聚乙二醇双水相萃取光度法测定铼

研究了聚乙二醇双水相体系中,金属离子络合物及萃取剂的光谱行为,研究了酸度、缓冲溶液用量、盐用量、萃取剂用量及表面活性剂对萃取铼的影响,并通过控制一定条件,可实现了混合离子的分离。     

聚乙二醇双水相萃取光度法测定锌

A novel method of extraction spectrophotometric determination of Zn~(2+) in aqueous two-phase system formed by polyethylene glycol-2000,sodium sulfate and zincon has been established.Amounts of PEG solution,zincon solution,sodium sulfate added and the acidity of the system were optimized.The interference effects of various coexistent ions and the method to remove the interference were investigated.The Zn-zincon complex that had been formed in the presence of H_2BO_3-Na_2B_4O_7 buffer solution at pH 7.4 was extracted into the upper PEG-rich phase,and the absorbance of the extracted complex in the upper PEG-rich phase was measured at 630 nm.The apparent molar absorptivity was 7.3 × 10~4 L / (mol·cm).Beer's law was obeyed over the range of 0～2.0 μg / mL Zn~(2+).The analytical results obtained for Zn~(2+) in water samples were in good agreement with values measured by atomic absorption spectrometry.     

十四烷基三甲基氯化铵/十二烷基苯磺酸钠混合表面活性剂双水相体系的萃取性能

研究了十四烷基三甲基氯化铵(TTAC)与十二烷基苯磺酸钠(SDBS)混合表面活性剂水溶液双水相体系的分相情况、萃取性能及两相的微观结构.结果表明,TTAC/SDBS混合表面活性剂水溶液在30℃下能够形成稳定的双水相体系;该双水相体系对亚甲基蓝、靛红都具有一定的萃取分离作用.其上、下两相的微观结构明显不同,这是其能够形成稳定双水相体系且具有萃取作用的重要原因.     

新型的萃取技术——双水相萃取

本文介绍了双水相萃取技术的原理与特点及近年来该技术在生命科学,复杂中药体系的分离以及抗生素药物提取等方面的研究进展。并探讨了其今后的发展趋势。     

正负离子表面活性剂/离子液体双水相性质研究

本文把短链离子液体(IL)四氟硼酸1-乙基-3-甲基咪唑鎓[C2mim]BF4引入正负离子表面活性剂十二烷基硫酸钠(SDS)和十二烷基三甲基溴化铵(DTAB)双水相体系(SDS/DTAB/H2O)中,研究了IL对双水相相图及相分离体系性质的影响。结果表明,[C2mim]BF4的阳离子性质是影响阴离子表面活性剂过量区域性质的主要因素,IL通过静电作用、氢键作用等改变体系中聚集体的形貌,最终导致阴离子双水相(ATPSa)的消失。IL的阴离子对阳离子双水相(ATPSc)区域性质起着决定作用;IL的盐效应引起的对表面活性剂混合胶束扩散双电层的压缩作用,不但促进胶团的形成,缩短了形成稳定胶团所需要的时间,加快了双水相的相分离速度,而且也造成了形成ATPSc所需DTAB含量的提高。IL的引入改变了ATPSc上、下相表面活性剂的组成及含量,使富含表面活性剂的上相中阳离子表面活性剂含量更高,进而提高了双水相的萃取性能,其上相对甲基橙的萃取效率可高达96.67%。     

离子液体双水相体系萃取分离牛血清白蛋白

建立了由亲水性离子液体四氟硼酸1-甲基-3-丁基咪唑([Bmim]BF4)和KH2PO4形成的双水相体系萃取分离牛血清白蛋白(BSA)的新方法。研究了不同盐及盐的浓度、离子液体浓度以及蛋白质用量、溶液酸度、其它共存物质对双水相成相及BSA萃取率的影响,结果表明,磷酸二氢钾盐浓度为80g/L,离子液体浓度在160~240mL/L,BSA的浓度为30~50mg/L,溶液酸度在pH4~8范围,离子液体双水相体系对BSA有较高的萃取率。用加入不同类型表面活性剂探讨了离子液体与蛋白质之间的作用。     

离子液体双水相萃取荧光法测定维生素B6

基于离子液体在盐的作用下能够形成双水相,用于目标物质的萃取,提出了离子液体-硫酸铵双水相萃取、荧光法测定痕量维生素B6的新方法.实验探讨了影响维生素B6萃取率的主要因素,如酸度、萃取剂的用量、时间等.在最适条件下,即λex/λem=342/418 nm,pH=8.69,离子液体和硫酸铵的用量分别为1.3mL、2.8g,...     

