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Método cualitativo rápido (screening) para la detección de residuos de plaguicidas en frutas y hortalizas 水果和蔬菜中农药残留的快速定性(筛选)检测方法
IF 0.8 Pub Date : 2018-04-01 DOI: 10.15446/REV.COLOMB.QUIM.V47N1.62240
Iván Mauricio Huérfano Barco, J. A. G. Dallos
Because of the importance of developing methodologies that allow agricultural residues analysis, a rapid screening qualitative method for the determination of pesticides residues in fruits and vegetables was validated. The methodology was based on the European QuEChERS extraction method with an additional cleaning step by gel permeation chromatography (GPC), which helped to reduce the number of matrix components in the final extract. The analysis was carried out by gas chromatography coupled to mass spectrometry with a single quadrupole analyzer. The methodology was appropriate for the qualitative analysis of 31 pesticides at their respective maximum residue limits. Consistent results were obtained with respect to a quantitative routine methodology in the analysis of real samples, hence the methodology was proven to be a good alternative for the fast analysis of these contaminants in fruits and vegetables.
由于开发农业残留分析方法的重要性,验证了一种用于测定水果和蔬菜中农药残留的快速筛选定性方法。该方法基于欧洲QuEChERS提取方法,通过凝胶渗透色谱法(GPC)进行额外的清洁步骤,这有助于减少最终提取物中基质成分的数量。分析通过气相色谱-质谱联用单四极杆分析仪进行。该方法适用于31种农药在各自最大残留限量下的定性分析。在实际样品的分析中,定量常规方法获得了一致的结果,因此该方法被证明是快速分析水果和蔬菜中这些污染物的良好替代方法。
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引用次数: 0
Ensayo de migración global en empaques para alimentos: evaluación de patrones internos alternativos 食品包装的全球迁移测试:替代内部模式的评估
IF 0.8 Pub Date : 2018-01-01 DOI: 10.15446/REV.COLOMB.QUIM.V47N1.63859
Edgar Andres Avendaño Florez, Elianna Castillo Serna, Diana Cristina Sinuco León
In the global migration test for plastic packaging intended for fatty foods, glyceryl triheptadecanoate (GTM) is used as the internal standard for the quantification of fatty acid methyl esters (FAMEs) by gas chromatography. In this work, ethyl 3-phenyl propanoate (EFP) and tetradecanoic acid (AM) were evaluated as alternative internal standards. The use of (AM) presented linear behavior (r > 0.99 and %Sb < 5%), good intermediate precision (HORRATr = 0.9), and accuracy (%R = 100.6%). In contrast, the evaluation of (EFP) demonstrated that this is not an adequate internal standard for the quantification of FAMEs. In addition, it was statistically evaluated that there are no significant differences in the calculation of the global migration from FAMEs quantified using GTM or AM as internal standards, but the use of EFP presents significant differences.
在高脂肪食品用塑料包装的全球迁移试验中,采用三庚酸甘油酯(GTM)作为气相色谱法定量脂肪酸甲酯(FAMEs)的内标。以3-苯基丙酸乙酯(EFP)和十四烷酸(AM)作为备选内标进行了评价。(AM)的使用呈现线性行为(r = 0.99, %Sb < 5%),良好的中间精度(HORRATr = 0.9)和准确度(% r = 100.6%)。相比之下,EFP的评价表明,这不是一个适当的内部标准,以定量的FAMEs。此外,统计评估表明,使用GTM或AM作为内部标准量化的FAMEs的全球迁移计算没有显著差异,但使用EFP存在显著差异。
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引用次数: 2
Preparative method to obtain ursolic acid from Clinopodium revolutum 从羊角草中制备熊果酸的制备方法
IF 0.8 Pub Date : 2018-01-01 DOI: 10.15446/REV.COLOMB.QUIM.V47N1.65375
M. Huamán
A method to obtain ursolic acid (UA) in an easy, fast, and economical way was proposed, having as raw material the medicinal plant Clinopodium revolutum from Peru. This plant is known and marketed as flor de arena or te indio. The selective recrystallization technique used was efficient due to UA crystals were obtained without the need for chromatographic purification methods neither the use of toxic solvents. The purity determined by HPLC is greater than 95%. Thus, the flor de arena becomes an important biosource of this compound.
