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The RP-HPLC method for analysis of usnic acid as potential marker of herbal drugs-based formulations containing Usnea barbata 采用反相高效液相色谱法分析山茱萸中药制剂中山茱萸酸的潜在标记物
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc201216045t
V. Tadić, A. Zugic, S. Djordjevic, I. Zizović, I. Homšek, D. Mišić, I. Nešić
The aim of this study was to develop and validate sensitive RP-HPLC method for determination of usnic acid, as potential marker substance of the herbal product for oromucosal use being the complex mixture of plant extracts and an essential oil, including the extract of Usnea barbata. Analysis of usnic acid in the tested formulation was performed through an extraction with methanol, prior to injection on the HPLC column (Zorbax Eclipse XDB-C18 600 Bar (4.6?100 mm, 1.8 ?m)). Employed gradient procedure of the solvents (phosphoric acid (pH 2.5) and acetonitrile), at flow rate of 0.1 mL/min allowed efficient and reproducible separation of usnic acid from other compounds present in the investigated complex mixture. The established suitability, linearity, precision, accuracy and selectivity/specificity of this assay implied its applicability as a reliable examination in the stability study of the investigated multi-ingredient herbal preparation.
本研究的目的是建立并验证一种灵敏的反相高效液相色谱法(RP-HPLC),用于测定山茱萸酸的含量。山茱萸酸是一种由植物提取物和精油组成的复杂混合物,其中包括山茱萸提取物。在高效液相色谱柱(Zorbax Eclipse XDB-C18 600 Bar (4.6?100毫米,1.8 ?m))。采用溶剂(磷酸(pH 2.5)和乙腈)的梯度法,在0.1 mL/min的流速下,可以从所研究的复杂混合物中有效地分离出usic酸和其他化合物。该方法的适宜性、线性度、精密度、准确度和选择性/特异性表明其可作为一种可靠的检测方法用于所研究的多成分中药制剂的稳定性研究。
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引用次数: 3
Synthesis of novel fluorinated 1,5-benzothiazepine derivatives and their biological evaluation as anticancer and antibacterial agent 新型氟化1,5-苯并噻唑类衍生物的合成及其抗癌、抗菌生物学评价
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc210428041b
Sonal Bhabal, S. Shaikh, Ishita Yellapurkar, G. Pavale, M. Ramana
A series of novel fluorinated 1,5-benzothiazepine derivatives were synthesized, characterized and evaluated for in vitro anticancer and antibacterial activity. The in vitro anticancer activity of the synthesized compounds 4(a-h) was evaluated against four human cancer cell lines namely lung (A549), breast (MCF-7), liver (HEPG2) and prostate (PC-3) cancer. Compounds 4c, 4d, 4g and 4h exhibited good activity with GI50 <10 ?g ml-1 against all four human cancer cell lines which was comparable to standard drug Adriamycin. Additionally, antibacterial activity of synthesized compounds was estimated using resazurin microtiter assay (REMA) and compared with standard drug Ampicillin. Among the synthesized compounds, 4c, 4d, 4g and 4h showed in good antibacterial activity and all the synthesized compounds were found to be more active towards gram negative than gram positive. These promising results obtained from in vitro anticancer and antibacterial activity, inferred that the synthesized compounds are capable of being anticancer as well as antibacterial agent.