不同离子液体双水相萃取钯

为实现贵金属钯的绿色、高效萃取,本文使用有“绿色溶剂”之称的离子液体与磷酸钾形成的双水相体系,不加入其它萃取剂对钯(Ⅱ)进行萃取,并采用浊点法对所研究的6种咪唑类离子液体的双结线和系线进行测定。 结果表明,基于氯离子和溴离子的离子液体成相能力和萃取率无显著差异。 阳离子上支链的疏水性是影响咪唑类离子液体成相能力的关键因素之一。 与不含官能团的离子液体相比,支链上嵌入氨基和腈基的离子液体,成相能力较低,但萃取率分别提高了11.57%和34.26%。 当含腈基的离子液体浓度和磷酸钾浓度分别为5.00%和39.55%时,离子液体双水相体系对钯(Ⅱ)的萃取率可达到100%。 本文的研究成果为设计/选择可利用其双水相体系高效萃取钯(Ⅱ)的离子液体提供了理论基础和数据支持。     

PEG 800-Tween 80-(NH4)2 SO4-H2O双水相萃取紫外分光光度法测定银杏叶中的芦丁

采用聚乙二醇(PEG800)与吐温80(Tween80)组合表面活性剂、(NH4)2SO4、H2O形成双水相体系,研究芦丁在该双水相体系中的分配行为。用紫外分光光度法测定银杏叶中芦丁的含量。该体系对芦丁的平均萃取率为95．0％,测定芦丁浓度的线性范围为0～50ug／mL,相关系数r=0．9995。用该法对银杏叶中的芦丁进行测定,测定结果的相对标准偏差为3．1％,回收率为96．5％～105．2％。     

乙醇/硫酸铵双水相体系萃取螺旋藻多糖的研究

考察了低分子有机溶剂与无机盐-乙醇/硫酸铵双水相体系萃取螺旋藻多糖的可行性及影响因素。研究结果表明:为除去并有效回收螺旋藻细胞中的蛋白质成分,在藻细胞破碎后进行盐析沉淀蛋白质,再采用传统的热水浸提法,可得到螺旋藻多糖的溶出率为38.44±1.12mg/g干燥粉;通过乙醇/硫酸铵双水相体系的萃取分配,在w(乙醇)=19%,w(硫酸铵)=27.5%(即双水相体系系线长度TLL=42.9),体系相比VR=1.05,pH=7.0时,螺旋藻多糖的收率可达84.5±1.45%,富集因子可达6.2。该研究结果表明廉价的乙醇/硫酸铵双水相萃取螺旋藻多糖将有望开发成为一条简洁、高效、低成本的螺旋藻多糖分离提取工艺。     

Aqueous two-phase system of an anionic gemini surfactant and a cationic conventional surfactant mixture

The aqueous two-phase system formed by the mixture of dodecyltrimethylammonium bromide (DTAB) with a gemini surfactant O,O′-bis(sodium 2-lauricate)-p-benzenediol (C₁₁pPHCNa) has been studied. Two two-phase regions were observed, one was a wide region in the cationic surfactant-rich side and the other in the vicinity of R = 1:1, where R is the mixing mole ratio of DTAB to C₁₁pPHCNa in global solution. Multi-lamellar vesicles are formed in the concentrated upper phase of cationic surfactant-rich systems and spherical aggregates in the concentrated bottom phase at R = 1:1. The microstructure of the solution and the phase behavior of the aqueous two-phase system strongly depended on the total concentration and the composition of the system.     

