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Development and validation of valganciclovir hydrochloride in bulk and pharmaceutical dosage form by HPTLC method 高效液相色谱法研究盐酸缬更昔洛韦原料药和药剂剂的研制与验证
Pub Date : 2020-09-19 DOI: 10.14419/ijac.v8i2.30926
K. K, J. Gnana Babu C., Sowmya H.G
A simple, rapid and accurate High performance thin layer chromatography is described for the Development and validation of HPTLC method for Valganciclovir Hydrochloride in bulk and Pharmaceutical dosage form. The separation is carried out on Merck TLC aluminum sheets of silica gel 60 F254 using Chloroform: Methanol: Ammonia (6.5:3.4:0.1v/v) mobile phase. Quantification was done by Densitometric scanning at 254nm. The linearity was found to be the range of 100-500ng/spot for Valganciclovir hydrochloride with the correlation coefficient of 0.9993. The regression equation was found to be Y=10.168x-94.8. The Rf value of Valganciclovir hydrochloride was found to be 0.74. The LOD and LOQ were found to 9.19 and 27.87 respectively. Average recovery was found to be 99.66% which show that the method was free from interference from excipients present in the formulation. Simultaneously the Percentage relative standard deviation was well within the range of 2%. The above method was validated according to the ICH guidelines. The established method enabled accurate, precise and applied to the analysis of Valganciclovir hydrochloride in bulk and Pharmaceutical dosage form.  
建立了一种简便、快速、准确的高效薄层色谱法,并对盐酸缬更昔洛韦原料药和制剂的hplc法进行了验证。采用三氯甲烷:甲醇:氨(6.5:3.4:0.1v/v)流动相,在默克薄层色谱法硅胶60f254铝板上进行分离。定量采用254nm密度扫描。盐酸缬更昔洛韦在100 ~ 500ng/点范围内呈线性关系,相关系数为0.9993。回归方程为Y=10.168x-94.8。盐酸缬更昔洛韦的Rf值为0.74。LOD和LOQ分别为9.19和27.87。平均回收率为99.66%,表明该方法不受制剂中辅料的干扰。同时,相对标准偏差在2%的范围内。上述方法根据ICH指南进行了验证。所建立的方法准确、精密度高,适用于原料药和制剂剂型盐酸缬更昔洛韦的分析。
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引用次数: 1
Molecular interaction on imidazolium based ionic liquids and serum albumin: A spectroscopy approach 咪唑类离子液体与血清白蛋白的分子相互作用:光谱学方法
Pub Date : 2020-09-19 DOI: 10.14419/ijac.v8i2.30994
Manoj Kumar Banjare, Ramesh Kumar Banjare, Kallol Kumar Ghosh
Interaction between globular proteins with imidazolium based ionic liquids (ILs) is extremely significant considering that of the vast use of ILs, since protein stabilizer in the current years. The present work, the interaction of human serum albumin (HSA) and bovine serum albumin (BSA) with 1-butyl-3-methylimidazolium octylsulphate (BmimOS) and 1-decyl-3-methylimidazolium tetrafluoroborate (DmimBF4) have been examine the use of fluorescence and FTIR. Fluorescence spectra of HSA/BSA are extinguished by BmimOS /DmimBF4 ILs by way of the dynamic method. The various thermodynamic parameters were revealing that very susceptible interactions exist between HSA/BSA and BmimOS /DmimBF4. The conformational adjustments of HSA/BSA were observed by means of FTIR analysis. Fluorescence methods were completed to find out about the thermal balance of HSA/BSA at different temperature. The thermal balance of BSA in the presence of ILs follows the style BmimOS/DmimBF4 and presence of extra hydrophobic IL, decay increases swiftly as a characteristic of concentration.  
