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Supramolecular solvents based on quaternary ammonium salts and perfluorinated compounds for dispersive liquid-liquid microextraction of phthalates 基于季铵盐和全氟化合物的超分子溶剂分散液-液微萃取邻苯二甲酸盐
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4808
Vytautas Kavaliauskas, V. Olšauskaitė, A. Padarauskas
In this study, eight hydrophobic supramolecular (SUPRA) solvents composed of tetrabutylammonium chloride and tetradecyltrimethylammonium bromide as amphiphiles and four perfluorinated compounds (hexafluoroisopropanol, trifluoroacetic acid, pentafluoropropionic acid and heptafluorobutyric acid) as coacervation-inducing agents were developed. The SUPRA phase volumes were determined as a function of individual concentrations of the system components. The extraction properties of the SUPRA solvents for the extraction of phthalates from the model aqueous solutions were investigated and their applicability as sample diluents for the reversed-phase HPLC separations of phthalates was tested. Finally, the solvent consisting of tetradecyltrimethylammonium bromide and hexafluoroisopropanol was applied for dispersive liquid-liquid microextraction of phthalates from wastewater samples prior to HPLC analysis. Under optimised extraction conditions, the enrichment factors were around 75. The calibration curves were linear (R2 ≥ 0.9965) for the concentration level between 1.00 and 50.0 μg/L and the detection limits were in the range 0.3–0.6 μg/L. The recoveries of the phthalates of the developed method for the spiked wastewater samples were 93.1–104.4%, with the relative standard deviation values less than 7.4%.
本研究以四丁基氯化铵和十四烷基三甲基溴化铵为两亲体,以四种全氟化合物(六氟异丙醇、三氟乙酸、五氟丙酸和七氟丁酸)为凝聚剂,制备了八种疏水超分子(SUPRA)溶剂。确定了SUPRA相体积作为系统组分单个浓度的函数。研究了SUPRA溶剂从模型水溶液中提取邻苯二甲酸酯的萃取性能,并测试了其作为邻苯二甲酸酯反相HPLC分离样品稀释剂的适用性。最后,采用十四烷基三甲基溴化铵和六氟异丙醇组成的溶剂,对废水样品中的邻苯二甲酸盐进行分散液液微萃取,然后进行HPLC分析。在优化的提取条件下,富集因子在75左右。浓度水平在1.00 ~ 50.0 μg/L范围内,校准曲线呈线性(R2≥0.9965),检出限在0.3 ~ 0.6 μg/L范围内。该方法对加标废水样品的邻苯二甲酸盐回收率为93.1 ~ 104.4%,相对标准偏差值小于7.4%。
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引用次数: 1
Aqueous sol–gel synthesis, thermoanalytical, structural and vibrational studies of lithium aluminium molybdate (LiAlMo2O8) 钼酸铝锂(LiAlMo2O8)的水溶胶-凝胶合成、热分析、结构和振动研究
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4806
A. Žalga, Austėja Diktanaitė, Giedrė Gaidamavičienė
Aqueous tartaric acid-assisted sol–gel preparation technique was successfully applied to synthesise lithium aluminium molybdate with the initial composition of LiAl(MoO4)2. From the results of the thermal analysis and Xray diffraction measurement, the effect of tartaric acid as a ligand on the formation of homogeneous gel precursor was discussed. Besides, X-ray diffraction also revealed the crystallisation of the final LiAlMo2O8 ceramic below the temperature of 400°C. It was found that the initial composition of obtained ceramic significantly affected the formation of the impurity phase defined as AlMo2O12. The Rietveld refinement of the crystalline samples showed the tendency of crystallites growing with the increase of heat-treatment temperature. Similar trends of particle growing were also observed in the images of scanning electron microscopy (SEM) for the corresponding samples heat-treated at different temperatures. Finally, the Fourier-transform infrared spectroscopy (FT-IR) revealed the effect of both the surface morphology and the crystallite size on the intensity of characteristic vibration of the corresponding chemical bonds.
