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Analysis of Nitroaromatics: A Comparison Between Gas Chromatography, Liquid Chromatography and their Hyphenation with Solid Phase Micro-Extraction 硝基芳烃的分析:气相色谱法、液相色谱法及其固相微萃取联用的比较
Pub Date : 2019-09-18 DOI: 10.2174/2213240606666190423122358
P. Y. Ajmal, R. Bhangare, M. Tiwari, S. Sahu
A major class of nitro-explosives being used in military and commercialpurposes belongs to organic compounds containing nitro (NO2) groups like nitrobenzene, nitrotoluenes,and nitramines. Apart from being energetic materials, these substances are inherentlytoxic to human beings. These substances may find their way into different environmental matricesfrom the site of their military or commercial applications. They are present in nature at ultra-tracelevels.Chromatographic techniques have been widely used for the detection and quantificationof nitro-explosives from various environmental matrices. The current study involves a comparisonof the performance of liquid and gas chromatography with and without pre-concentration techniqueslike Solid Phase Micro-extraction (SPME) to detect ultra-trace levels nitrobenzene and nitrotoluenesin water.The addition of SPME to chromatographic techniques significantly improves the qualityof the analysis in terms of ease and sensitivity. Both SPME-HPLC and SPME-GC are equallycompetent techniques for the analysis of nitroaromatic explosives from water. Detection limitswere improved by upto 5 orders of magnitude by these methods.The methodology for determining nitroaromatic explosives in water samples hasbeen optimized and validated after trying four different methods and comparing their performance.GC and HPLC techniques used alone cannot be sensitive enough to detect these compoundsat ultra-trace levels. Both SPME-HPLC-UV and SPME-GC-FID are equally competent techniques.SPME method has been proved to be an excellent tool with no requirement of any tedioussample preparation and chemical processing of the samples.
用于军事和商业目的的一类主要的硝基炸药属于含有硝基(NO2)基团的有机化合物,如硝基苯、硝基甲苯和硝胺。这些物质除了是高能物质外,对人类本身也是有毒的。这些物质可能会从它们的军事或商业应用场所进入不同的环境基质。它们以超痕量水平存在于自然界中。色谱技术已广泛应用于各种环境基质中硝基炸药的检测和定量。目前的研究涉及比较液相和气相色谱法在检测水中超痕量硝基苯和硝基甲苯时,使用和不使用固相微萃取(SPME)等预浓缩技术的性能。在色谱技术中加入SPME可显著提高分析质量,使分析更加容易和敏感。SPME-HPLC和SPME-GC都是分析水中硝基芳香族炸药的有效方法。检测限提高了5个数量级。对水样中硝基芳香族炸药的测定方法进行了优化和验证,并对四种方法进行了性能比较。单独使用气相色谱和高效液相色谱技术不能足够灵敏地检测这些超痕量水平的化合物。SPME-HPLC-UV和SPME-GC-FID都是同样有效的技术。SPME法已被证明是一种极好的工具,不需要任何繁琐的样品制备和样品的化学处理。
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引用次数: 0
Quantitative Explanation of Retention Mechanisms in Reversed-phase Mode Liquid Chromatography, and Utilization of Typical Reversed-phase Liquid Chromatography for Drug Discovery 反相模式液相色谱保留机制的定量解释及典型反相液相色谱在药物发现中的应用
Pub Date : 2019-09-18 DOI: 10.2174/2213240606666190619120733
T. Hanai
The retention mechanism in reversed-phase liquid chromatography was quantitativelydescribed using log P (octanol-water partition coefficient). The hydrophobic (lipophilic) interactionliquid chromatography was then used to measure the hydrophobicity of a variety of compounds.Furthermore, the technique has been used as an analytical method to determine molecularproperties during the drug discovery process. However, log P values cannot be applied to otherchromatographic techniques. Therefore, the direct calculation of molecular interactions was proposedto describe the general retention mechanisms in chromatography. The retention mechanismsin reversed-phase liquid chromatography were quantitatively described in silico by using simplemodel compounds and phases. The competitive interactions between a bonded-phase and a solventphase clearly demonstrated the retention mechanisms in reversed-phase liquid chromatography.Chromatographic behavior of acidic drugs on a pentyl-, an octyl-, and a hexenyl-phase was quantitativelydescribed in the in silico analysis. Their retention was based on their hydrophobicity, andhydrogen bonding and electrostatic interaction were selectivity of the hexenyl-phase. This reviewfocuses on the quantitative explanation of the retention mechanisms in reversed-phase liquidchromatography and the practical applications in drug discovery.