考虑到近年来咪唑类离子液体作为蛋白质稳定剂的广泛应用,球状蛋白与离子液体之间的相互作用是非常重要的。本文利用荧光和红外光谱研究了人血清白蛋白(HSA)和牛血清白蛋白(BSA)与1-丁基-3-甲基咪唑辛基硫酸酯(BmimOS)和1-癸基-3-甲基咪唑四氟硼酸酯(DmimBF4)的相互作用。BmimOS /DmimBF4 il通过动态方法熄灭HSA/BSA的荧光光谱。各种热力学参数显示HSA/BSA与BmimOS /DmimBF4之间存在非常敏感的相互作用。FTIR分析观察了HSA/BSA的构象调整。采用荧光法测定不同温度下HSA/BSA的热平衡。在IL存在的情况下,BSA的热平衡遵循BmimOS/DmimBF4的模式,并且存在额外的疏水IL,作为浓度的特征,衰变迅速增加。
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引用次数: 4
Optimization of groundnut shell fast pyrolysis for the production and characterization of bio-oil using fabricated fixed bed reactor 花生壳快速热解制备生物油的工艺优化及固定式反应器表征
Pub Date : 2020-09-19 DOI: 10.14419/ijac.v8i2.31050
Ige Ayodeji Rapheal, Elinge Cosmos Moki, A. Muhammad, G. Muhammed, Lawal Gusau Hassan
Renewable plant materials are regarded as one of the most affirmative option for the production of fuels and chemicals. With the concept of pyrolysis process, there is every possibility to produce alternative sources of energy and fuels from renewable biomass. The study depicts the production, optimization and characterization of bio-oil from pyrolyzed groundnut shell using fabricated reactor. The pyrolysis process was produced with bio-oil response, bio-char response and non condensable gases response as products. The effect of pyrolysis variables were observed by the production of the bio-oil as the response. Sixty runs of pyrolysis experiments were suggested by box Benkhen design indicated optimum pyrolysis condition at particle size of 1.15mm mesh, reaction time of 83 mins and temperature of 650oC. The maximum bio-oil yield was obtained with 33.91% at optimum condition. The bio-oil samples had better performance which met the specifications for the measured properties and compares well with the ASTM standard. Therefore, using groundnut shell for bio-oil production via pyrolysis process can serve as an approach of providing a sustainable alternative source of fuel and friendly environment.  
可再生植物材料被认为是生产燃料和化学品的最肯定的选择之一。有了热解过程的概念,从可再生生物质中生产替代能源和燃料是完全可能的。介绍了利用自制反应器从花生壳热解制备生物油的工艺、优化及表征。热解过程以生物油反应、生物炭反应和不凝性气体反应为产物。以生物油的生产为响应,观察热解变量的影响。通过box Benkhen设计,共进行60次热解实验,得出最佳热解条件为:粒径为1.15mm,反应时间为83 min,温度为650℃。在最佳条件下,生物油收率最高达33.91%。所制备的生物油样品具有较好的性能,满足了测定性能的要求,与ASTM标准比较良好。因此,利用花生壳热解生产生物油可以作为一种可持续的替代燃料来源和环境友好的方法。
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引用次数: 2
Development and validation of HPTLC method for the estimation of cefadroxil in bulk and tablet dosage form 高效液相色谱法测定头孢地洛西原料药和片剂含量的建立与验证
Pub Date : 2020-09-02 DOI: 10.14419/ijac.v8i2.30963
Kirankumar S V, J. Gnana Babu C., S. H G
A novel and simple HPTLC method has been developed for the estimation of Cefadroxil (CFD) in bulk and pharmaceutical dosage form on silica gel precoated aluminum 60F254 plates, (10 cm x10 cm) with 0.25 mm thickness. The separation was carried out using ethyl acetate: chloroform (8:2v/v) as mobile phase. The Chromatographic scanning was carried out at 254 nm. The Rf (± SD) values were found to be 0.38 ± 0.05 for CFD. The linearity for analyte was in the range 100-500 ng/band for CFD with correlation coefficients, r2 = 0.9996. The percentage recovery obtained for CFD was in the range of 99.28-100.13% respectively. The proposed method was optimized and validated as per the ICH guidelines17.  
建立了一种新型、简便的高效液相色谱法,用于在厚度为0.25 mm、硅胶预涂60F254铝板(10 cm × 10 cm)上对头孢地洛辛(CFD)散装和药用剂型进行定量分析。以乙酸乙酯:氯仿(8:2v/v)为流动相进行分离。在254 nm处进行色谱扫描。计算所得的Rf(±SD)值为0.38±0.05。分析物在100 ~ 500 ng/波段内线性良好,相关系数r2 = 0.9996。CFD的回收率分别为99.28 ~ 100.13%。根据ICH指南对该方法进行了优化和验证。
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引用次数: 0
Development and validatation of HPTLC method for estimation of irbesartan in bulk and tablet dosage form 厄贝沙坦片剂和散装剂型hplc法的建立与验证
Pub Date : 2020-08-04 DOI: 10.14419/ijac.v8i1.30800
Yogeesh C S, S. H G, J. Gnana Babu C.
