, olive, soy bean, corn) would lie in the oil price.
本研究报道了蓖麻籽油的特性。通过理化性质评价蓖麻油对头发的生物美容潜力。按照美国标准测试方法规范对其各项理化参数(碘值、pH值、比重、折射率、过氧化值等)进行测试,并与摩洛哥坚果油进行比较。因此,测试的参数符合一些化妆品杂志。生物化妆品作为不经任何改性的合成化妆品或混合原料替代化妆品具有很大的潜力。蓖麻油相对于其他油(向日葵、橄榄油、大豆油、玉米油)的优势在于油价。
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引用次数: 0
Determination of Short Chain Chlorinated Paraffins in Textile Samples by GC-MS 气相色谱-质谱法测定纺织样品中的短链氯化石蜡
Pub Date : 2019-07-08 DOI: 10.11648/J.AJAC.20190703.14
Zenghui Zheng, Shao Yuwan, L. Xian, Du Juan
The method of determining short-chain chlorinated paraffins in textiles by GC-MS was established. Short-chain chlorinated paraffins, short for SCCPs, are a mixture of polychlorinated n-alkanes. These high production volume chemicals are widely used as leather coating, plasticizers for PVC and chlorinated rubber and flame retardants for plastics and textile. Due to their toxicity, as well as capacity for bioaccumulation and persistence in the environmental residue, SCCPs have become an obviously environmental issue. The current analytical equipment combination are very expensive and require a lot of laboratory space and advanced skills for operation, a ready-to-use commercially available method with relatively short time and satisfactory sensitivity urge to be established. In this new method, samples were extracted by n-hexane under ultrasonic followed by concentration and constant-volume and then identified by GC-MS and quantified by external standard method. With this method, a good linear relationship was found between 5 μg/mL ~30μg/mL with a linear correlation coefficient (R2) above 0.995. The detection limit for SCCPs by this method was found to be as low as 10mg/kg. The recoveries of SCCPs in textiles at three levels which covers low, media and high concentration ranges are ranged from 82.3% to 106.9% with relative standard deviation (RSD) of 3.41%~7.61%(RSD, N = 6).
建立了用气相色谱-质谱法测定纺织品中短链氯化石蜡的方法。短链氯化石蜡,简称SCCPs,是多氯化正构烷烃的混合物。这些大批量生产的化学品广泛用于皮革涂料,PVC和氯化橡胶的增塑剂以及塑料和纺织品的阻燃剂。由于其毒性,以及在环境残留物中的生物蓄积性和持久性,短链氯化石蜡已成为一个明显的环境问题。目前的分析设备组合非常昂贵,需要大量的实验室空间和先进的操作技能,迫切需要建立一种时间相对较短且灵敏度令人满意的即用型商业可用方法。该方法采用超声正己烷萃取、定容浓缩、气相色谱-质谱鉴别、外标法定量的方法。该方法在5 μg/mL ~30μg/mL之间存在良好的线性关系,线性相关系数(R2)均在0.995以上。该方法对短链氯化石蜡的检出限低至10mg/kg。在低、中、高浓度3个浓度范围内,纺织品中SCCPs的回收率为82.3% ~ 106.9%,相对标准偏差(RSD)为3.41%~7.61%(RSD, N = 6)。
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引用次数: 0
Synthesis and Microbial Activity of Manganese (II) and Cobalt (III) Complexes of 3-Methoxy-4-Hydroxyphenylmethyelene (2- Hydroxyphenyl) Amine 3-甲氧基-4-羟基苯基甲基(2-羟基苯基)胺锰(II)和钴(III)配合物的合成及微生物活性
Pub Date : 2019-06-26 DOI: 10.11648/J.AJAC.20190703.13
Belachew Kebede
Transition metal complexes of Mnanganese (II) and Cobalt (III) were synthesized from the Schiff’s base ligand, 3-methoxy-4-hydroxyphenylmethyelene (2-hydroxyphenyl) amine which is derived from vanillin and 2-aminohpenol by the reaction of the metal ions. The Structural features of these complexes were obtained from their elemental analyses, magnetic susceptibility, molar conductance, FT-IR, electronic spectra, and Atomic Absorption Spectroscopic studies. In order to study the binding modes of the ligand (Schiff’s base) with metal ions in the complexes, the FT- IR spectrum of the free ligand was compared with the spectra of its complexes. The spectral data suggest the involvement of phenolic oxygen and azomethane nitrogen in coordination to the central metal ions. On the basis of spectral studies and magnetic susceptibility measurements, an octahedral geometry has been assigned for both complexes. The free ligand and its metal complexes were tested in vitro against bacteria (Escherichia coli, Staphylococcus aureus) and fungi (Aspergillus Niger, Colletotricum) in order to assess their antimicrobial activities. And the results indicated that all compounds are effective against both tested bacteria and fungi though their effects are dose dependent. The free ligand showed higher activities than its complexes in both bacteria and fungi case, which suggests the promising potential of the ligand for both bacterial and fungi test.
