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Historical essay of the development of chromatography at the Zaporizhzhia State Medical University. 中国国立医科大学色谱学发展历史随笔。
Pub Date : 2022-12-14 DOI: 10.15407/zht2021.67.056
B. Varynskyi
The purpose of this work is to analyze the chronology and state of development of chromatographic methods at the Zaporizhzhia State Medical University (ZSMU). A historical overview of the use of chromatographic methods at ZSMU is provided. First of all, emphasis is placed on the introduction of high-performance liquid chromatography and gas-liquid chromatography. The main scientific laboratories and groups that worked and are working at the Zaporizhzhia State Medical University in the field of instrumental chromatography are shown. There were groups at the Department of Biological Chemistry, the Department of Faculty Pediatrics, the Department of Physical and Colloidal Chemistry. Currently, the Department of Physical Colloid Chemistry is actively working on a new laboratory of liquid chromato-mass spectrometry of the Department of Experimental Pharmaceutical Research of the training medical-laboratory center. The laboratory performs research for many departments of ZSMU, including the Faculty of Pharmacy, the Faculty of Postgraduate Education, the Faculty of Medicine. The laboratory develops, validates and uses methods to establish the purity and confirm the molecular weight and structure of new biologically active substances synthesized to search for new drugs, research of impurities in drug substances, determination of biologically active substances in extracts of medicinal plant raw materials, determination of residual amounts drugs in poultry meat and eggs, and other livestock and poultry products, determination of concentrations of disease markers, determination of distribution, metabolism and excretion of drugs.
这项工作的目的是分析扎波里日亚国立医科大学(ZSMU)色谱方法的发展历程和状态。提供了ZSMU色谱方法使用的历史概述。首先,重点介绍了高效液相色谱法和气液色谱法。显示了在扎波里日亚国立医科大学从事和正在从事仪器色谱领域工作的主要科学实验室和小组。生物化学系、儿科系、物理和胶体化学系都有小组。目前,物理胶体化学系正在积极筹建一个新的实验室——液相色谱-质谱法实验药物研究系医学实验中心。该实验室为ZSMU的许多部门进行研究,包括药学院、研究生教育学院和医学院。实验室开发、验证和使用方法来建立纯度并确认为寻找新药而合成的新生物活性物质的分子量和结构,研究药物中的杂质,测定药用植物原料提取物中的生物活性物质,测定禽肉和蛋中药物的残留量,以及其他畜禽产品,疾病标志物浓度的测定,药物分布、代谢和排泄的测定。
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引用次数: 0
Effect of Carbonization Temperature on Properties of Char from Canarium schweinfhurthii (Atili) Seed Shell. 炭化温度对金丝雀籽壳炭性能的影响。
Pub Date : 2021-12-22 DOI: 10.15407/zht2021.67.098
A. Sallau, U. Hassan, A. Kolo, A. Jauro, Okon Dominic Ekanem
The effect of carbonization temperature on canarium schweinfhurthii seed shell was investigated. Atili seed shell particles was carbonized at different temperatures of 600, 800, 1000 and 1150°C under inert condition for 60 mins each to obtain char products. The effect of temperature on the properties of char was investigated in detail, using several characterization techniques including, mass yield, elemental analysis, and electrical property measurements while structural transformations were monitored using X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy and scanning electron microscope (SEM) techniques. The char yield decreased from 30.50 % to 26.55 % as the temperature increases from 600°C to 1150°C. The fixed carbon (82.3 to 92.66 %) and ash content (1.35 to 1.72 %) increase as temperature increase while the volatile matter (12.61 to 4.18 %) and moisture content (3.81 to 1.44 %) decreases. Ultimate analysis showed elemental carbon to increase from 85.96 % to 95.79 %. The electrical conductivity of obtained char improved significantly (1.99 x 10-9 to 7.24 x 10-2 S/cm) as well as the structural, morphology and near graphitization of char. Statistical analysis of the FTIR and XRD data via the principal component analysis showed similarity trend on the effect of temperature on the carbonization products. The improved electrical property, pore development in char morphology as well as the development of near graphitization features suggest possible use as electrode materials.