采用酒石酸水溶液辅助溶胶-凝胶法制备技术,成功合成了初始组成为LiAl(MoO4)2的钼酸铝锂。根据热分析和X射线衍射测量的结果,讨论了酒石酸作为配体对均匀凝胶前体形成的影响。此外,X射线衍射还揭示了最终LiAlMo2O8陶瓷在400°C以下的结晶。发现所获得的陶瓷的初始组成显著影响定义为AlMo2O12的杂质相的形成。结晶样品的Rietveld细化表现出晶粒随着热处理温度的升高而生长的趋势。在不同温度下热处理的相应样品的扫描电子显微镜(SEM)图像中也观察到类似的颗粒生长趋势。最后,傅立叶变换红外光谱(FT-IR)揭示了表面形态和晶粒尺寸对相应化学键特征振动强度的影响。
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引用次数: 0
Solid-state synthesis and luminescence study of Bi or Eu-doped LiAlGeO4 Bi或Eu掺杂LiAlGeO4的固态合成及发光研究
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4805
Artur Harnik, M. Misevicius
In this research pristine, Bi-doped and Eu-doped LiAlGeO4 were prepared using a solid-state synthesis method. All samples were analysed by X-ray powder diffraction (XRD) and luminescence measurements. The highest Eu3+ concentration yielding monophasic samples in LiAl1-xGeO4: Eux was x = 0.08, while higher doping concentrations resulted in the formation of additional phases. The luminescence measurements revealed that the highest emission intensity was observed in the 16% Eu sample. Furthermore, the same sample demonstrated the highest quantum yield, while the longest luminescence decay was observed in the LiAlGeO4:Eu 1% sample. The temperature-dependent luminescence measurements revealed that phosphor lost half of its efficiency at 323 K.
在本研究中,采用固态合成方法制备了Bi掺杂和Eu掺杂的LiAlGeO4。通过X射线粉末衍射(XRD)和发光测量对所有样品进行分析。在LiAl1-xGeO4:Eux中产生单相样品的最高Eu3+浓度为x=0.08,而较高的掺杂浓度导致额外相的形成。发光测量显示在16%Eu样品中观察到最高的发射强度。此外,同一样品表现出最高的量子产率,而在LiAlGeO4:Eu1%样品中观察到最长的发光衰减。与温度相关的发光测量表明,磷光体在323K时失去了一半的效率。
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引用次数: 1
The effect of sowing rate on the bioaccumulation of biologically active compounds and their radical scavenging activity in Cannabis sativa L 播量对大麻生物活性物质积累及其自由基清除活性的影响
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4811
Ieva Čalkaitė, Algimanta Kundrotaitė, V. Tilvikienė, K. Barčauskaitė
Industrial hemp (Cannabis sativa L.) is a very beneficial plant because it is characterised as easy adaptable and advantageous raw material for many products which are used in daily life. Hempseeds are investigated most of all, but there is no a lot of information about other parts of this plant (stem, leaves and inflorescences). In this study, polyphenolic compounds, flavonoids and the radical scavenging activity of Cannabis sativa L. were investigated. The influence of two different sowing rates (15 and 80 plants per square meter) and two solvents on the recovery of biologically active compounds was determined. Spectrophotometric tests were used for the identification of phenolic compounds and flavonoids content and their radical scavenging activity. It was found that industrial hemp which grew in the sparse area accumulated more biologically active compounds and was a better radical scavenger than the other one, which grew under denser conditions. Moreover, it was determined that polyphenolic compounds dissolved better in methanol and thus showed better radical scavenging properties while flavonoids dissolved better in ethanol.
