铟在聚乙二醇-硫酸铵双水相体系中的分配

研究了稀散元素铟在有配合剂PAR（4－（2－吡啶偶氮）－间苯二酚）存在和无PAR存在的聚乙二醇PEG－（NH4）2SO4双水相体系中的分配行为。讨论了酸度、PEG分子量、PEG浓度及温度等因素对铟分配比的影响，发现酸度对分配比的影响最大，随着PEG分子量的增加及温度的上升分配比逐渐增大；随着PEG浓度的增加分配比逐渐减小。     

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。     

RP-HPLC法测定红花中红花红色素的含量

经从红花(Carthamus tinctorius L)中分离纯化、HPLC检测、质谱鉴定得红花红色素纯品,并用其作为标准品,采用反相高效液相色谱法,测定了不同产地红花和商业红花产品中红花红色素的含量。该方法准确性高、重现性好,平均回收率为98．1％。     

丙醇-硫酸铵双水相体系萃取金(Ⅲ)-氯化物-罗丹明B

水溶性聚合物如聚乙二醇 (ＰＥＧ )、吐温(Ｔｗｅｅｎ) 80的水溶液在电解质存在下萃取分离贵金属离子已有报道[1] ;小分子的有机物如乙醇、丙醇在硫酸铵、氯化钠等电解质存在下也能分为两相形成双水相体系 ,可应用于金属离子的分离[2 ] ;该类体系也可以用于萃取分离贵金属络阴离子[3,4] 。我们发现金 (Ⅲ )与氯离子在碱性染料罗丹明Ｂ(ＲｈＢ)参与下所形成的三元缔合物 ,可被丙醇 硫酸铵双水相体系定量萃取而与大量常见贱金属分离 ,体系同时具有溶剂萃取法及溶剂浮选法的优点 :既可以分离简单贵金属络阴离子[3,4] ,又可以分离贵金属三元缔…     

乙醇-硫酸铵双水相萃取荧光法测定痕量α-萘乙酸

提出了一种基于有机溶剂-盐-水体系双水相萃取、荧光法测定痕量α-萘乙酸的新颖而简便的方法.研究了包括盐及有机溶剂的种类和用量、α-萘乙酸的荧光光谱和浓度、萃取时间、共存物和pH等的影响.在最佳萃取体系乙醇-(NH4)2SO4-H2O中,测定α-萘乙酸的线性范围2.4×10-7～5.2×10-6 mol/L,检出限7.8×10-9 mol/L.方法用于强化水样和大米样品中痕量α-萘乙酸的测定,回收率95%～103%,相对标准偏差2.2%～4.3%.     

高速逆流色谱双水相体系分离蛋白质

利用多分离柱高速逆流色谱仪,研究了聚乙二醇1000(PEG1000)-磷酸盐双水相体系的固定相保留率及该体系对蛋白质混合物和鸡蛋清样品的分离。以14.0%PEG1000-16.0%磷酸盐体系的上相为固定相,在流速0.6 mL/min和转速900 r/min的条件下,固定相的保留率达到33.3%。在pH 9.2的PEG1000-磷酸盐双水相体系中,细胞色素C、溶菌酶和血红蛋白的分配系数差异最大,采用该pH值的14.0%PEG1000-16.0%磷酸钾盐双水相体系,在流速1.0 mL/min和转速850 r/min的条件下,成功地分离了这3种蛋白质的混合物。鸡蛋清中的主要蛋白质成分卵转铁蛋白、卵白蛋白和溶菌酶在pH 9.2的15.0%PEG1000-17.0%磷酸钾盐体系中也具有最大的分配系数差异。采用该体系,在流速1.0 mL/min和转速850 r/min的条件下,成功地分离了鸡蛋清样品,得到的卵白蛋白、溶菌酶和卵转铁蛋白的电泳纯度分别为100％,100％和60％,收率均大于90％。     

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。     

丙酮双水相萃取预富集荧光法测定痕量1-萘胺

基于丙酮水溶液在适当电解质作用下能形成双水相及1-萘胺能发射荧光的特点,建立了一种丙酮-电解质-水体系双水相萃取、蠕动泵进样荧光法测定1-萘胺的新方法.研究了电解质的种类和用量、丙酮体积、1-萘胺浓度、温度、酸度和共存物等的影响.发现在最佳萃取体系丙酮-K3PO4-H2O中,1-萘胺的一次性萃取率82.7%～89.9%,测定1-萘胺的线性范围7.2×10-8～6.0×10-1 mol/L,检出限2.6×10-9 mol/L.方法用于强化水样和豆芽样品中痕量1-萘胺的测定,回收率96%～106%,相对标准偏差2.8%～5.8%.     