研究了炭化温度对金丝雀籽壳的影响。将Atili籽壳颗粒在600、800、1000和1150°C的不同温度下在惰性条件下碳化60分钟,以获得焦炭产物。使用几种表征技术,包括质量产率、元素分析和电性能测量,详细研究了温度对焦炭性能的影响,同时使用X射线衍射、傅里叶变换红外光谱和扫描电子显微镜技术监测结构转变。随着温度从600°C升高到1150°C,焦炭产率从30.50%下降到26.55%。随着温度的升高,固定碳(82.3%至92.66%)和灰分(1.35%至1.72%)增加,而挥发性物质(12.61%至4.18%)和水分含量(3.81%至1.44%)降低。最终分析表明,元素碳从85.96%增加到95.79%。所得炭的电导率显著提高(1.99×10-9至7.24×10-2 S/cm),炭的结构、形态和接近石墨化程度也得到了改善。通过主成分分析对FTIR和XRD数据的统计分析表明,温度对炭化产物的影响有相似的趋势。电性能的改善、焦炭形态中的孔隙发展以及近石墨化特征的发展表明有可能用作电极材料。
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引用次数: 0
Development of micellar liquid and thin-layer chromatography. 胶束液相色谱和薄层色谱的发展。
Pub Date : 2021-11-11 DOI: 10.15407/zht2021.67.004
A. Kulikov
The review of the development of micellar high-performance liquid chromatography and micellar thin-layer chromatography is presented. The results of the research of the theoretical foundation and the organized solution usage as mobile phases for the analysis of plant and animal biological active substances, medicinal substances and drugs are demonstrated. The investigations had been carried out on the Chemical Metrology Department V.N. Karazin Kharkiv National University and in the State Enterprise “Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines”.
综述了胶束高效液相色谱法和胶束薄层色谱法的研究进展。论证了作为动植物生物活性物质、药用物质和药物分析流动相的理论基础和有组织的溶液用途的研究结果。调查是在化学计量部门V.N.卡拉津哈尔科夫国立大学和国有企业“乌克兰药物质量科学药理学中心”进行的。
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引用次数: 0
Practical application of high-performance liquid chromatography and high-performance thin-layer chromatography in pharmaceutical analysis. 高效液相色谱和高效薄层色谱在药物分析中的实际应用。
Pub Date : 2021-09-21 DOI: 10.15407/zht2021.67.046
A. Yegorova, Y. Scrypynets, G. Fedosenko, G. Maltsev, S. Kashutskiy
Currently, chromatographic methods are widely used to control the quality of products in the pharmaceutical and food industries. This article is devoted to the systematization of the results of scientific research of the authors on the development, validation and application of a number of chromatographic methods in the creation of generic drugs, as well as in the analysis of medicinal plant materials. The developed methods are validated according to the following parameters: specificity, linearity, accuracy and limit of detection. The specificity of the methods is based on the ability to evaluate the analyte in the presence of other components and is confirmed by using external standards. The accuracy was assessed by the results of the analysis of different weights or by the "added-found" method. For the developed methods, parameters of the suitability of chromatographic systems were established (peak symmetry factor, number of theoretical plates, relative standard deviation of retention time and peak area).
目前,色谱法在制药和食品行业被广泛用于控制产品质量。本文致力于系统化作者在开发、验证和应用多种色谱方法开发仿制药以及分析药用植物材料方面的科学研究结果。根据以下参数对所开发的方法进行了验证:特异性、线性、准确性和检测限。该方法的特异性基于在存在其他成分的情况下评估分析物的能力,并通过使用外部标准进行确认。准确性通过不同权重的分析结果或“添加-发现”方法进行评估。对于所开发的方法,建立了色谱系统适用性的参数(峰对称因子、理论板数、保留时间和峰面积的相对标准偏差)。
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引用次数: 0
Development of chromatography at the Department of Analytical Chemistry of National Taras Shevchenko University of Kyiv. 基辅国立塔拉斯舍甫琴科大学分析化学系色谱法的发展。
Pub Date : 2021-09-10 DOI: 10.15407/zht2021.67.066
M. Zuy, M. A. Ishchenko, T. Keda, V. Doroshchuk, S. Kulichenko, O. Lysenko, V. Raks, O. Tananaiko
An information about teaching and scientific activities in the field of chromatographic methods of analysis at the Department of Analytical Chemistry of the National Taras Shevchenko University of Kiev for the period from the 70s of the twentieth century till present days given. The perspective directions of the development of academic disciplines and scientific research of the department in this area are outlined.