工业大麻(大麻sativa L.)是一种非常有益的植物,因为它的特点是适应性强,是许多日常生活中使用的产品的有利原料。对大麻种子的研究最多,但对这种植物的其他部分(茎、叶和花序)的研究却不多。研究了大麻中多酚类化合物、黄酮类化合物和自由基清除活性。测定了两种不同播量(15株/ m2和80株/ m2)和两种溶剂对生物活性化合物回收率的影响。用分光光度法测定了黄酮类化合物和酚类化合物的含量及其清除自由基的活性。研究发现,生长在稀疏地区的工业大麻比生长在密集地区的工业大麻积累了更多的生物活性物质,具有更好的自由基清除能力。此外,多酚类化合物在甲醇中溶解性较好,具有较好的自由基清除能力,而黄酮类化合物在乙醇中溶解性较好。
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引用次数: 2
Gas chromatography for β-caryophyllene determination in St. John’s wort infused oil 气相色谱法测定圣约翰草浸提油中β-石竹烯
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4810
V. Vickackaite, Sandra Petrokaitė, Vilius Poškus
Hypericum Perforatum L., commonly known as St. John’s wort, is one of the best-known medicinal herbs. St. John’s wort infused oils are mostly used externally, but can be taken orally for stomach ulcers, are used as a food supplement. Therefore, it is important to develop methods that allow a rapid and reliable determination of β-caryophyllene, which is one of the main active components of St. John’s wort. In this work, two gas chromatographic techniques, static headspace gas chromatography (SHS-GC) and solid phase microextraction, combined with gas chromatography-mass spectrometry (SPME-GC-MS), were examined for the determination of β-caryophyllene in St. John’s wort infused oils. A comparison of these two techniques revealed that SPME-GC-MS can be successfully applied for the analysis. The other method, SHS-GC, is simple and fast, but because of its high detection limit, it can only be applied to oil samples with β-caryophyllene concentration higher than 0.1 mg/g.
金丝桃,俗称圣约翰草,是最著名的草药之一。圣约翰麦汁精油主要用于外用,但也可口服治疗胃溃疡,用作食品补充剂。因此,开发能够快速可靠地测定β-石竹烯的方法是重要的,β-石竹烯是圣约翰草的主要活性成分之一。本文采用静态顶空气相色谱(SHS-GC)和气相微萃取-气相色谱-质谱联用(SPME-GC-MS)两种气相色谱技术测定了圣约翰麦汁中β-石竹烯的含量。对这两种技术的比较表明,SPME-GC-MS可以成功地应用于分析。另一种方法SHS-GC简单快速,但由于其检测限高,只能用于β-石竹烯浓度高于0.1mg/g的油样。
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引用次数: 0
Resistivity to corrosion via corrosionphilia. Professor Rimantas Ramanauskas turned 70 耐腐蚀性通过耐腐蚀性。里曼塔斯·拉马瑙斯卡斯教授70岁了
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4830
R. Pauliukaitė, J. Juodkazytė, A. Malinauskas
Lithuanian writer and poet Justinas Marcinkevičius said: ‘If there is a vocation at all, then the noblest vocation is work.’ These words well characterise Prof. Rimantas Ramanauskas, whose diligent work and dedication to science had a great impact on electrochemical research in Lithuania and the Center for Physical Sciences and Technology (FTMC).
立陶宛作家兼诗人Justinas Marcinkevičius说:“如果有一种职业,那么最崇高的职业就是工作。”这些话很好地描述了里曼塔斯·拉马瑙斯卡斯教授的特点,他勤奋的工作和对科学的奉献对立陶宛和物理科学与技术中心(FTMC)的电化学研究产生了巨大影响。
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引用次数: 1
A novel strategy to develop electrochemical atrazine sensor 一种开发电化学阿特拉津传感器的新策略
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4804
Emilija Katinaitė, Vytautas Žutautas, Aneta Bytautaitė, R. Pauliukaitė
Determination of pesticides is important for human health. Sensors are one of the best solutions because they do not require a long sample preparation and can be used not only in a laboratory. Electrochemical sensors can be easily minimised and employed for the detection of pesticides in liquid samples such as ground or wastewater. Conducting polymers have a few roles in electrochemical sensors, therefore, they can be good candidates for sensor development. Electrochemically co-polymerised folic acid and riboflavin as well as folic acid and L-lysine were employed for the detection of atrazine using square wave voltammetry. The co-polymer composition was optimised and characterised electrochemically and spectroscopically. The optimal composition of polyfolic acid and poly-L-lysine co-polymer electrosynthesised from the monomer ratio 1:10 was the best in terms of stability and sensitivity to atrazine. The best method was the square wave voltammetry showing the best sensitivity to atrazine 198 ± 1 μA/μM cm2, and the limit of detection was 14.8 nM. However, the sensitivity in tap water was significantly lower but still suitable for atrazine detection by the spike method.