Extraction and determination of papaverin in pericarpium papaveris using aqueous two-phase system of poly(ethylene glycol)-(NH4)2SO4 coupled with high-performance liquid chromatography

Based on aqueous two-phase system (ATPS) of poly(ethylene glycol) (PEG)–(NH₄)₂SO₄, a simple pretreatment approach was developed for the extraction and determination of papaverin in pericarpium papaveris. The influence factors on phase behavior of the ATPS and partition behavior of papaverin was investigated, and partition mechanism based on the hydrophobic interaction between PEG and analyte molecules was proposed. Under the optimal conditions, the extraction efficiencies for papaverin were 93–96%, and the recoveries of the added standard were 97–106% with relative standard deviations of 1.8–2.5%. Combined with a high-performance liquid chromatography (HPLC) method, this extraction technique has been successfully applied to the determination of papaverin in pericarpium papaveris with the detection limit of 2 ng mL⁻¹ and the linear range of 0.10–10 μg mL⁻¹. Compared with the conventional liquid–liquid extraction or solid-phase extraction, this method was more environmentally benign, more cost effective and much simpler due to the direct injection of the upper phase into HPLC system.     

Interfacial tension of the aqueous two-phase systems of cationic-anionic surfactant mixtures

Interfacial tensions of the aqueous two-phase systems formed by cationic-anionic surfactant mixtures were measured using spinning drop method. The effects of surfactant structure, molar ratio of cationic to anionic surfactants, surfactant concentration, salt, and temperature on the interfacial tensions were investigated. It was shown that the values of the interfacial tensions of the aqueous two-phase were in the scale of ultra-low interfacial tensions at certain molar ratios of cationic to anionic surfactants. Three types of interfacial tension curves were observed. The first curve comprised two curves that were located on either side of 1:1 molar ratio, and the interfacial tension decreased with the increase of excessive surfactant components. The second one was a saddle-shaped curve that strode over the 1:1 molar ratio. The third type was a saddle-shaped curve that was located beside the 1:1 molar ratio. The types of interfacial tensions depended on the molecular structure of the surfactants such as the hydrophilic groups and the lengths and symmetry of hydrophobic chains.     

乙醇-硫酸铵双水相萃取镉-碘化钾-罗丹明B离子缔合物

研究了在(NH4)2SO4存在下,碘化钾-罗丹明B-乙醇体系萃取Cd(Ⅱ)的行为及最佳分相条件。实验表明,在pH 1～3时,乙醇-(NH4)2SO4双水相体系对[CdI4]2-络阴离子的萃取率只有35.5%;加入罗丹明B后,该体系能完全萃取镉-碘化钾-罗丹明B形成的离子缔合物,而干扰离子Zn2+、Fe3+、Co2+、Cu2+、Ni2+不被萃取,实现Cd2+与上述离子的分离。     

离子液体双水相萃取分离苋菜红的研究

建立了由亲水性离子液体四氟硼酸1-丁基-3-甲基咪唑([Bmim]BF4)和NaH2PO4形成的双水相体系萃取分离苋菜红的新方法.研究了盐的浓度、离子液体浓度、溶液酸度、其它共存物质对苋菜红萃取率的影响.结果表明,NaH2PO4加入量在2～2.5 g,离子液量在1.0～2.0 mL,苋菜红溶液量在1.5 mL,溶液酸度在pH 4～6范围,离子液体双水相体系对苋菜红有较高的萃取率(E%＞90).用加入无机离子、不同类型表面活性剂和吸收光谱探讨了离子液体与苋菜红之间的作用.     