以香兰素和2-氨基苯酚为原料,由希夫碱配体3-甲氧基-4-羟基苯基甲基(2-羟基苯基)胺与金属离子反应,合成了锰(II)和钴(III)的过渡金属配合物。这些配合物的结构特征通过元素分析、磁化率、摩尔电导、红外光谱、电子光谱和原子吸收光谱研究得到。为了研究配合物中配体(希夫碱)与金属离子的结合方式,将自由配体的FT- IR光谱与其配合物的光谱进行了比较。光谱数据表明酚氧和偶氮甲烷氮与中心金属离子配合。在光谱研究和磁化率测量的基础上,这两种配合物都具有八面体的几何形状。对游离配体及其金属配合物进行了体外抑菌试验,考察其对细菌(大肠杆菌、金黄色葡萄球菌)和真菌(黑曲霉、炭疽菌)的抑菌活性。结果表明,所有化合物对细菌和真菌都有效,但其作用是剂量依赖性的。游离配体在细菌和真菌中均表现出比其配合物更高的活性,这表明该配体在细菌和真菌检测中都具有广阔的应用前景。
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引用次数: 1
Corrosion Inhibition of Mild Steel in Sulphuric Acid (H2SO4) Medium of the Stem Extract of Tetrapleura Tetraptera 四翅草茎提取物在硫酸(H2SO4)介质中对低碳钢的缓蚀作用
Pub Date : 2019-06-17 DOI: 10.11648/J.AJAC.20190703.12
Rita Oghenenyerhovwo Ididama, V. Ajiwe, C. N. Emeruwa
The inhibitive action of stem extracts of Tetrapleura tetraptera on mild steel corrosion in 1.0M & 5.0M H2SO4 solutions was studied. The stem were dried under room temperature and mechanically ground into powder form. 100g of the stem powder were extracted with a mixture of methanol/water in the ratio of 4:1 using a Soxhlet extractor for 24 hours. The extracts were distilled at 60°C in a water bath until almost the entire methanol evaporated. 4.0g of the methanol extracts were digested in 1000ml of 1M H2SO4 and 5M H2SO4 and left to cool for 24 hours and the resulting solution was filtered and stored in a 1.0L volumetric flask. The stem extracts test solutions were prepared from the stock solution by dissolving 0.5g/L, 1.0g/L, 2.0g/L and 4.0g/L of the extracts in 1L solution of 1M H2SO4 and 5M H2SO4. Phytochemical analysis was carried out and the result showed the presence of some secondary metabolites such as alkoliods, flavonoids, steroids, saponins and tannins. Weight loss (gravimetric) and gasometric techniques were used to determine the inhibition action of the stem of Terapleaura tetraptera. The results showed that stem of Tetrapleura tetraptera can function as good corrosion inhibitor in acid medium. Inhibition efficiencies (%I) of the stem of Tetrapleura tetraptera extracts was found to reach 73.69% & 50.39% for 1.0M H2SO4 while for 5.0M was 83.31% & 79.54% for gravimetric and gasometric analyses respectively. The corrosion inhibition efficiency increased with increase in the concentration of the extracts and decreased with the increase in time and temperature. The corrosion inhibition efficiency exhibited by the Tetrapleura tetraptera stem extracts is attributed to the stronger adsorption of the phytochemicals present in the plant extracts unto the mild steel. The mechanism of adsorption proposed for the Tetrapleura tetraptera stem extracts is physical adsorption. The corrosion inhibition of the stem of Tetrapleura tetraptera extracts followed Langmuir, Tempkin and Freundlich adsorption isotherm for both 1.0M & 5.0M H2SO4.