A simple, rapid and accurate High performance thin layer chromatography is described for the Development and validation of HPTLC method for Irbesartan in bulk and Pharmaceutical dosage form. The separation is carried out on Merck TLC aluminum sheets of silica gel 60 F254 using Ethyl acetate: Chloroform (6.5:3.5v/v) mobile phase. Quantification was done by Densitometric scanning at 254nm. The linearity was found to be the range of 100-500ng/spot for Irbesartan with the correlation coefficient of 0.9992. The regression equation was found to be Y=7.2733x+703.15. The Rf value of Irbesartan was found to be 0.55. The LOD and LOQ were found to 8.24 and 24.74 respectively. Average recovery was found to be 99.66% which show that the method was free from interference from excipients present in the formulation. Simultaneously the Percentage relative standard deviation was well within the range of 2%. The above method was validated according to the ICH guidelines. The established method enabled accurate, precise and applied to the analysis of Irbesartan in bulk and Pharmaceutical dosage form.  
建立了一种简便、快速、准确的高效薄层色谱法,用于厄贝沙坦散装和药用剂型的hplc分析。采用醋酸乙酯:氯仿(6.5:3.5v/v)流动相,在默克薄层色谱法硅胶60f254铝板上进行分离。定量采用254nm密度扫描。厄贝沙坦在100 ~ 500ng/spot范围内呈线性关系,相关系数为0.9992。回归方程为Y=7.2733x+703.15。厄贝沙坦的Rf值为0.55。LOD和LOQ分别为8.24和24.74。平均回收率为99.66%,表明该方法不受制剂中辅料的干扰。同时,相对标准偏差在2%的范围内。上述方法根据ICH指南进行了验证。所建立的方法准确、精密度高,适用于厄贝沙坦原料药和制剂剂型的分析。
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引用次数: 0
Hydride generation atomic fluorescence spectrometry (HG-AFS) determination of total arsenic in lipstick 氢化物发生原子荧光光谱法测定口红中总砷
Pub Date : 2020-07-25 DOI: 10.14419/ijac.v8i1.30889
M. E. Ghanjaoui, I. Adraoui, A. Gammoun, L. Cervera, M. El Rhazi, M. de la Guardia
This study aimed to determine the total arsenic concentration in lipsticks and evaluate the potential health risks due to daily ingestion of this toxic element from this product. The samples were analyzed using atomic fluorescence spectrometry technique after mineralization and hydride generation (HG-AFS). The calibration curve is linear over a concentration range from 0.125 to 2 µg L-1 with a regression coefficient of the order of 0.9899. The limit of detection is reaches 3 ng g-1. The standard deviation is of the order of 4%.The accuracy of this method was evaluated by calculating the recoveries of additions of arsenic to three lipstick samples. These results indicate recovery rates between 91% and 98%. Finely, the results found demonstrate that the method used in this work is suitable for arsenic detection in lipsticks samples.  
本研究旨在确定口红中砷的总浓度,并评估每日从该产品中摄入这种有毒元素所带来的潜在健康风险。矿化和氢化物生成后,采用原子荧光光谱法(HG-AFS)对样品进行分析。在0.125 ~ 2µg L-1的浓度范围内,校正曲线呈线性,回归系数为0.9899数量级。检测限为3 ng g-1。标准差约为4%。通过计算三种口红样品中砷的添加回收率,评价了该方法的准确性。结果表明,回收率在91% ~ 98%之间。结果表明,本方法适用于口红样品中砷的检测。
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引用次数: 0
The nutritional potentials and the fatty acid profile of the seed and seed oil of Caesalpinia bonducella 山葵种子及籽油的营养潜力及脂肪酸谱
Pub Date : 2020-07-25 DOI: 10.14419/ijac.v8i1.26278
A. Adeniyi, Sulaiman Wasiu Kayode, Akinyode Olakunle Abayomi
The physicochemical properties of the seed and fatty acid profile of the seed oil of Caesalpinia bonducella were analyzed in this study, using standard methods of the Association of Official Analytical Chemists (AOAC). The proximate composition was found as follows: Moisture (3.24%), crude fat (41.76%), crude protein (28.63%), crude fibre (4.35%), ash content (2.94%) and carbohydrate (19.08%). The total unsaturated fatty acids (57.36%) was more abundant than the total saturated ones (42.68%). The seed oil had a high level of linoleic acid (28.15%), followed by oleic (18.41%), stearic (13.83%) and palmitic (13.56%). Other fatty acids had less than 10% each. There was a high level of unsaturation (57.36%) with oleic and linoleic acids dominating all other fatty acids with a total of 46.56%. The percentage of essential fatty acids (linoleic & linolenic acids) (32.96%) was also high at about ⅓ of the total oil content. The total poly-unsaturated fatty acids (36.99%) was higher than those of mono-unsaturated (20.37%). The high level of poly-unsaturated fatty acids in the oil sample is an advantage as these are essential components of the diet of man. The good total unsaturated/saturated (or P/S) ratio of the oil, (i.e.1.344), makes it to be very nutritionally useful if adopted for domestic purposes.  