基辅国立塔拉斯-舍甫琴科大学分析化学系色谱分析方法领域从20世纪70年代至今的教学和科学活动信息。概述了该系在这一领域学术学科和科学研究发展的前景方向。
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引用次数: 0
Development of ion chromatography in Ukraine. 离子色谱法在乌克兰的发展。
Pub Date : 2021-09-04 DOI: 10.15407/zht2021.67.039
O. Zui
The ways of development of ion chromatography in Ukraine from the eighties of the last century to the present time are shown. The achievements of research institutes, in particular, the Dumansky Institute of Colloid Chemistry and Water Chemistry of the National Academy of Sciences of Ukraine, in the development of ion chromatographic methods for the analysis of organic and inorganic anions in various objects, including natural and drinking waters, are highlighted. Scientists of Ukraine (A.T. Pilipenko, O.V. Zuy, A.V. Terletskaya) compared commercially available sorbents for ion chromatography – HIKS-1, ANIEKS-N and KANK ASt for their use in water analysis. The studies were carried out on an ion chromatograph "Tsvet-3006" with a conductometric detector. It has been shown that ANIEKS-N with a borate eluent is the best sorbent for the determination of organic monocarboxylic acid ions, and KANK ASt with a carbonate-hydrocarbonate eluent – for the determination of inorganic anions. Ion chromatography has been used to solve a number of practical problems: for the separation of oxoanions  iodate, chlorate and bromate in waters, to control the results in the development of chemiluminescent methods for the determination of chloride, nitrite and nitrate, to establish the mechanism of destruction of anionic surfactants under the action of vacuum ultraviolet radiation and corona discharge. The method was applied to the analysis of iodine-containing bottled waters for bromide ions due to the absence of the interference from iodides. The accumulated experience has contributed to the adoption in Ukraine of four state standards for water quality, based on the use of the ion chromatographic method. It is shown that the method of ion chromatography at the present stage is widely used in various sectors of the national economy: to determine the traces of anions in steam condensate of power plants, to control the anionic composition of water at nuclear power plants, to correct water treatment processes at waterworks, in particular, when analyzing chlorite ions in tap water obtained with the use of chlorine dioxide as a disinfectant.
介绍了乌克兰离子色谱法从上世纪八十年代到现在的发展情况。重点介绍了研究机构,特别是乌克兰国家科学院杜曼斯基胶体化学和水化学研究所在开发用于分析各种物体(包括天然和饮用水)中的有机和无机阴离子的离子色谱方法方面取得的成就。乌克兰科学家(A.T. Pilipenko, O.V. Zuy, A.V. Terletskaya)比较了市售离子色谱吸附剂- HIKS-1, ANIEKS-N和KANK ASt在水分析中的应用。研究是在带有电导检测器的“Tsvet-3006”离子色谱仪上进行的。结果表明,硼酸盐洗脱液的ANIEKS-N是测定有机单羧酸离子的最佳吸附剂,碳酸盐-碳酸盐洗脱液的KANK - ASt是测定无机阴离子的最佳吸附剂。离子色谱法已被用于解决许多实际问题:用于水中氧阴离子的分离,用于控制氯、亚硝酸盐和硝酸盐的化学发光测定方法的结果,用于建立真空紫外线辐射和电晕放电作用下阴离子表面活性剂的破坏机理。由于没有碘离子的干扰,本方法应用于含碘瓶装水中溴化物离子的分析。积累的经验有助于乌克兰在使用离子色谱法的基础上通过四项国家水质标准。结果表明,现阶段离子色谱法已广泛应用于国民经济的各个部门:测定电厂蒸汽冷凝水中阴离子的痕量,控制核电站水的阴离子组成,纠正自来水厂的水处理工艺,特别是分析用二氧化氯作为消毒剂获得的自来水中的亚氯酸盐离子。
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引用次数: 0
Development of chromatographic research in Lviv region. 利沃夫地区色谱研究进展。
Pub Date : 2021-09-02 DOI: 10.15407/zht2021.67.77
I. Poliuzhyn, M. Gertsiuk
Scientific research in the field of chromatography has been intensively developed and continues to develop in higher educational institutions of Lviv, research institutes, which is due to the widespread use of chromatographic methods of analysis in the scientific field, at enterprises of Lviv region, in the practice of controlling laboratories. Among the scientific achievements of scientists of Lviv region should be noted research in the field of the use of zeolites and other sorbents in chromatogaphy, the study of chemical reactions, the development and application of methods for analysis in the field of medicine, biology, veterinary, medicine, industrial products and environmental objects. Higher educational institutions of Lviv provide training of qualified chromatography specialists. Established cooperation of scientific laboratories and laboratories in industry, which contributes to the development and implementation of new methods of chromatographic analysis in practice.