合成了一系列新型氟化1,5-苯并噻唑类衍生物,并对其体外抗癌和抗菌活性进行了表征和评价。合成的化合物4(a-h)对肺癌(A549)、乳腺癌(MCF-7)、肝癌(HEPG2)和前列腺癌(PC-3)四种人癌细胞的体外抗癌活性进行了评价。化合物4c、4d、4g和4h对四种人类癌细胞具有良好的活性,其GI50 <10 μ g ml-1,与标准药物阿霉素相当。此外,采用瑞唑脲微效价测定法(REMA)评估合成化合物的抗菌活性,并与标准药物氨苄西林进行比较。在所合成的化合物中,4c、4d、4g和4h均表现出较好的抗菌活性,且所有化合物对革兰氏阴性菌的活性均高于革兰氏阳性菌。从体外抗癌和抗菌活性的研究结果来看,所合成的化合物具有抗癌和抗菌的双重作用。
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引用次数: 0
Synthesis of some benzylidene thiosemicarbazide derivatives and evaluation of their cytotoxicity on U87, MCF-7, A549, 3T3 and HUVEC cell lines 一些苄基硫代氨基脲衍生物的合成及其对U87、MCF-7、A549、3T3和HUVEC细胞的细胞毒性评价
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc210630016e
Touba Eslaminejad, Yaghoub Pourshojaei, M. Naghizadeh, Hoda Eslami, Mohammad Daneshpajouh, A. Hassanzadeh
Iron homeostasis is altered in tumours in response to a perturbation in the expression of iron-dependent proteins. Therefore, iron chelators make cancerous cells more vulnerable to iron deficiency. Compounds having thiosemicarbazide scaffold with the ability to metal complex formation have the potential to act as anticancer. A series of thiosemicarbazide derivatives were designed, synthesized successfully and their cytotoxicity was then tested on some cancerous as well as laboratory normal model systems by using colorimetric assay based on WST-1 reagent. According to the cytotoxicity results, some compounds showed high toxicity effect on both the cancerous and healthy cell lines. The results of toxicity assays on U87 and A549 cell lines showed the survivability less than 50% at all concentrations higher than 10 ppm for all the synthesized compounds. The MCF-7 cell line approximately exhibited the same behaviour and had survivability less than 60%. The 3T3 in compared with HUVEC cell line showed a completely different behaviour against the synthesized compounds and had survivability more than 50%. The selectivity index was also measured and based on the study results this could be concluded that the cytotoxicity profile of the synthesized compounds on 3T3 cell line shows a significant difference, indicating a good anticancer effect for these compounds.
铁稳态在肿瘤中被改变以响应铁依赖蛋白表达的扰动。因此,铁螯合剂使癌细胞更容易受到缺铁的影响。具有巯基氨基脲支架和金属络合物形成能力的化合物具有潜在的抗癌作用。设计并成功合成了一系列硫代氨基脲衍生物,并采用WST-1试剂比色法对其在肿瘤和实验室正常模型系统上的细胞毒性进行了检测。根据细胞毒性结果,一些化合物对癌变细胞系和健康细胞系均表现出高毒性作用。对U87和A549细胞株的毒性试验结果表明,在浓度高于10 ppm时,所有化合物的存活率均低于50%。MCF-7细胞系表现出大致相同的行为,存活率低于60%。与HUVEC细胞株相比,3T3对合成化合物表现出完全不同的行为,存活率超过50%。同时测定了选择性指数,根据研究结果可以得出,合成的化合物对3T3细胞株的细胞毒性谱有显著差异,表明这些化合物具有良好的抗癌作用。
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引用次数: 1
Green chemical principles based regioselective functionalization of 2,4,6-trichloropyrimidine-5-carbaldehyde: Application in the synthesis of new pyrimidines and pyrrolopyrimidine 基于2,4,6-三氯嘧啶-5-乙醛区域选择性功能化的绿色化学原理:在新嘧啶和吡咯嘧啶合成中的应用
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc210804063u
Allu Udayasri, Manchikanti Chandrasekhar, Brahmeswararao Naga, Ganesh Varanasi, D. Ramakrishna
The present work reports the synthesis of three new nitrogen-containing heteronuclear molecules (two pyrimidines and one pyrrolopyrimidine). Based on the 12 principles of green chemistry, chemical methodologies are planned and executed. Various phase transfer catalysts were examined in the crucial step to execute C-N bond formation (through SnAr mechanism), TBAI was found to be a better option than that of TBand CTAB. The one-pot synthetic methodology was optimized involving Wittig olefination and bromination to achieve a key precursor for the synthesis of a new pyrrolopyrimidine.
本文报道了三个新的含氮杂核分子(两个嘧啶和一个吡咯嘧啶)的合成。基于绿色化学的12条原则,化学方法被规划和执行。在形成C-N键的关键步骤(通过SnAr机制)中考察了各种相转移催化剂,发现TBAI比TBand CTAB更好。优化了Wittig烯烃和溴化的一锅合成方法,获得了合成新型吡咯嘧啶的关键前驱体。
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引用次数: 3
Optimization of the slaughterhouse water treatment rate by a new Marinobacter carbonoclasticus SF and its biosurfactant 新型破碳海洋杆菌及其生物表面活性剂对屠宰场水处理率的优化
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc211029023m
Nadia Mihoubi, S. Ferhat, R. Alouaoui, A. Ibrir, M. Nedjhioui, A. Badis
The aim of this study consists of the production of a bio-surfactant from a new bacterial strain, Marinobacter hydrocarbono clasticus SF (96.76 % simila-rity) isolated from soil contaminated by hydrocarbons in Hassi-Messaoud. (Southern Algeria) to treat liquid effluent from slaughterhouse water. The characteristics of organic matter biodegradation tests were discussed. Despite the high pollutant load and the unfavorable Physico-chemical composition of the effluent, the specific growth rate of the isolated strain after 10 days of incubation in the range of 0-30 g L-1 of NaCl was at neutral pH 7.4 and temperature of 45 ?C. The best bio-surfactant production yield was obtained after 72 h of incubation and under the optimal production conditions such as diesel as carbon source, ammonium chloride as nitrogen source, and a C/N ration of 5. The bio-surfactant produced is of glycolipid type with a low critical micellar concentration (CMC), good emulsifying power, and chemical and functional stability. Significant pollutant removal efficiency was obtained using the bacterial strain (up to 82 %) and the bio-surfactant (up to 96 %). Several anions, such as nitrates, phosphates, ammonium, and suspended solids, were measured.