本文采用美国官方分析化学家协会(AOAC)的标准方法,对山葵种子的理化性质和籽油的脂肪酸谱进行了分析。其近似组成为:水分(3.24%)、粗脂肪(41.76%)、粗蛋白质(28.63%)、粗纤维(4.35%)、灰分(2.94%)、碳水化合物(19.08%)。总不饱和脂肪酸(57.36%)高于总饱和脂肪酸(42.68%)。种子油中亚油酸含量最高(28.15%),其次是油酸(18.41%)、硬脂酸(13.83%)和棕榈酸(13.56%)。其他脂肪酸的含量都不到10%。不饱和脂肪酸占57.36%,其余脂肪酸以油酸和亚油酸为主,占46.56%。必需脂肪酸(亚油酸和亚麻酸)的比例也很高(32.96%),约占总油含量的1 / 3。多不饱和脂肪酸(36.99%)高于单不饱和脂肪酸(20.37%)。油样中多不饱和脂肪酸含量高是一个优势,因为这些是人类饮食的重要组成部分。这种油的总不饱和/饱和(或P/S)比(即1.344)很好,如果用于家庭用途,它的营养价值很高。
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引用次数: 0
Quantum chemical analysis of harmful dye 3-[ (4-anilinophenyl) diazenyl] benzenesulfonate, metanil yellow 有害染料3-[(4-苯胺苯基)二氮基]苯磺酸甲胺黄的量子化学分析
Pub Date : 2020-07-25 DOI: 10.14419/ijac.v8i1.30753
Shreyas Parbat
In the present work, quantum chemical study of the harmful dye, metanil yellow is conducted. The optimized molecular geometry and harmonic vibrational frequencies of metanil yellow were calculated by DFT-B3LYP method with LANL2DZ basis set. The vibrational assignments were performed on the basis of the potential energy distribution (PED) of the vibrational modes. Infrared spectra and Bulk Raman spectra were also obtained and characteristic peaks for the title compound were studied. The nonlinear optical properties of the title compound were calculated and discussed. Dipole moment, polarizability and first-order hyperpolarizability of the title compound were reported in order to study nonlinear optical properties (NLO). HOMO-LUMO energy levels were also computed in order to get the bandgap energy. Global reactivity descriptors were calculated using the HOMO and LUMO to predict compound reactivity. UV–Vis spectrum of the title compound was calculated using TD–DFT method. The molecular orbital contributions were studied by density of states (DOSs). Mulliken atomic charges and atomic polar tensors (APT) on each atom were tabulated. A discussion of the vibrational energy of each mode is also presented in this article.   
本文对有害染料金属黄进行了量子化学研究。在LANL2DZ基集上,用DFT-B3LYP方法计算了金属黄优化后的分子几何结构和谐波振动频率。根据振动模态的势能分布(PED)进行了振动赋值。获得了该化合物的红外光谱和体拉曼光谱,并对其特征峰进行了研究。对标题化合物的非线性光学性质进行了计算和讨论。本文报道了该化合物的偶极矩、极化率和一阶超极化率,以研究其非线性光学性质。为了得到带隙能量,还计算了HOMO-LUMO能级。利用HOMO和LUMO计算了整体反应性描述符,预测了化合物的反应性。采用TD-DFT方法计算了标题化合物的紫外可见光谱。用态密度(DOSs)研究了分子轨道的贡献。将每个原子上的Mulliken原子电荷和原子极性张量(APT)制成表格。本文还讨论了各模态的振动能。
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引用次数: 0
Formulation of Paint using Natural Pigment from Lawsonia Inermis Leaves 用槐叶天然色素制备涂料的研究
Pub Date : 2020-06-14 DOI: 10.14419/ijac.v8i1.30712
Z. Y. Abba, S. M.Gumel, A. A.Idris, M. A.Ibrahim
The increased application of paint in coating industry for interior and exterior decoration and corrosion inhibition, has inspired research in paint formulations. However, due to the toxic effect of preparatory chemicals used in paints, and the restrictive environmental legislation, research efforts have been directed to a more green process. In this work colouring matter from Lawsonia inermis leaves were extracted using water and analyzed by TLC and FTIR spectroscopy. White emulsion paint was formulated using pigment volume concentration (PVC) of 0.07%, the colouring matter extract was dispersed providing colour for the paint. The paint produced with the natural colourant was found to have similar properties with the paint produced using commercial pigment. Paint produced with aqueous extract faded under exposure to 5000 watts Tungsten Lamp after 48 hours but showed excellent fastness to rubbing. The extract induced excellent brownish colouration in the paint which maintained excellent, opacity, adhesion and good water resistance.   