研究了四翅木茎提取物在1.0M和5.0M H2SO4溶液中对低碳钢的腐蚀抑制作用。茎在室温下干燥,机械磨成粉末。取茎粉100g,用索氏提取器用甲醇/水的混合物以4:1的比例提取24小时。提取液在60°C的水浴中蒸馏,直到几乎全部甲醇蒸发。取4.0g甲醇提取物于1000ml 1M H2SO4和5M H2SO4中消化,冷却24小时,过滤后保存于1.0L容瓶中。从原液中提取0.5g/L、1.0g/L、2.0g/L、4.0g/L的提取物,分别溶于1M H2SO4和5M H2SO4的1L溶液中,制备茎提取物试验溶液。植物化学分析结果表明,其次生代谢产物有生物碱、黄酮类化合物、类固醇、皂苷和单宁等。采用失重法(重量法)和气相法测定了四翅天牛茎的抑菌作用。结果表明,四翅蕨茎在酸性介质中具有良好的缓蚀剂作用。在1.0M H2SO4条件下,四胸草提取物茎部的抑制率(%I)分别为73.69%和50.39%,在5.0M H2SO4条件下,其抑制率分别为83.31%和79.54%。缓蚀效果随浸提液浓度的增加而增加,随浸提液时间和温度的增加而降低。四翅草茎提取物具有较好的缓蚀性能,主要是由于其对低碳钢具有较强的吸附作用。提出了四翅草茎提取物的吸附机制为物理吸附。四翅木提取物对1.0M和5.0M H2SO4的缓蚀作用均遵循Langmuir、Tempkin和Freundlich吸附等温线。
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引用次数: 0
The Application of NIR Process Analytical Chemistry in Studying Competitive Adsorption Process 近红外过程分析化学在竞争吸附过程研究中的应用
Pub Date : 2019-06-13 DOI: 10.11648/J.AJAC.20190703.11
Hong-wei Yang, C. Cai, Lu Xu, Lun Li, Yanzhao Zou, Yong-Yuan Tao, Mei-Qiong Wen
With an experimental setup of near-infrared process analytical chemistry, a competitive adsorption process of orthoxylene and aniline vapor onto silica gel has been revealed in the paper. The mixture vapor of orthoxylene and aniline has been introduced into a quartz adsorption bed, which was filled with adsorbent of silica gel and monitored continuously by a near-infrared spectrometer. Based on near-infrared spectra recorded during the adsorption process and chemometrics methodologies, the competitive adsorption process has been studied completely as well as clearly: 1) at about 62 minutes the adsorption achieved its equilibrium or stable state with aniline concentration of 0.22 g/g, and without any orthoxylene; 2) othoxylene was adsorbed first, but then rapidly replaced by aniline; 3) the adsorption of aniline resulted from the hydrogen bonds between aniline’s amino groups and silica gel’s silanol groups while that of orthoxylene was due to physical adsorption; 4) aniline was adsorbed vertically on the silica gel but orthoxylene laid evenly; 5) some surface of silica gel was more active for adsorption than others.