Droplet-based microextraction in the aqueous two-phase system

This report is about microfluidic extraction systems based on droplets of aqueous two-phase system. Mass transfer between continuous phase and dispersed droplet is demonstrated by microextraction of ruthenium red in a microfluidic device. Droplets are generated with electrohydrodynamic method in the same device. By comparing brightness in the digital image of a solution with known concentrations of ruthenium red and those of a droplet in the microextraction, ruthenium red concentration was measured along the microextraction channel, resulting in good agreement with a simple diffusion model. The maximum partition coefficient was 9.58 in the experiment with the 70-mm-long-channel microextractor. The method is usable for terminating microextraction by electrohydrodynamic manipulation of droplet movement direction. Droplets of different ruthenium red concentration, 0.12 and 0.24% (w/w) in this experiment, can be moved to desired place of microfluidic system for further reaction through respectively branched outlets. In this study droplet-based microextraction is demonstrated and the mass transport is numerically analyzed by solving the diffusion–dissolution model.     

Drop formation in aqueous two-phase systems

Extraction using aqueous two-phase systems (ATPSs) is a versatile technique for the downstream processing of various proteins/enzymes. The study of drop formation deals with the fundamental understanding of the behavior of liquid drops under the influence of various external body as well as surface forces. These studies provide a basis for designing of the extractions in column contactors in which liquid drops play a major role. Most of the drop formation studies reported so far is restricted to aqueous-organic systems. ATPSs, differ from aqueous-organic systems in their physical properties. In view of this, an attempt was made to develop a model for drop formation in ATPSs adopting the information available on aqueous-organic systems. In order to validate the model, experiments were performed by using polyethylene glycol (PEG)/salt systems of different phase compositions at various flow rates. At low flow rates the single stage model and at high flow rates the two stage model are able to predict the drop volume during its formation from tip of capillary. The experimental results were found to agree reasonably well with those predicted by the model.     

Extraction and determination of morphine in compound liquorice using an aqueous two-phase system of poly(ethylene glycol)/K2HPO4 coupled with HPLC

An aqueous two-phase system (ATPS) of poly(ethylene glycol) (PEG)/K₂HPO₄ coupled with high performance liquid chromatography (HPLC) method was developed for the separation and determination of morphine in compound liquorice. Morphine and its analogs were used as model compounds to investigate influence of various factors on extraction behaviors of ATPS, such as the types and concentrations of salts, PEG molecular mass, temperature and pH. It was observed that the types of salt had much influence on extraction efficiencies of morphine and its analogs. The results indicated that hydrophobic force cooperating with hydrogen bond interaction between analytes and phases played important role in extraction process. In the optimal system of containing 0.5 g PEG2000 and 1.5 g K₂HPO₄, the recoveries of the spiked standards for the analytes were all 91.7-100.3% with relative standard deviation of 1.0-3.0%. Morphine in compound liquorice was determined by the proposed method and the results were consistent with those of LC-MS method. Compared with conventional liquid-liquid extraction or solid-phase extraction, this extraction method can be completed in one operation and is low-cost. Since the entire extraction process is organic solvent-free, this new technique is environmental friendly.     

Extraction of testosterone and epitestosterone in human urine using aqueous two-phase systems of ionic liquid and salt

Based on aqueous two-phase systems (ATPS) consisting of 1-butyl-3-methylimidazolium chloride, a hydrophilic ionic liquid (IL), and K2HPO4, a new and simple extraction technique, coupled with a reversed-phase high performance liquid chromatography (RP-HPLC), was developed for the simultaneous concentration and analysis of testosterone (T) and epitestosterone (ET) in human urine. Under the optimal conditions, the extraction efficiencies for both analytes were 80-90% in a one-step extraction. The method required only 3.0 mL of urine and a single hydrolysis/deproteinization/extraction step followed by direct injection of the IL-rich upper phase into HPLC system for analysis. The method has been satisfactorily applied to the analysis of T and ET in human urine with detection limits of 1 ng/mL and linear ranges of 10-500 ng/mL for both compounds. Compared with conventional liquid-liquid extraction or solid phase extraction, this new method is much "greener" due to no use of volatile organic solvent and low consumption of IL. The proposed extraction technique opens up new possibilities in the separation of other drugs.     

聚乙二醇双水相萃取光度法测定镍

用水溶性高聚物、表面活性剂及有机物与无机盐形成的双水相体系萃取分离色素、蛋白质及测定金属离子已有报道[1-5].