油漆在涂料工业中的应用越来越多,用于室内和室外装饰和防腐,激发了涂料配方的研究。然而,由于油漆中使用的预备化学品的毒性作用,以及限制性的环境立法,研究工作已指向更绿色的过程。本文采用水提法提取了刺槐叶中的着色剂,并用薄层色谱和红外光谱对其进行了分析。采用体积浓度为0.07%的聚氯乙烯(PVC)配制白色乳胶漆,将着色剂提取物分散,为涂料提供颜色。用天然着色剂生产的油漆被发现与用商业颜料生产的油漆具有相似的性能。用水萃取物制备的涂料在5000瓦钨丝灯下暴露48小时后褪色,但耐摩擦牢度极佳。该提取物可使涂料呈良好的褐色,并保持良好的不透明度、附着力和耐水性。
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引用次数: 1
Adsorption of Methyl Orange Dye onto Raw Maize Cob and Maize Cob Activated Carbon: Isotherms and Thermodynamic Studies 甲基橙染料在玉米芯和玉米芯活性炭上的吸附:等温线和热力学研究
Pub Date : 2020-06-14 DOI: 10.14419/ijac.v8i1.30676
Safiyya Ibrahim Abubakar, Muhammad Adamu Ibrahim, Muhammad Bashir Ibrahim
This study was aimed to evaluate the adsorption of Methyl orange (MO) onto raw maize cob (RMC) and maize cob activated carbon (MCAC) from aqueous solution using batch adsorption studies. The produced adsorbents were characterized by Scanning electron microscope (SEM), and Fourier transform infrared spectroscopy (FTIR). The influence of contact time, dosage, concentration, temperature, and pH were investigated as well as Isotherm and Thermodynamic studies. Effect of contact time showed that Methyl orange adsorption were found to reach equilibrium within 125 and 110 minutes with optimum percentage removal of about 86.98% and 94.57% for raw maize cob and maize cob activated carbon respectively. The dye removal efficiency was found to increase with increasing initial dye concentration from 10 mg/L to 100 mg/L, and adsorption efficiency was found to be high at lower pH. However, increase in the dosage of the adsorbents lead to the increase in the adsorption process. The equilibrium adsorption data were analyzed using four adsorption models: Langmuir, Freundlich, Temkin, and D-R. The results revealed that MO with raw maize cob and maize cob activated carbon fit well to Freundlich with R2 value 0.977 and Temkin with R2 value 0.990 respectively and mean adsorption energy calculated from D-R shows it is physical adsorption and also values of enthalpy and Gibbs free energy proves that. Values of activation parameters such as free energy changes (∆G), enthalpy change (∆H) and entropy change (∆S) were calculated using Van't Hoff equation. All ∆G values were negative indicating that the adsorption was feasible and spontaneous. The result indicated that RMC and MCAC can be used for removal of MO from aqueous solution. The maize cob waste which is discarded as waste material was found to be effective adsorbent for the removal of Methyl orange dye from aqueous solution.  
研究了甲基橙(MO)在玉米芯(RMC)和玉米芯活性炭(MCAC)上的吸附性能。用扫描电镜(SEM)和傅里叶变换红外光谱(FTIR)对制备的吸附剂进行了表征。考察了接触时间、投加量、浓度、温度和pH的影响以及等温线和热力学研究。接触时间的影响表明,甲基橙在125分钟和110分钟内达到吸附平衡,对生玉米芯和玉米芯活性炭的最佳去除率分别为86.98%和94.57%。当初始染料浓度从10 mg/L增加到100 mg/L时,染料去除率随着染料浓度的增加而增加,并且在较低的ph下吸附效率较高。但随着吸附剂用量的增加,吸附过程会增加。采用Langmuir、Freundlich、Temkin和D-R四种吸附模型对平衡吸附数据进行分析。结果表明,玉米芯和玉米芯活性炭的MO与Freundlich和Temkin的拟合度分别为0.977和0.990,由D-R计算的平均吸附能表明MO为物理吸附,焓值和吉布斯自由能也证实了这一点。利用范霍夫方程计算自由能变化(∆G)、焓变化(∆H)、熵变化(∆S)等活化参数的值。所有∆G值均为负,表明吸附是可行的、自发的。结果表明,RMC和MCAC可用于去除水溶液中的MO。研究发现,废弃玉米芯是去除甲基橙染料的有效吸附剂。
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引用次数: 1
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International Journal of Advanced Chemistry
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