本研究的目的是利用从hassii - messaoud被碳氢化合物污染的土壤中分离到的一株新的细菌Marinobacter hydrocarbono clasticus SF(相似度为96.76%)生产生物表面活性剂。(阿尔及利亚南部)处理屠宰场水排出的液体。讨论了有机物生物降解试验的特点。在NaCl浓度为0 ~ 30 g L-1的条件下,在中性pH值为7.4、温度为45℃的条件下,培养10 d后,分离菌株的比生长率达到了较高的水平。在以柴油为碳源、氯化铵为氮源、C/N比为5的最佳生产条件下,培养72 h生物表面活性剂的产率最佳。所制得的生物表面活性剂为糖脂型,具有临界胶束浓度低、乳化性能好、化学稳定性和功能稳定性好等特点。该菌株对污染物的去除率高达82%,生物表面活性剂的去除率高达96%。测量了几种阴离子,如硝酸盐、磷酸盐、铵离子和悬浮物。
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引用次数: 0
The influence of different enzymatic preparations and skin contact time on aromatic profile of wines produced from autochthonous grape varieties Krstac and Zizak 不同酶制剂和皮肤接触时间对本地葡萄品种Krstac和Zizak葡萄酒芳香特征的影响
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc220311056m
Valerija Madzgalj, A. Petrovic, U. Čakar, V. Maras, Ivana Sofrenić, V. Tešević
This study aimed to show aromatic profile of wines produced from two autochthonous grape cultivars Krstac (K) and Zizak (Z). During the wine production two enzymatic preparations (EP) (Lallzyme cuvee blanc (CB) and Lallzyme enzymatic preparation ? (EB)) and different time of skin contact (4 and 8 h) were applied. Aromatic compounds were detected by GC/FID-MS analysis. Significantly higher content of total detected aromatic compounds compared to appropriate controls (168.54 and 161.72 mg L-1) was observed for K EB4h (176.33 mg L-1) and Z CB4h (177.29 mg L-1) wines. Skin contact and usage of EP mostly increased content of 2-phenylethyl and isoamyl alcohols. Wines from both varieties showed higher content of hexanoic and octanoic acids compared to control. It is interesting to emphasize that content of esters which are responsible for fruity aroma of wine which is important for pleasant taste (isoamyl acetate - banana, ethyl hexanoate - ripe banana, 2-phenylethyl acetate - powerful fruity rose like) were increased in all samples compared to controls. The highest grades after sensory evaluation were obtained for K EB 8h (18.0 out of 20.0) and Z CB 8h (18.2 out of 20.0).