色谱学领域的科学研究在利沃夫的高等教育机构、研究机构中得到了深入的发展,并将继续发展,这是由于色谱分析方法在科学领域、利沃夫地区的企业、控制实验室的实践中得到了广泛的应用。在利沃夫地区科学家的科学成就中,应该注意到在色谱中使用沸石和其他吸附剂领域的研究,化学反应的研究,医学,生物学,兽医,医学,工业产品和环境对象领域的分析方法的开发和应用。利沃夫的高等教育机构提供合格色谱专家的培训。建立了科学实验室和工业实验室的合作关系,促进了色谱分析新方法的开发和实施。
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引用次数: 0
Determination of curcumin in bouillon cubes by high-performance thin-layer chromatography 高效薄层色谱法测定肉汤中姜黄素的含量
Pub Date : 2021-02-18 DOI: 10.15407/zht2020.66.004
A. Yegorova, Y. Loskutova, G. Voitiuk, A. Maltsev, E. Malinka, Y. Scrypynets
Currently, high-performance thin-layer chromatography (HPTLC) is widely used to control product quality in the pharmaceutical and food industries. In the manufacture of food products, the most important requirement is the control of the content of various additives (preservatives, dyes, antioxidants). For the first time, a method for determining curcumin by high-performance thin-layer chromatography in bouillon cubes "Gallina Blanca" was proposed. Detection was carried out by densitometric scanning using CAMAG equipment when measuring absorbance at a wavelength 265 nm. The method is based on determining the peak area of curcumin in the chromatogram depending on its concentration. Curcumin content is determined by the calibration curve. The developed method was validated by the following tests: specificity, linearity, accuracy and detection limit. The calibration curve is linear in the range of curcumin concentrations from 120 to 520 ng/spot, the detection limit is 65 ng/spot. The specificity of the method is based on the ability to unambiguously evaluate the analyte in the presence of other components and is confirmed by using an external standard. The spots on the chromatograms of the test solution and the reference solution coincide in the value of Rf, which confirms the specificity of the method. Accuracy was evaluated according to the results of the analysis of various samples. The requirement for statistical insignificance of systematic error is fulfilled. The proposed method is express, characterized by satisfactory metrological characteristics, ease of implementation. Key words: high-performance thin-layer chromatography, curcumin, validation.
目前,高效薄层色谱法(HPTLC)在制药和食品行业被广泛用于控制产品质量。在食品生产中,最重要的要求是控制各种添加剂(防腐剂、染料、抗氧化剂)的含量。首次提出了一种用高效薄层色谱法测定高卢汤中姜黄素含量的方法。当测量波长265nm处的吸光度时,使用CAMAG设备通过密度计扫描进行检测。该方法基于根据姜黄素浓度确定色谱图中姜黄素的峰面积。姜黄素含量由校准曲线确定。所开发的方法通过以下测试进行了验证:特异性、线性、准确度和检测限。在姜黄素浓度为120至520纳克/点的范围内,校准曲线呈线性,检测限为65纳克/点。该方法的特异性基于在存在其他成分的情况下明确评估分析物的能力,并通过使用外部标准进行确认。供试品溶液和对照品溶液色谱图上的斑点在Rf值上一致,这证实了该方法的特异性。根据各种样品的分析结果来评估准确性。满足了系统误差在统计上不重要的要求。所提出的方法是快速的,具有令人满意的计量特性,易于实施。关键词:高效薄层色谱法,姜黄素,验证。
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引用次数: 0
Herbicides from the group of nitrodiphenyl ethers: applications in Ukraine, control methods, methods for determination of oxifluorphene residues in soybean grain and oil 硝基二苯醚类除草剂:在乌克兰的应用,控制方法,大豆籽粒和豆油中氧化氟苯残留量的测定方法
Pub Date : 2021-02-18 DOI: 10.15407/zht2020.66.015
Y. Baranov, V. Demchenko, I. Zajets, S. Olszewski
A review of analytical methods for the determination of herbicide residues from the group of nitrodiphenyl ethers in the environment and agricultural products, developed and validated a method for oxyfluorfen determination in soybean grain and oil method GC/ECD, which meets regulatory requirements and solves the problem of toxicant control in the above matrices. The developed method uses modern methods of sample preparation, identification and quantification of oxyfluorfen (selective extraction, capillary gas-liquid chromatography (GC/ECD GC/MS). The method is validated according to EU requirements) (SANTE/12682/2019 quality control and analytical validation procedures for pesticide residues analysis in food and feed). Key words: gas-liquid chromatography, mass spectrometry, herbicides, nitrodiphenyl ethers, control, residual amounts.