用log P(辛醇-水分配系数)定量描述了辛醇-水在反相液相色谱中的保留机理。然后用疏水(亲脂)相互作用液相色谱法测定了各种化合物的疏水性。此外,该技术已被用作药物发现过程中确定分子性质的分析方法。然而,对数P值不能应用于其他色谱技术。因此,提出了直接计算分子相互作用来描述色谱中一般的保留机制。用简单模型化合物和相对反相液相色谱中的保留机理进行了定量描述。结合相和溶剂相之间的竞争性相互作用清楚地证明了反相液相色谱中的保留机制。在硅分析中定量描述了酸性药物在戊基、辛基和己基相上的色谱行为。它们的保留是基于它们的疏水性,氢键和静电相互作用是对己基相的选择性。本文综述了反相液相色谱保留机制的定量解释及其在药物发现中的实际应用。
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引用次数: 5
Distribution of Quercetin in Different Organs of Male Sprague Dawley Rats Under Hypoxia: A High-Performance Thin Layer Chromatography Approach 低氧条件下雄性大鼠不同脏器中槲皮素的分布:高效薄层色谱法
Pub Date : 2019-07-25 DOI: 10.2174/2213240606666190725104244
A. Tripathi, Jigni Mishra, Anuja Bhardwaj, K. Misra, Sarada S K Sagi
Quercetin (3’,3’,4,5,7-pentahydroxyflavonol), a natural flavonoid found infruits, vegetables, beverages, and other phytoproducts, exerts multiple health benefits including a reductionin hypoxia-induced oxidative stress, inflammation, lipid peroxidation, allergic disorders,neurodegenerative disorders, and cardiovascular diseases.Despite knowledge of such therapeutic efficacy of quercetin to human health, there islimited literature available that sheds light on an organ-wise distribution of quercetin. Therefore, thecurrent study was performed to accurately estimate the distribution of quercetin in its supplementedform in different tissues of a mammalian model, i.e., male Sprague Dawley (SD) rats.The rats were exposed to different durations (1 h, 3 h, 6 h, and 12 h) of hypoxiain a simulated hypobaric hypoxia chamber, with parameters maintained at 8 % O2 and 282 mmHg, following which they were sacrificed. Plasma and different tissue samples were duly collected.A high-performance thin layer chromatography (HPTLC) approach was employed for the first time,using our own reported method, along with an optimized sample preparation procedure for quercetindetermination. Briefly, the samples were developed in a mobile phase constituted of ethyl acetate,dichloromethane, methanol, formic acid, and glacial acetic acid.Distinct bands of quercetin in resultant HPTLC profiles verified that theamount of quercetin varied among different tissues, with varying durations to hypoxia exposure.Quercetin was substantially retained in vital organs namely, lungs, liver, and heart for relativelylonger durations.The present study established HPTLC as an efficient and high throughput tool, leading toa satisfactory evaluation of the amount of quercetin present in various tissue samples under hypoxia.
槲皮素(3 ',3 ',4,5,7-五羟基黄酮醇)是一种天然类黄酮,存在于水果、蔬菜、饮料和其他植物产品中,具有多种健康益处,包括减少缺氧诱导的氧化应激、炎症、脂质过氧化、过敏性疾病、神经退行性疾病和心血管疾病。尽管知道槲皮素对人体健康的这种治疗功效,但现有的文献有限,阐明了槲皮素的器官分布。因此,本研究旨在准确估计槲皮素补充形式在哺乳动物模型(即雄性SD大鼠)不同组织中的分布。将大鼠置于模拟低压缺氧舱中,在8 % O2和282 mmHg的条件下,连续缺氧1、3、6、12小时,然后处死。及时收集血浆和不同组织样本。本文首次采用高效薄层色谱法(HPTLC)测定槲皮素的含量,并优化了样品制备工艺。简单地说,样品在由乙酸乙酯、二氯甲烷、甲醇、甲酸和冰醋酸组成的流动相中进行冲洗。槲皮素在HPTLC图谱中的不同条带证实,槲皮素的含量在不同组织中随缺氧暴露时间的不同而变化。槲皮素在肺、肝和心脏等重要器官中保留的时间相对较长。本研究建立了HPTLC作为一种高效、高通量的工具,在缺氧条件下对各种组织样品中槲皮素的含量进行了满意的评估。
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引用次数: 0
Unusual Regularity in GC Retention of Simple Amino Acid Derivatives. 简单氨基酸衍生物气相色谱保留的异常规律。
Pub Date : 2019-05-01 DOI: 10.2174/2213240606666190709100858
I. Zenkevich, Nino G. Todua, A. Mikaia
BackgroundApplication of simple regularities and general principles along with direct use of reference gas chromatography retention index data for reliable structure determination of compounds can be enhanced by determination of new regularities that are specific to certain structural elements.ObjectiveRevelation and interpretation of an anomaly in the elution order of alkyl esters of alkoxycarbonyl derivatives of glycine and alanine on standard and semi-standard non-polar phases.MethodPreliminary derivatization of amino acids to alkyl esters of N-alkoxycarbonyl analogs and interpretation of their gas chromatographic characteristics.ResultsAlkyl esters of N-alkoxycarbonyl derivatives of alanine (Alkyl = C2H5, n- and iso-C3H7) elute prior to the same derivatives of glycine, despite the presence of an additional methyl group at C(2) in the molecule. Elution order is reversed for methyl esters of N-methoxycarbonyl derivatives.ConclusionIt is established that the peculiar behavior of alkyl esters of N-alkoxycarbonyl derivatives of glycine and alanine agrees with the concepts of gas chromatography and the known retention index regularities of organic compounds. A decrease of retention index values is a result of an introduction of an additional methyl group to a carbon atom connected to two polar fragments in a molecule like CH2XY. The dependence of the difference of retention index values for homologs of the types of CH3-CHXY and CH2XY vs. the total mass of fragments (X + Y) is similar to those for other sub-groups of analytes.