提出了一种以秘鲁药用植物羊角草为原料,简便、快速、经济地制备熊果酸的方法。这种植物被称为flor de arena或the indio。所采用的选择性重结晶技术是高效的,因为UA晶体不需要色谱纯化方法,也不需要使用有毒溶剂。HPLC法测定其纯度大于95%。因此,地面成为该化合物的重要生物来源。
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引用次数: 2
Transamidación y transamidación-reducción de N-benciltiramina con DMF DMF的n-苄基酪胺转胺和转胺还原
IF 0.8 Pub Date : 2018-01-01 DOI: 10.15446/REV.COLOMB.QUIM.V47N1.63976
Christian Díaz Oviedo, Ariel Rodolfo Quevedo Pastor
La tiramina y la N-benciltiramina reaccionan con formaldehido para formar azaciclofanos por medio de condensaciones tipo Mannich aromaticas y reaccionan con aldehidos no enolizables para formar las respectivas bases de Schiff. En este articulo se presenta la sintesis inesperada de N-bencil-N-formiltiramina y N-bencil-N-metiltiramina por medio de reacciones de transamidacion y de transamidacion-reduccion de N-benciltiramina con N,N-dimetilformamida. Para explicar el curso de la reaccion se propuso un mecanismo que involucra la formilacion de N-benciltiramina y posterior reduccion de Leuckart-Wallach inducida por acido formico generado in situ.
酪胺和n -苯基酪胺与甲醛通过芳香曼尼奇缩合反应生成氮杂环芬,并与非烯化醛反应生成各自的席夫碱。本文介绍了N-苄基-N-甲酰酪胺和N-苄基-N-甲基酪胺与N,N-二甲基甲酰胺的转胺和转胺还原反应的意外合成。为了解释反应过程,提出了一种机制,包括n -苄基酪胺的甲酰化和随后由原位生成的甲酸诱导的Leuckart-Wallach还原。
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引用次数: 0
Synthesis, characterization, X-ray crystal structure and DFT calculations of 4-([2,2':6',2''-terpyridin]- 4'-yl)phenol 4-([2,2':6',2 " -三联吡啶]- 4'-基)苯酚的合成、表征、x射线晶体结构和DFT计算
IF 0.8 Pub Date : 2018-01-01 DOI: 10.15446/REV.COLOMB.QUIM.V47N1.66281
César A. Sierra, Brian Castro Agudelo, Cristian Ochoa‐Puentes, William Rodríguez-Córdoba, A. Reiber
The synthesis of new terpyridine (Tpy) derivatives has been subject of extensive research due to its potential as functional materials for solar energy conversion, among other applications. In this contribution, the 4-([2,2':6',2''-terpyridin]-4'-yl)phenol (TpyOH) has been synthesized, characterized and studied through several methods, including X-ray crystallography and computational approaches. Single crystal X-ray structure analysis shows that TpyOH is essentially planar, with dihedral angles of about 5.03° between the central pyridinyl and the phenolic ring, and also 6.05 and 12.2° in the terpyridine moiety. In the crystal, molecules are linked by intermolecular hydrogen bonds and through π-π stacking interactions. Using a time-dependent density functional theory approach and taking into account bulk solvent effects, the absorption and fluorescence spectra of TpyOH were investigated and compared. The TD-DFT S0 → Sn and S1 → S0 transition energies are in good agreement with experimental results. The frontier molecular orbitals analysis showed that the low-energy absorption band has an intraligand charge transfer character (ICT), while the high-energy band is a common feature of π-π* transitions of the Tpy moiety. The S1→S0 emission transition also has an ICT character, with a 90% contribution from the HOMO→LUMO transitions.