农药的测定对人类健康很重要。传感器是最好的解决方案之一,因为它们不需要长时间的样品制备,而且不仅可以在实验室中使用。电化学传感器可以很容易地最小化并用于检测液体样品(如地面或废水)中的农药。导电聚合物在电化学传感器中有一些作用,因此,它们可以成为传感器开发的良好候选者。采用电化学共聚合叶酸和核黄素以及叶酸和L-赖氨酸的方波伏安法检测阿特拉津。对共聚物组合物进行了优化,并对其进行了电化学和光谱表征。从稳定性和对阿特拉津的敏感性来看,由单体比例1:10电合成的聚叶酸和聚赖氨酸共聚物的最佳组成是最好的。最佳方法是方波伏安法,其对阿特拉津的灵敏度为198±1μA/μM cm2,检测限为14.8 nM。然而,自来水中的灵敏度明显较低,但仍然适用于刺突法检测阿特拉津。
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引用次数: 0
Hydrogels – a desirable alternative to water paper restoring procedures: impacting paper properties 水凝胶——一种理想的替代水纸修复程序:影响纸张性能
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-12-09 DOI: 10.6001/chemija.v33i4.4807
Monika Baublytė, J. Kupčiūnaitė, Milda Liubinienė, A. Beganskiene
Water immersion is a common practice for treating paper media. However, this treatment could irreversibly damage paper and the information written on it – such procedures are advised if the documents do not contain water-resistant components such as inks or paints and the form is mechanically stable. Thus, polymeric materials are an attractive alternative to water immersion cleaning. Various polymers are used to produce hydrogels, but there is not much information on cleaning effects before and after aging. Due to their highly rigid properties, Kelcogel, TopVision Agarose and PhytagelTM hydrogels could be applied to clean fragile paper media instead of water immersion. The hydrogel could safely clean without any residue or change of paper properties. Selected polymers were analysed for composition, water discharge and acidity according to the corresponding requirements for restoration processes: to establish changes in chemical and physical paper properties after hydrogel cleaning, filter paper samples were analysed with SEM, TGA, FTIR and pH-meter and compared to the benchmarks of filter paper cleaned with distilled water.