本研究旨在展示两种本土葡萄品种Krstac (K)和Zizak (Z)生产的葡萄酒的芳香特征。在葡萄酒生产过程中,两种酶制剂(Lallzyme cuvee blanc (CB)和Lallzyme酶制剂?(EB)和不同的皮肤接触时间(4和8 h)。采用GC/FID-MS分析方法检测芳香族化合物。K EB4h (176.33 mg L-1)和Z CB4h (177.29 mg L-1)的总芳香化合物含量显著高于对照(168.54和161.72 mg L-1)。皮肤接触和EP的使用增加了2-苯乙基和异戊醇的含量。两个品种的葡萄酒中己酸和辛酸的含量均高于对照。有趣的是,与对照组相比,所有样品中负责葡萄酒水果香气的酯类含量都有所增加,这些酯类对令人愉悦的口感很重要(乙酸异戊酯-香蕉,己酸乙酯-成熟香蕉,2-苯乙酸乙酯-强大的果味玫瑰)。感官评价得分最高的是K EB 8h(18.0 / 20.0)和Z CB 8h(18.2 / 20.0)。
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引用次数: 9
Ammonia removal by natural modified clinoptilolite 天然改性斜沸石脱氨研究
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc211110051g
Aytaç Günal, Burcu Erdoğan
In this study, cation exchange and acid activation processes were applied to determine the effects of different cationic compositions of clinoptilolite on ammonia (NH3) adsorption properties. Thermogravimetric (TG), differential thermal analysis (DTA), X-ray diffraction (XRD), X-ray fluorescence (XRF) and nitrogen adsorption techniques were used for the characterization of the clinoptilolite samples. As a result of ion exchange and acid activation, the amount, type, and location of exchangeable cations in the structure significantly affected the thermal properties as well as NH3 removal efficiency. Ammonia adsorption isotherms were obtained at 298 K up to 100 kPa volumetrically. In addition, NH3 adsorption capacities of the clinoptilolite samples within this study (3.823 to 5.372 mmol g-1) were compared with those of the other materials (1.77 to 12.2 mmol g-1) in terms of their textural and structural differences.
本研究采用阳离子交换法和酸活化法测定斜发沸石不同阳离子组成对氨(NH3)吸附性能的影响。采用热重(TG)、差热分析(DTA)、x射线衍射(XRD)、x射线荧光(XRF)和氮吸附等技术对斜沸石样品进行表征。由于离子交换和酸活化,结构中可交换阳离子的数量、类型和位置对热性能和NH3去除率有显著影响。在298 K ~ 100 kPa条件下获得了氨吸附等温线。此外,比较了本研究中斜沸石样品的NH3吸附量(3.823 ~ 5.372 mmol g-1)与其他材料(1.77 ~ 12.2 mmol g-1)在结构和结构上的差异。
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引用次数: 0
Synthesis of activated carbons from water hyacinth biomass and its application as adsorbents in water pollution control 水葫芦生物质活性炭的合成及其吸附剂在水污染控制中的应用
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc212121006m
Ahmad Mohammaad, M. Kijevčanin
The water hyacinth biomass was used for the synthesis of activated carbons in process of chemical activation with ZnCl2, followed by controlled pyrolysis. The applied impregnation weight ratios ZnCl2 and dry hyacinth biomass were in the range of 0.5 - 3.5. The carbonization was conducted at four different temperatures (T= 400-700?C) under an inert atmosphere. The highest yield of activated carbon was obtained for the impregnation ratio of 0.5 and carbonization temperature of 400?C. The samples were characterized using elemental analysis, adsorption-desorption isotherms of nitrogen and SEM analysis. The activated carbon obtained with an impregnation ratio 2.0 and carbonization temperature of 500?C (2.0AC500) showed the highest values of specific surface area and total pore volume of 1317 m2 g-1 and 0.697 cm3 g-1, respectively. The adsorption of glyphosate, pesticide with a strong negative environmental impact, was fast process, with equilibrium time of 120 min. The adsorption isotherms were fitted with Langmuir and Freundlich model. The Langmuir adsorption capacity of qmax=240.8 mg g-1 for 2.0AC500 classified the selected adsorbent as a very efficient one. The tested adsorption process followed the kinetics of the pseudo-second-order model.