新型三吡啶(Tpy)衍生物的合成由于其作为太阳能转换功能材料的潜力而受到广泛的研究。本文合成了4-([2,2':6',2 " -terpyridin]-4'-yl)苯酚(TpyOH),并通过x射线晶体学和计算方法对其进行了表征和研究。单晶x射线结构分析表明,TpyOH基本呈平面结构,中心吡啶基与酚环之间的二面角约为5.03°,三吡啶部分的二面角为6.05°和12.2°。在晶体中,分子通过分子间氢键和π-π堆叠相互作用连接。采用随时间变化的密度泛函理论方法,考虑体积溶剂效应,对TpyOH的吸收光谱和荧光光谱进行了研究和比较。TD-DFT的S0→Sn和S1→S0跃迁能与实验结果吻合较好。前沿分子轨道分析表明,低能吸收带具有配体内电荷转移特征(ICT),而高能吸收带是Tpy部分π-π*跃迁的共同特征。S1→S0的发射跃迁也具有ICT特征,其中90%的能量来自HOMO→LUMO跃迁。
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引用次数: 3
Diseño experimental para determinar el efecto del tamaño del pellet de catalizadores bimetálicos Cu-Ni en la reacción de desplazamiento de agua 测定双金属铜镍催化剂颗粒大小对水置换反应的影响的实验设计
IF 0.8 Pub Date : 2018-01-01 DOI: 10.15446/REV.COLOMB.QUIM.V47N1.64699
Oscar Felipe Arbeláez Pérez, Víctor Ignacio López Ríos, Aída Luz Villa Holguín, Adriana Patricia Villegas Quiceno
Bimetallic Cu-Ni catalysts were synthesized with molar ratio 2-1 in cylindrical activated carbon pellets of different diameters (0.2 cm, 0.3 cm, and 0.4 cm) and length (0.4 cm and 0.6 cm). They were evaluated in the water gas shift reaction at 330 °C and atmospheric pressure. An experimental design was developed to evaluate the effect of variables, diameter and length of the pellets, over carbon monoxide conversion. The importance of the main factors and their interactions were examined by analysis of variance (ANOVA). The results showed that both diameter and length of the pellets had significant effect on carbon monoxide conversion. The results of the catalytic activity indicated that up to 96% CO conversion was obtained at the optimum characteristic of the pellets, diameter of 0.2 cm and length of 0.6 cm.
以不同直径(0.2 cm、0.3 cm和0.4 cm)和长度(0.4 cm和0.6 cm)的圆柱形活性炭球为原料,以摩尔比2-1的比例合成了Cu-Ni双金属催化剂。在330°C和常压下的水气转换反应中对它们进行了评价。开发了一种实验设计来评估变量,颗粒直径和长度对一氧化碳转化的影响。通过方差分析(ANOVA)检验了主要因素的重要性及其相互作用。结果表明,球团直径和球团长度对一氧化碳转化率均有显著影响。催化活性结果表明,在粒径为0.2 cm、长度为0.6 cm的球团的最佳性能条件下,CO转化率可达96%。
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引用次数: 3
Nanopartículas de CuO y su propiedad antimicrobiana en cepas intrahospitalarias 纳米氧化铜及其对医院内菌株的抗菌性能
IF 0.8 Pub Date : 2017-09-01 DOI: 10.15446/REV.COLOMB.QUIM.V46N3.62386
L. Román, F. Castro, D. Maurtua, C. Condori, Darwin Vivas, A. E. Bianchi, F. Paraguay-Delgado, J. Solís, M. M. Gómez
Using a prototype reactor, CuO nanoparticles (NPs) were synthetized through the precipitation method, starting from CuSO2·5H2O and Cu(CH3COO)2·H2O. The obtained NPs were characterized by XDR, FT-IR, SEM, and TEM. The antimicrobial activity of the NPs was determined by the plate diffusion method, placing 20 mg of NPs onto four nosocomial strains obtained from north Lima national hospital Intensive-Care Unit (Staphylococcus epidermidis, Aerococcus viridans, Ochrobactrum anthropic, and Micrococcus lylae). NPs characterization revealed that those synthetized from acetate (CuO–Acet) shown pure CuO phase, while those synthetized from sulphate CuO–Sulf shown two phases where CuO was the predominant one, having more than 84%. The crystal domains for CuO–Acet and CuO–Sulf were 15 and 19 nm, respectively. The inhibition halos for the studied strains were larger for CuO–Sulf NPs than CuO–Acet NPs, only Ochrobactrum anthropi displayed similar inhibition halos for both types of NPs.