综述了测定环境和农产品中硝基二苯醚类除草剂残留量的分析方法,开发并验证了大豆粮油中氧氟芬的GC/ECD测定方法,该方法符合监管要求,解决了上述基质中毒物控制的问题。所开发的方法使用了氧氟芬的现代样品制备、鉴定和定量方法(选择性提取、毛细管气相色谱法(GC/ECD GC/MS))。该方法根据欧盟要求进行验证)(SANTE/12682/2019食品和饲料中农药残留分析的质量控制和分析验证程序)。关键词:气液色谱、质谱、除草剂、硝基二苯醚、对照、残留量。
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引用次数: 0
Improvement of analytical determination of residual quantities of active substances of the triasole class in juices 果汁中三索类活性物质残留量分析测定方法的改进
Pub Date : 2020-11-24 DOI: 10.15407/zht2020.66.024
O. Vavrinevych, D. Hyrenko, T. Hyrenko, S. Omelchuk, A. Syrota
Today, the most common among fungicides approved for use in Ukraine, as well as in other countries, are compounds of the triazole class. Juices, as a product of processing agricultural raw materials, can be consumed by a wide range of the population. The purpose of work was to develop analytical methods for compound of triazole (difenoconazole and propiconazole) in juices to ensure quality control of agricultural products grown with the use of these fungicides. Conditions for chromatography of difenoconazole and propiconazole using gas-liquid chromatography with capillary column SH-Rxi-5ms (30 m 0,25 mm) and electron capture detector were determined. Optimal conditions of difenoconazole chromatography were established: thermostat column temperature - 280 C, evaporator temperature - 290 C, detector thermostat temperature - 300 C. Retention time: isomer 1 - (6,91 +- 0,1) minutes, isomer 2 - (7,04 +- 0,1) minutes. The linear range of detection is 0,01-0,04 ug/cm3. The optimal conditions for chromatography of propiconazole were also established: the temperature of the column thermostat in the programming mode: initial T - 100 C with an exposure of 1 minute; from 90 C to 260 C - rate of temperature rise 40 C/min; exposure - 7,45 minutes; evaporator temperature - 270 C, detector temperature - 280 C. The retention time under these conditions was 3,49 +- 0,1 minutes for isomer 1 and 3,57 +- 0,1 minutes for isomer 2. The linear range of detection is 0,01-0,05 ug/cm3. The calibration dependence of the area of peaks of the investigated substances on their concentration was established and described by the linear regression equation.
今天,在乌克兰和其他国家批准使用的杀菌剂中,最常见的是三唑类化合物。果汁作为一种加工农业原料的产品,可以被广泛的人群消费。本研究旨在建立果汁中三唑(二苯醚康唑和丙环康唑)化合物的分析方法,以保证使用这些杀菌剂生长的农产品的质量控制。采用气液色谱法,采用SH-Rxi-5ms毛细管柱(30 m,25 mm)和电子捕获检测器,确定了二苯醚康唑和丙环康唑的色谱条件。建立了二苯醚康唑色谱的最佳条件:恒温柱温- 280℃,蒸发器温度- 290℃,检测器恒温温度- 300℃。保留时间:异构体1 - (6,91 +- 0,1)min,异构体2 - (7,04 +- 0,1)min。检测线性范围为0.01 ~ 0.04 ug/cm3。确定了丙环唑色谱的最佳条件:柱恒温器在编程模式下,初始温度为T ~ 100℃,曝光时间为1分钟;从90℃至260℃-升温速率40℃/min;暴露- 7,45分钟;在此条件下,异构体1的保留时间为3.49 +- 0.1 min,异构体2的保留时间为3.57 +- 0.1 min。检测线性范围为0.01 ~ 0.05 ug/cm3。建立了所研究物质的峰面积随其浓度的定标关系,并用线性回归方程描述了该关系。
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引用次数: 0
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