本文利用近红外分析化学实验装置,揭示了邻二甲苯和苯胺蒸气在硅胶上的竞争吸附过程。将邻二甲苯和苯胺的混合蒸汽引入石英吸附床,在床内填充硅胶吸附剂,用近红外光谱仪对其进行连续监测。基于近红外光谱记录和化学计量学方法,对竞争吸附过程进行了全面而清晰的研究:1)在约62 min时,吸附达到平衡或稳定状态,苯胺浓度为0.22 g/g,不含邻二甲苯;2)先吸附邻二甲苯,然后迅速被苯胺取代;3)苯胺的吸附是由于苯胺的氨基与硅胶的硅醇基团之间的氢键,而邻二甲苯的吸附是由于物理吸附;4)苯胺垂直吸附在硅胶上,邻二甲苯均匀分布;5)硅胶的某些表面吸附活性较强。
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引用次数: 0
Inhibitory Action of Methanol Leaf Extract of Irvingia Gabonensis on the Corrosion of Mild Steel in H2SO4 加蓬树甲醇叶提取物对低碳钢在H2SO4中腐蚀的抑制作用
Pub Date : 2019-06-12 DOI: 10.11648/J.AJAC.20190702.15
V. Ajiwe, Chinedu Ejike
The corrosion inhibition efficiency of methanol leaf extracts of Irvingia gabonensis for mild steel in 0.4, 0.5, 0.6 and 2.5M H2SO4 was investigated using weight loss and gasometric techniques in other to determine the phytochemical components of the crude leaf extract, the corrosion inhibition potential of the leaf extract, the thermodynamic parameters that aided the corrosion inhibition, the adsorption isotherm of the corrosion inhibition of the extracts using the Langmuir and Freundlich models and investigate the kinetics of the corrosion inhibition process. Preliminary phytochemical screening revealed the presence of tannins, saponnins, flavonoids, terpenes and alkaloids. From the results, the corrosion rates decreased with increase in inhibitor concentration. The maximum inhibition efficiency of 58.71% was obtained at extract concentration of 0.6g/L in 0.4M H2SO4 at 303K, 41.83% at extract concentration of 0.6g/L at 303K in 0.5M H2SO4 and 57.33% at extract concentration of 0.6g/L in 0.6M H2SO4 at 303K, for the gravimetric technique. In 2.5M H2SO4, maximum inhibition efficiency for the gasometric technique was 53.53% in 0.6g/L inhibitor concentration at 303K and for the gravimetric technique, the maximum inhibition efficiency was 29.42% in 0.6g/L inhibitor concentration at 303K. The kinetic and thermodynamic studies showed that activation energy (Ea) in the presence of inhibitor is greater than in the absence of inhibitor. From the Ea and ∆Goads values obtained, a physical adsorption mechanism was proposed. The Langmuir isotherm was found to show better correlation (R2) at lower temperature while the Freundlich isotherm had better correlation at higher temperature.