在原型反应器上,以CuSO2·5H2O和Cu(CH3COO)2·H2O为原料,采用沉淀法合成了CuO纳米颗粒。通过XDR、FT-IR、SEM、TEM等手段对所得NPs进行了表征。通过平板扩散法测定NPs的抗菌活性,将20 mg NPs置于从北利马国家医院重症监护室获得的4株医院菌株(表皮葡萄球菌、绿质空气球菌、人嗜冷杆菌和lylae微球菌)上。NPs表征表明,由乙酸酯(CuO - acet)合成的NPs表现为纯CuO相,而由硫酸盐(CuO - sulf)合成的NPs表现为两相CuO为主,占比超过84%。CuO-Acet和CuO-Sulf的晶域分别为15 nm和19 nm。研究菌株对cuo -硫NPs的抑制晕大于CuO-Acet NPs,只有人类Ochrobactrum对这两种NPs表现出相似的抑制晕。
{"title":"Nanopartículas de CuO y su propiedad antimicrobiana en cepas intrahospitalarias","authors":"L. Román, F. Castro, D. Maurtua, C. Condori, Darwin Vivas, A. E. Bianchi, F. Paraguay-Delgado, J. Solís, M. M. Gómez","doi":"10.15446/REV.COLOMB.QUIM.V46N3.62386","DOIUrl":"https://doi.org/10.15446/REV.COLOMB.QUIM.V46N3.62386","url":null,"abstract":"Using a prototype reactor, CuO nanoparticles (NPs) were synthetized through the precipitation method, starting from CuSO2·5H2O and Cu(CH3COO)2·H2O. The obtained NPs were characterized by XDR, FT-IR, SEM, and TEM. The antimicrobial activity of the NPs was determined by the plate diffusion method, placing 20 mg of NPs onto four nosocomial strains obtained from north Lima national hospital Intensive-Care Unit (Staphylococcus epidermidis, Aerococcus viridans, Ochrobactrum anthropic, and Micrococcus lylae). NPs characterization revealed that those synthetized from acetate (CuO–Acet) shown pure CuO phase, while those synthetized from sulphate CuO–Sulf shown two phases where CuO was the predominant one, having more than 84%. The crystal domains for CuO–Acet and CuO–Sulf were 15 and 19 nm, respectively. The inhibition halos for the studied strains were larger for CuO–Sulf NPs than CuO–Acet NPs, only Ochrobactrum anthropi displayed similar inhibition halos for both types of NPs.","PeriodicalId":43662,"journal":{"name":"Revista Colombiana de Quimica","volume":null,"pages":null},"PeriodicalIF":0.8,"publicationDate":"2017-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41543703","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 4
Diseño y producción de diversas proteínas fusión de la nicotinamida/nicotinato mononucleótido adenilil transferasa (NMNAT) de Plasmodium falciparum
IF 0.8 Pub Date : 2017-09-01 DOI: 10.15446/REV.COLOMB.QUIM.V46N3.63492
C. Clavijo, Nicolás Forero Baena, Marializ Magaly Ramírez Hernández
Recombinant proteins have become useful tools in biochemistry research. During their production, however, inclusion bodies (IB) appear, on the one hand, due to the high expression rate from the recombinant plasmids, which have high efficiency promoters, and, on the other hand, intrinsic characteristics of the expressed protein. Furhtermore, the nicotinamide/nicotinate mononucleotide adenilyl transferase (NMNAT) is a central protein in NAD(H)+ biosynthesis, an essential cofactor in cell metabolism, and in protozoon parasite has been studied. To study the NMNAT protein of these parasites, their recombinant version in E. coli has been expressed, getting a great quantity of IB as a by-product. To increase the solubility of the protein, the coding sequence of the NMNAT enzyme of Plasmodium falciparum was cloned in different expression plasmids which were subsequently transformed into E. coli BL21(DE3) expression strain. The solubility of the recombinant proteins was assessed and the one with the highest presence in the soluble fraction was subsequently purified and its enzyme activity was determined. The recombinant protein with a MBP (maltose-binding protein) tag showed an increased solubility and purity.