通过确定特定结构元素的新规律,可以增强对简单规律和一般原理的应用以及直接使用参考气相色谱保留指数数据进行可靠的化合物结构测定。目的探讨甘氨酸和丙氨酸烷氧羰基衍生物的烷基酯在标准和半标准非极性相上的异常洗脱顺序。方法将氨基酸初步衍生为n -烷氧羰基类似物的烷基酯,并分析其气相色谱特征。结果丙氨酸的n-烷氧羰基衍生物(烷基= C2H5, n-和iso-C3H7)的烷基酯比甘氨酸的相同衍生物更容易被洗脱,尽管在分子的C(2)处存在一个额外的甲基。n -甲氧羰基衍生物甲酯的洗脱顺序相反。结论甘氨酸和丙氨酸的n -烷氧羰基衍生物的烷基酯的特殊行为符合气相色谱的概念和已知的有机化合物的保留指数规律。在像CH2XY这样的分子中,与两个极性片段相连的碳原子上引入一个额外的甲基会导致保留指数值的降低。CH3-CHXY和CH2XY类型同源物的保留指标值差异与片段总质量(X + Y)的相关性与其他亚群分析物相似。
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引用次数: 1
A Modified QuEChERS Extraction and LC-MS/MS Method for the Determination of Pesticide Residues in Curry Leaves (Murraya koenigii) 改良QuEChERS萃取- LC-MS/MS法测定咖喱叶中农药残留
Pub Date : 2019-05-01 DOI: 10.2174/2213240606666181226143757
Ranjith Arimboor, K. R. Menon, N. Babu, Haneesh Chandran
Increased consumer demand for curry leaves free from pesticides demands fast and reliable analytical methods for the analysis of pesticide residues.The optimization of a QuEChERS based sample preparation technique with improved analytical accuracy by removing interfering matrix components for LC-MS/MS analysis of pesticide residues from curry leaves.A modified QuEChERS solid phase extraction method was developed and validated for the analysis of 26 pesticides in fresh and dried curry leaves. The effects of the sample preparation steps and column retention time on the matrix suppression of analyte ions were also evaluated.Validation parameters were found within an acceptable range. The matrix effect evaluation studies showed that the QuEChERS sample preparation was able to minimize the ion suppression of analytes due to co-eluting matrix of components and that a d-SPE clean up step had major role in reducing matrix effect. The gradient mobile phase with longer retention time for analytes resulted in comparatively lesser matrix effects than the isocratic mobile phase of non-polar nature. Even after the clean up, a considerable number of compounds had more than 20% reduction in their MS response in the gradient mobile phase.This study emphasized the need of proper sample clean up before a LC-MS/MS analysis and the usage of matrix matched standards and mobile phase that ultimately results in an appropriate analyte separation in reasonable retention times.