以水葫芦生物量为原料,通过ZnCl2化学活化合成活性炭,然后进行可控热解。ZnCl2与干风信子生物量的浸渍质量比在0.5 ~ 3.5之间。在惰性气氛下,在4种不同温度(T= 400-700℃)下进行炭化。浸渍比为0.5、炭化温度为400℃时,活性炭得率最高。采用元素分析、氮的吸附-解吸等温线和扫描电镜对样品进行了表征。浸渍比为2.0,炭化温度为500?C (2.0AC500)的比表面积和总孔体积最高,分别为1317 m2 g-1和0.697 cm3 g-1。吸附过程快速,平衡时间为120 min,吸附等温线符合Langmuir和Freundlich模型。对2.0AC500的Langmuir吸附量qmax=240.8 mg g-1,为高效吸附剂。吸附过程符合准二阶动力学模型。
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引用次数: 2
Leaching of heavy metals from wood biomass ash, before and after binding in cement composite 水泥复合材料粘结前后木材生物质灰中重金属的浸出
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc220217054d
D. Drljaca, Ljiljana Vukic, Dajana Dragic, A. Borkovic, T. Botic, P. Dugic, Saša Papuga, Marko Solic, S. Maletić, P. Gvero, Jelena Savkovic
Wood ash is a complex mixture of inorganic and organic compounds. It is heterogeneous in composition, which can vary considerably. Ash is mainly disposed of in landfills, which poses a risk for air, soil and groundwater contamination by trace elements. In order for wood biomass ash to be used as a secondary raw material, it is necessary to perform leaching tests, to determine which microelements it contains, and which of them could be released into the environment during the ash disposal. Sequential extraction showed that in the exchangeable and carbonate fraction, the most volatile metals As, Cd, Zn and Pb are released the most from the ash of deciduous trees, while the leaching of ash from coniferous trees is significantly lower. The evaluation of risk assessment code (RAC) for the tested biomass ash samples, indicates that Pb is a high-risk leaching element due to its condensation on the ash particles. By performing TCLP (Toxicity Characteristic Leaching Procedure) and SPLP (Synthetic Precipitation Leaching Procedure) tests, it was established that the released concentrations of tested metals are below the maximum allowable concentration, given by the Regulation. The leaching tests of composites, prepared from wood ash in combination with cement, indicate that the leaching of ash is reduced to a minimum, and that all heavy metals are bound in a cement matrix, which indicates the possibility of using wood ash for construction purposes.
木灰是一种无机和有机化合物的复杂混合物。它的成分是异质的,可以有很大的不同。灰烬主要在垃圾填埋场处理,这对空气、土壤和地下水造成了微量元素污染的风险。为了将木材生物质灰分用作二级原料,必须进行浸出试验,以确定其中含有哪些微量元素,以及在灰分处置过程中哪些微量元素可能被释放到环境中。序次提取结果表明,在交换性组分和碳酸盐组分中,挥发性最强的金属As、Cd、Zn和Pb以落叶树灰分释放最多,而针叶树灰分的淋滤量明显较低。对所测生物质灰样的风险评价代码(RAC)评价表明,Pb在灰颗粒上的凝结是一种高风险浸出元素。通过执行TCLP(毒性特性浸出程序)和SPLP(合成沉淀浸出程序)测试,确定测试金属的释放浓度低于法规规定的最大允许浓度。由木灰与水泥混合制备的复合材料的浸出试验表明,灰的浸出减少到最低限度,所有重金属都结合在水泥基质中,这表明将木灰用于建筑目的的可能性。
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引用次数: 1
Divergent synthesis and antitumour activity of novel conformationally constrained (−)-muricatacin analogues 新型构象约束(−)-穆里卡星类似物的发散合成和抗肿瘤活性
IF 1 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-01-01 DOI: 10.2298/jsc220613069s
Sladjana Stanisavljevic, Bojana Sreco-Zelenovic, Mirjana Popsavin, M. Rodić, V. Popsavin, V. Kojić
Four novel conformationally restricted (?)-muricatacin analogues bearing a methoxy group at the C-5 position, with an alkoxymethyl group ?s the C-7 side chain, have been synthesised and their in vitro antiproliferative activity was evaluated against a panel of seven human tumour cell lines, as well as a single normal cell line. All analogues (9-12) showed diverse antiproliferative effects against all tested human malignant cell lines, but were devoid of any significant cytotoxicity towards the normal foetal lung fibroblasts (MRC-5). A SAR study reveals that the introduction of THF ring, exchange of C-8 methylene group in the side chain of muricatacin analogues with the O-8 ether functionality, as well as the length of side chain may be beneficial for the antiproliferative effects of these lactones. All novel analogues were more potent than lead compound, (?)-muricatacin, against HL-60 cell line.
合成了四种新的构象限制性(?)-穆里卡星类似物,其C-5位置上有一个甲氧基,C-7侧链上有一个烷氧甲基,并对七种人类肿瘤细胞系和一种正常细胞系进行了体外抗增殖活性评估。所有类似物(9-12)对所有测试的人类恶性细胞系显示出不同的抗增殖作用,但对正常胎儿肺成纤维细胞(MRC-5)没有任何显著的细胞毒性。SAR研究表明THF环的引入、具有O-8醚官能团的穆里卡星类似物侧链上C-8亚甲基的交换以及侧链的长度可能有利于这些内酯的抗增殖作用。所有新型类似物对HL-60细胞株的抑制作用均优于先导化合物(?)-穆里卡星。
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引用次数: 0
期刊
Journal of The Serbian Chemical Society
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