聚乙二醇-硫酸铵双水相萃取次甲基蓝的研究

利用分光光度法研究了次甲基蓝在聚乙二醇-硫酸铵双水相体系的萃取行为,探索了质量配比(mPEc/m(NH4)2SO4)、温度和次甲基蓝的浓度对双水相及次甲基蓝萃取率(Y)的影响.实验表明:(1)在一定的温度和浓度下,随着mPEC/m(NH4)2SO4的减小,分配系数K( cup/clow)增加,萃取率Y略有减小;(2)在一定的质量配比和浓度下,分配系数K(cup/clow)随温度的升高而增大,但萃取率Y却基本保持不变;(3)在一定的质量配比和温度下,随着次甲基蓝浓度的增加,分配系数K(cup/clow)增大;萃取率Y略有增加.在mPEG/m( NH4) 2SO4为1.50∶1,c次甲基蓝=8.915×10-5mol/L、t=30℃的实验条件下,K(cup/clow)=22.14,萃取率(y)可达95.43％.     

醇-盐双水相技术去除废水中的酚类物质

A novel method for treatment of phenolic compounds in cokery wastewater by propyl-alcohol ammonium sulfate aqueous two-phase system was investigted.The effects of the amount of ammonium sulfate used,the amount of propyl-alcohol used,pH value on extractield was studied.Extraction was optimized using a L9(34)orthogonal test.The results indicated optimum extraction conditions were the amount of ammonium sulfate used of 18.0 g,the amount of propyl-alcohol used of 16 mL,and pH value of 3.0.A extraction yield of 99.37% was achived under optimum extraction conditions and via secondary extraction.     

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].     

成相无机盐种类对PEG双水相相平衡影响

不同种类无机盐分别与PEG1000、PEG2000、PEG,4000和PEG6000构成双水相体系,在298.15K下,采用浊点滴定法研究双水相体系相平衡,通过Merchuk经验方程拟合实验点确定双水相体系的双节线,进而考察成相无机盐种类对PEG双水相相平衡的影响.结果表明:具有相同阴离子,易于形成双水相的无机盐顺序为...     

Partitioning of alkali halides in aqueous dextran-ficoll two-phase system

Partitioning of alkali halides MeX in aqueous dextran-Ficoll two-phase system of fixed polymer and ionic composition was studied. It is found that NaCl and LiX concentrate in the Ficoll-rich phase, while all KX, RbX, and CsX concentrate in the dextran-rich phase. Partitioning of KX, RbX, and CsX in the presence of a large excess of NaCl is found to depend on the type of the halide anion X^–.     

PEG/(NH4)2SO4双水相体系萃取甘草中的有效成分

甘草的主要有效成份甘草酸具有消炎解毒、抗氧自由基、调节机体免疫力等作用,目前已被广泛应用于食品、饮料、化妆品、医药、卷烟等行业。工业上广泛应用的是水提法,该法操作容易、设备简单、溶剂价廉,但提取效率不高,易造成资源浪费。双水相萃取技术(Two-aqueous phase extraction,简称．ATPS),是近年出现的新型生物化工分离技术。由于双水相萃取分离过程条件温和、可调节因素多、易于放大和操作,不存在有机溶剂残留问题,特别适用于生物物质及天然资源中有效成分的分离和提纯。     

Partition behavior and partial purification of hexokinase in aqueous two-phase polyethylene glycol/citrate systems

This study dealt with the partition behavior and partial purification of hexokinase (HK) from baker’s yeast by liquid-liquid extraction using aqueous two-phase polyethylene glycol (PEG)/citrate systems. First, we investigated the effect of agitation type (vortex and 8 rpm rotation) on the stability of the system, and then the effects of sodium citrate concentration, PEG concentration, and molar mass of PEG on the partition coefficient of this enzyme by using a 2⁵ factorial experimental design. The results of this factorial experiment showed the possibility of a partial purification of HK by using two extraction steps, since the enzyme preferentially migrated to the top phase and the total proteins (mainly contaminants) remained in the bottom phase. The purification factor (Pur _TOP) of the enzyme in the top phase was 1.87, and the partition coefficient of the total proteins (K _Prot ) was 0.47.     