浸水是处理纸介质的常见做法。然而,这种处理可能会不可逆转地损坏纸张及其上所写的信息——如果文件中不包含墨水或油漆等防水成分,并且形式机械稳定,则建议使用此类程序。因此,聚合物材料是一种有吸引力的水浸清洁替代品。各种聚合物被用于生产水凝胶,但关于老化前后的清洁效果的信息并不多。由于其高刚性特性,Kelcogel、TopVision琼脂和PhytagelTM水凝胶可以应用于清洁易碎的纸介质,而不是水浸泡。水凝胶可以安全清洁,不会有任何残留物或纸张性质的变化。根据修复过程的相应要求,对所选聚合物的成分、排水量和酸度进行了分析:为了确定水凝胶清洁后纸张化学和物理性质的变化,用SEM、TGA、FTIR和pH计对滤纸样品进行了分析,并与用蒸馏水清洁的滤纸的基准进行了比较。
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引用次数: 0
Evaluation of free amino acids in Cirsium vulgare (Bull thistle) plant materials using gas chromatography–mass spectrometry 气相色谱-质谱法评价牛蓟植物原料中游离氨基酸
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-08-07 DOI: 10.6001/chemija.v33i3.4749
U. Griškevičienė, M. Marksa, A. Ževžikovienė, A. Ževžikovas, L. Ivanauskas
Amino acids are one of the main particles in a living organism. They perform many different functions, such as structural, receptor, energetic and enzymatic functions [1]. The aim of the investigation was to identify and evaluate the qualitative composition of free amino acids in samples of Cirsium vulgare material using gas chromatography–mass spectrometry (GC-MS). Our objectives were to apply the gas chromatography– mass spectrometry (GC-MS) method for free amino acids from Cirsium vulgare raw materials grown in Lithuania and determine the qualitative composition of free amino acids from extracts of Cirsium vulgare raw materials: roots, leaves, flowers and seeds. MTBSTFA (N-methyl-N-(tertbutyldimethylsilyl) trifluoroacetamide) was selected for derivatisation in free amino acid analysis. Applying gas chromatography–mass spectrometry with compound derivatisation and based on the mass spectral database free amino acids were identified in bull thistle raw material: L-alanine, glycine, L-valine, L-leucine, L-isoleucine, L-proline, L-serine, L-threonine, L-phenylalanine, L-lysine, L-tyrosine, L-aspartic acid and L-glutamic acid. Studies have shown that the qualitative composition of free amino acids depends on the plant vegetation phase and plant parts.
氨基酸是生物体内的主要颗粒之一。它们具有许多不同的功能,如结构、受体、能量和酶功能[1]。本研究的目的是使用气相色谱-质谱联用技术(GC-MS)鉴定和评价Cirsium vulgare材料样品中游离氨基酸的定性组成。我们的目标是应用气相色谱-质谱法(GC-MS)测定立陶宛种植的小白菜原料中的游离氨基酸,并测定小白菜原料提取物(根、叶、花和种子)中游离氨基酸的定性组成。在游离氨基酸分析中选择MTBSTFA(N-甲基-N-(叔丁基二甲基甲硅烷基)三氟乙酰胺)进行衍生化。应用化合物衍生的气相色谱-质谱法,并基于质谱数据库,在牛蓟原料中鉴定出游离氨基酸:L-丙氨酸、甘氨酸、L-缬氨酸、L-亮氨酸、L-异亮氨酸、L-脯氨酸、L-丝氨酸、L-苏氨酸、L-苯丙氨酸、L-赖氨酸、L-酪氨酸、L-天冬氨酸和L-谷氨酸。研究表明,游离氨基酸的定性组成取决于植物的植被阶段和植物部位。
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引用次数: 0
Synthesis of novel 2,4-diamino-6-(arylaminomethyl)thieno[2,3-d]pyrimidines as potential antifolates 新型2,4-二氨基-6-(芳基氨基甲基)噻吩[2,3-d]嘧啶的合成
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-08-07 DOI: 10.6001/chemija.v33i3.4752
M. Dailidė, S. Tumkevičius
ynthesis of 2,4-diamino-6-(arylaminomethyl)thieno[2,3-d]pyrimidines as potential lipophilic antifolates has been developed. The synthetic strategy is based on a sequential transformation of readily available ethyl 2-amino-4-chlorothieno[2,3-d]pyrimidine-6-caboxylate to 2,4-diaminothieno[2,3-d]pyrimidine-6-carbaldehyde, which in the reaction with the corresponding anilines in titanium isopropoxide in the presence of sodium borohydride furnished the title compounds.
研究了2,4-二氨基-6-(芳基氨基甲基)噻吩[2,3-d]嘧啶作为潜在的亲脂性抗叶酸盐的合成。该合成策略是基于易得的2-氨基-4-氯噻吩[2,3-d]嘧啶-6-羧酸乙酯的顺序转化为2,4-二氨基噻吩[2,3-d]嘧啶-6-乙醛,在硼氢化钠存在的异丙醇钛中与相应的苯胺反应,形成标题化合物。
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引用次数: 1
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Chemija
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