采用失重法和气相法研究了加蓬树甲醇叶提取物在0.4、0.5、0.6和2.5M H2SO4中对低碳钢的缓蚀效果,测定了粗叶提取物的植物化学成分、叶提取物的缓蚀电位、有助于缓蚀的热力学参数。采用Langmuir和Freundlich模型计算了提取物的缓蚀吸附等温线,并研究了缓蚀过程的动力学。初步的植物化学筛选显示其含有单宁、皂苷、黄酮类化合物、萜烯和生物碱。结果表明,随着缓蚀剂浓度的增加,腐蚀速率降低。重量法中,萃取液浓度为0.6g/L,萃取液浓度为0.4M H2SO4,萃取液浓度为303K,萃取液浓度为0.6g/L,萃取液浓度为0.5M H2SO4,萃取液浓度为303K,萃取液浓度为41.83%,萃取液浓度为0.6g/L,萃取液浓度为0.6M H2SO4,萃取液浓度为303K,萃取液浓度为57.33%。在2.5M H2SO4中,当缓蚀剂浓度为0.6g/L、303K时,气相法的最大缓蚀率为53.53%;当缓蚀剂浓度为0.6g/L、303K时,重量法的最大缓蚀率为29.42%。动力学和热力学研究表明,有抑制剂时的活化能大于无抑制剂时的活化能。根据得到的Ea和∆Goads值,提出了物理吸附机理。Langmuir等温线在较低温度下具有较好的相关性(R2), Freundlich等温线在较高温度下具有较好的相关性(R2)。
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引用次数: 0
Synthesis, Characterisation and Acetylcholinesterase Inhibition Activity of Nickel(II) and Copper(II) Complexes of 3-Hydroxybenzaldehyde-4-nitrobenzoic Acid Hydrazone 3-羟基苯甲醛-4-硝基苯甲酸腙镍(II)和铜(II)配合物的合成、表征及乙酰胆碱酯酶抑制活性
Pub Date : 2019-05-27 DOI: 10.11648/J.AJAC.20190702.14
T. A. Ajayeoba, O. Akinyele, A. O. Ayeni, I. Olawuni
A new ligand namely 3-hydroxybenzaldehyde-4-nitrobenzoic acid hydrazone, its Nickel(II) and Copper(II) complexes were synthesised and characterised by spectroscopic methods: 1H NMR, Infrared (IR), UV-Vis, magnetic susceptibility measurement and % metal analysis. 1H NMR spectroscopy showed the diagnostic N-H signal at 12.10 ppm indicating the formation of the ligand. Infrared spectra showed that the ligand coordinated to the metal ion in keto form through the carbonyl oxygen (C=O) and the azomethine nitrogen (C=N). The UV-Vis spectrum of the ligand displayed two prominent bands at 47169 cm-1 and 30303 cm-1 which were ascribed to the intraligand transitions of π-π*, and n-π* respectively. These bands had hypsochromic shifts in the metal complexes indicating coordination with the metal ion. The nickel complex had a magnetic moment of 2.92 B.M, suggesting an octahedral geometry, while the copper complex had a value of 1.65 B.M. which is close to the expected value for a d9 copper(II) complex with possibility antiferromagnetic interactions. The % metal calculated had a good agreement with the observed values. The acetylcholinesterase inhibition activity of the ligand measured was 190 ± 20 μg/mL compared to the standard Eserin that had 68 ± 1.13 μg/mL. The copper(II) complex had a value of 220 ± 20 μg/mL, while the Nickel(II) complex had the least inhibitory value at 390 ± 80 μg/mL. The compounds could serve as primary target in the study of acetylcholinesterase inhibitors
合成了一种新的配体- 3-羟基苯甲醛-4-硝基苯甲酸腙及其镍(II)和铜(II)配合物,并通过1H NMR、IR、UV-Vis、磁化率测定和%金属分析等光谱方法对其进行了表征。1H NMR在12.10 ppm时显示诊断性N-H信号,表明配体形成。红外光谱表明,配体通过羰基氧(C=O)和亚甲基氮(C=N)与酮态金属离子配位。该配体的紫外可见光谱在47169 cm-1和30303 cm-1处显示出两个突出的波段,分别归因于配体内π-π*和n-π*的跃迁。这些波段在金属配合物中有异色移位,表明与金属离子的配位。镍配合物的磁矩为2.92 B.M,表明其为八面体,而铜配合物的磁矩为1.65 B.M,接近于d9铜(II)配合物的预期磁矩,可能存在反铁磁相互作用。计算的金属含量与实测值吻合较好。该配体对乙酰胆碱酯酶的抑制活性为190±20 μg/mL,而标准配体的抑制活性为68±1.13 μg/mL。铜(II)配合物的抑制值为220±20 μg/mL,镍(II)配合物的抑制值最低,为390±80 μg/mL。这些化合物可作为研究乙酰胆碱酯酶抑制剂的主要靶点
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引用次数: 3
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American Journal of Applied Chemistry
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