重组蛋白已成为生物化学研究的有用工具。然而,在其生产过程中,包含体(IB)的出现,一方面是由于重组质粒具有高效启动子的高表达率,另一方面是由于所表达蛋白的固有特性。烟酰胺/烟酸单核苷酸腺苷转移酶(NMNAT)是NAD(H)+生物合成的中心蛋白,是细胞代谢的重要辅助因子,在原虫寄生虫中也有研究。为了研究这些寄生虫的NMNAT蛋白,我们在大肠杆菌中表达了它们的重组蛋白,得到了大量的IB作为副产物。为了提高该蛋白的溶解度,将恶性疟原虫NMNAT酶的编码序列克隆到不同表达质粒中,转化到大肠杆菌BL21(DE3)表达菌株中。评估了重组蛋白的溶解度,随后纯化了可溶性部分中存在最高的重组蛋白,并测定了其酶活性。带有MBP(麦芽糖结合蛋白)标签的重组蛋白显示出更高的溶解度和纯度。
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引用次数: 1
Synthesis of acyl-hydrazone from usnic acid and isoniazid and its anti-Mycobacterium tuberculosis activity usnic酸和异烟肼合成酰基腙及其抗结核分枝杆菌活性
IF 0.8 Pub Date : 2017-09-01 DOI: 10.15446/REV.COLOMB.QUIM.V46N3.61980
Melissa Barrera Tomas, Gloria Eva Tomas Chota, Patricia Sheen Cortavarría, Patricia Fuentes Bonilla, Miguel Angel Inocente Camones, J. Contreras
Compound usnic acid (1), isolated from lichen Evernia prunastri (Cajamarca-Peru) and the synthesis and characterization of its acyl-hydrazone (2), from the condensation reaction between usnic acid and isoniazid in an ethanol solution under reflux, giving an overall yield of 95%, were evaluated. Both compounds were evaluated and compared with isoniazid according to its anti-Mycobacterium tuberculosis activity based on the tetrazolium microplate assay (TEMA). Compound 1 had MIC (minimal inhibitory concentration) value of 16.0 μg/mL in each test of H37Rv (susceptible type), TB DM 97 (resistant wild type) and MDR DM 1098 (multi drug resistances type) strains. In similar tests, compound 2 MIC values were 2.0, 64.0 and 64.0 μg/mL respectively.
从秘鲁苔草(Cajamarca Peru)中分离得到化合物usnic酸(1),并对其酰基腙(2)的合成和表征进行了评价,该化合物由usnic和异烟肼在乙醇溶液中回流缩合反应得到,总收率为95%。基于四氮唑微板测定法(TEMA),根据异烟肼的抗结核分枝杆菌活性对两种化合物进行评估并与异烟肼进行比较。化合物1在H37Rv(易感型)、TB DM 97(耐药野生型)和MDR DM 1098(多药耐药型)菌株的每次测试中具有16.0μg/mL的MIC(最小抑制浓度)值。在类似的试验中,化合物2的MIC值分别为2.0、64.0和64.0μg/mL。
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引用次数: 7
Aporphine alkaloids with antitubercular activity isolated from Ocotea discolor Kunth (Lauraceae) 从樟科变色木中分离到的具有抗结核活性的阿啡生物碱
IF 0.8 Pub Date : 2017-09-01 DOI: 10.15446/REV.COLOMB.QUIM.V46N3.62963
L. T. Albarracin, O. J. Patino, J. Guzman, Neelu Begum, Timothy D McHugh, L. Cuca, M. Ávila
La tuberculosis causa miles de muertes a nivel mundial y que, actualmente, los farmacos usados no son suficientes y en ocasiones son obsoletos para su tratamiento, se hace necesaria la busqueda de nuevos compuestos que ayuden a combatirla. Por tanto, se evaluo la actividad antituberculosis de los alcaloides ocoxilonina (1), ocoteina (2), dicentrina (3) y 1,2-metilendioxi-3, 10,11-trimetoxiaporfina (4), aislados de la madera de Ocotea discolor. Las estructuras fueron identificadas por medio del analisis de los datos espectroscopicos de resonancia magnetica nuclear (NMR 1D – 1H, 13C, 2D – COSY, HSQC y HMBC), espectros de masas y comparacion con datos de la literatura. Todos los compuestos aislados demostraron actividad antituberculosa, con un rango de variacion en la concentracion minima inhibitoria entre 140 y 310 μM, siendo la ocoteina (2) la mas activo contra la cepa virulenta de Mycobacterium tuberculosis H37Rv.
结核病在全球造成数千人死亡,目前使用的药物还不够,有时已经过时,需要寻找新的化合物来帮助对抗结核病。因此,评估了从彩色ocotea木材中分离的生物碱coxylonin(1)、ocoteina(2)、dicentrin(3)和1,2-亚甲基二氧基-3、10,11-三甲氧基Aporfin(4)的抗结核活性。通过分析核磁共振波谱数据(1D-1H、13C、2D-Cosy、HSQC和HMBC)、质谱并与文献数据进行比较,确定了结构。所有分离的化合物都表现出抗结核活性,最低抑制浓度的变化范围在140至310μm之间,其中奥科坦(2)对结核分枝杆菌H37RV毒株最为活跃。
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引用次数: 1
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Revista Colombiana de Quimica
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