阳离子表面活性剂结构对两相体系长链烯烃氢甲酰化反应的影响

合成了四种季铵盐型阳离子表面活性剂，C16H33N（N2H5）3Br(十六烷基三乙基溴化铵)，C16H33N(CH3)2C12H25Br(十六烷基十二烷基二甲基溴化铵)，C22H45N(CH3)3I(二十二烷基三甲基碘化铵)和C22H45N(CH3)2C16H33Br(二十二烷基十六烷基二甲基溴化铵)，考察其在水-有机两相体系中对Rh-TPPTS催化的长链烯烃氢甲酰化反应的促进作用。结果表明，表面活性剂中疏水长链和阳离子头的变化对催化性能有重要影响，疏水长链的增长和疏水长链数目的增加、小的阳离子头均有利于加快催化反应的速度，而疏水长链对催化活性的影响更为显著。     

Design of functional guanidinium ionic liquid aqueous two-phase systems for the efficient purification of protein

A series of novel cationic functional hexaalkylguanidinium ionic liquids and anionic functional tetraalkylguanidinium ionic liquids have been devised and synthesized based on 1,1,3,3-tetramethylguanidine. The structures of the ionic liquids (ILs) were confirmed by ¹H nuclear magnetic resonance (¹H NMR) and 13C nuclear magnetic resonance (13C NMR) and the production yields were all above 90%. Functional guanidinium ionic liquid aqueous two-phase systems (FGIL-ATPSs) have been first designed with these functional guanidinium ILs and phosphate solution for the purification of protein. After phase separation, proteins had transferred into the IL-rich phase and the concentrations of proteins were determined by measuring the absorbance at 278 nm using an ultra violet visible (UV–vis) spectrophotometer. The advantages of FGIL-ATPSs were compared with ordinary ionic liquid aqueous two-phase systems (IL-ATPSs). The proposed FGIL-ATPS has been applied to purify lysozyme, trypsin, ovalbumin and bovine serum albumin. Single factor experiments were used to research the effects of the process, such as the amount of ionic liquid (IL), the concentration of salt solution, temperature and the amount of protein. The purification efficiency reaches to 97.05%. The secondary structure of protein during the experimental process was observed upon investigation using UV–vis spectrophotometer, Fourier-transform infrared spectroscopy (FT-IR) and circular dichroism spectrum (CD spectrum). The precision, stability and repeatability of the process were investigated. The mechanisms of purification were researched by dynamic light scattering (DLS), determination of the conductivity and transmission electron microscopy (TEM). It was suggested that aggregation and embrace phenomenon play a significant role in the purification of proteins. All the results show that FGIL-ATPSs have huge potential to offer new possibility in the purification of proteins.     

离子液体双水相萃取山楂黄酮和多糖的相行为研究

用分光度法研究了[Bmim]BF4/(NH4)2SO4双水相体系萃取山楂黄酮和多糖的相行为,考察了同时提取这两种组分时[Bmim]BF4的浓度、(NH4)2SO4的浓度、山楂的用量、超声萃取时间等因素对双水相的上下相体积以及分配系数的影响。结果表明:(1)离子液体浓度的增加,双水相的上、下相体积分别明显增大和减小。但黄酮和多糖在双水相中的分配系数仅有波动,均小于5%;(2)硫酸铵浓度的增加,双水相的上下相体积分别明显减小和增大。同时黄酮和多糖的分配系数均有较明显先降低后升高的趋势;(3)山楂质量的增减,不影响双水相的形成,但存在一个实验条件下的溶出饱和值,该值为0.15g,此时黄酮和多糖的分配系数最大;(4)超声萃取时间的延长或缩短,同样不影响双水相的形成,但存在对山楂有效成分达到饱和溶出的阈值,对于黄酮为25min,多糖为20min。     

混合表面活性剂双水相性质的研究

本文利用电导法及冷冻蚀刻实验技术研究了正负离子表面活性双水相上相中的液晶结构状态及其相关性质。在双水相相体积比一组成关系曲线上及上相电导率—组成曲线上,均存在明显的转折。转折处组成是有偏光现象的双水相与无偏光现象的双水相的分水岭,立方液晶导电能力与容纳水的能力强于层状液晶或六方液晶。冷冻蚀刻实验证实了无偏光现象的立方液晶的存在。本文对一些机理进行了讨论。