消费者对无农药咖喱叶的需求不断增加,对快速、可靠的农药残留分析方法提出了要求。基于QuEChERS的样品制备技术优化,去除干扰基质成分,提高分析精度,用于hplc -MS/MS分析咖喱叶中农药残留。建立了一种改进的QuEChERS固相萃取法,并对鲜咖喱叶和干咖喱叶中26种农药进行了分析。考察了样品制备步骤和柱保留时间对基质抑制分析离子的影响。验证参数在可接受范围内。基质效应评价研究表明,QuEChERS样品制备能够最大限度地减少组分基质共洗脱对分析物的离子抑制,d-SPE清理步骤对降低基质效应起主要作用。与非极性等压流动相相比,具有较长停留时间的梯度流动相的基质效应相对较小。即使在清理后,相当多的化合物在梯度流动相的MS响应也降低了20%以上。本研究强调在LC-MS/MS分析前需要适当的样品清理,使用基质匹配的标准品和流动相,最终在合理的保留时间内得到适当的分析物分离。
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引用次数: 2
Manuscripts from Different Brands of Ballpoint Pens – GC/MS Ageing Profile in Brazilian Tropical Weather 不同品牌的圆珠笔手稿-巴西热带气候下的GC/MS老化特征
Pub Date : 2019-05-01 DOI: 10.2174/2213240606666190410152956
Carina Maria Bello de Carvalho, Scorsatto R. Ortiz, R. Limberger
Dating of ballpoint pen manuscripts in forensic documents is still a challengefor experts. Methods of ink dating consider solvent evaporation through time, especially 2-phenoxyethanol (2-PE).The objective of the researchers was to perform a continued study with pen ink strokesof ballpoint pens commercialized in Brazil, to characterize the ageing profile of 15 brands of blueand black pens.Solvent composition analysis of ballpoint pen ink lines written in white and recycledpaper was performed by gas chromatography/mass spectrometry, to quantify 2-PE, in recentlywritten lines and in lines aged 4, 18, 27 and 36 months.The results showed that the pens had initial quantities of 2-PE smaller than in the Europedespite of having similar ageing behavior. Such kind of paper had more influence on aged penstrokes than in the recently applied pen strokes. Light and heat accelerated ageing. Some pensstopped ageing at 18, 27 and 36 months.The results obtained were promising for elucidation of the ageing behavior of pen inklines in tropical weather, but further statistical treatments could be done to adequate interpretationin real cases.
鉴定法医文件中圆珠笔手稿的年代对专家来说仍然是一个挑战。油墨测年的方法考虑溶剂随时间的蒸发,特别是2-苯氧乙醇(2-PE)。研究人员的目的是对巴西商业化的圆珠笔的笔触进行持续研究,以表征15个品牌的蓝色和黑色钢笔的老化特征。采用气相色谱/质谱法对白色和再生纸书写的圆珠笔墨水线进行溶剂成分分析,以定量最近书写的线条和4、18、27和36个月的线条中的2-PE。结果表明,尽管具有相似的老化行为,但这些笔的初始2-PE数量比欧洲少。这种纸对旧笔法的影响比新近使用的笔法更大。光和热加速老化。一些人在18个月、27个月和36个月时停止衰老。所获得的结果对于解释笔墨线在热带天气下的老化行为是有希望的,但在实际情况下,进一步的统计处理可以做充分的解释。
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引用次数: 3
Development and Validation of a Novel HPLC Method for the Analysis and Quantification of Dehydroleucodine in Plant Extracts 植物提取物中去氢亮碱的高效液相色谱分析与定量方法的建立与验证
Pub Date : 2019-01-11 DOI: 10.2174/2213240605666181109154409
M. Mariani, A. Penissi
Fil: Mariani, Maria Laura Lucia. Consejo Nacional de Investigaciones Cientificas y Tecnicas. Centro Cientifico Tecnologico Conicet - Mendoza. Instituto de Histologia y Embriologia de Mendoza Dr. Mario H. Burgos. Universidad Nacional de Cuyo. Facultad de Ciencias Medicas. Instituto de Histologia y Embriologia de Mendoza Dr. Mario H. Burgos; Argentina
线程:Mariani, Maria Laura Lucia。国家科学技术研究委员会。科学技术中心Conicet - Mendoza。门多萨组织与胚胎研究所Mario H. Burgos博士。库约国立大学。医学科学学院。门多萨组织学和胚胎学研究所Mario H. Burgos博士;阿根廷
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引用次数: 0
Effect of Organic Modifier on Elution Behavior of Voriconazole in Supercritical Fluid Chromatography: Development of Validated SFC Method 有机改性剂对伏立康唑在超临界流体色谱中洗脱行为的影响:验证SFC方法的建立
Pub Date : 2019-01-11 DOI: 10.2174/2213240605666180912144153
P. Porwal, S. Sawant, S. Tambe
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引用次数: 0
Analytical Methodologies Used in Nanoparticles Remediation Processes for Monitoring of Organic Pollutants. An Overview 用于监测有机污染物的纳米颗粒修复过程的分析方法。概述
Pub Date : 2019-01-11 DOI: 10.2174/2213240605666180810104156
M. L. Alonso, N. Ayarza, I. S. Román, L. Bartolomé, R. Alonso
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引用次数: 1
Core-shell Particles: A Way to Greening Liquid Chromatography in Environmental Applications 核-壳颗粒:绿色液相色谱在环境应用中的一种方法
Pub Date : 2019-01-11 DOI: 10.2174/2213240605666180913100054
C. Waterlot, A. Ghinet, E. Lipka
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引用次数: 8
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