POLYMERIC SURFACTANTS BASED ON OLEIC ACID III. Copolymerization of Sodium Acrylamidostearate and Oleic Acid in a Lamellar Liquid Crystal

Copolymerization of sodium acrylamidostearate (NaAAS) and oleic acid was performed in the lamellar liquid crystal (LLC) formed by NaAAS, oleic acid and water, in the absence of N.N’-methylenebisacrylamide (MBAA) and in the presence of MBAA, respectively. In the absence of MBAA, after the polymerization the lamellar structure remained, and the disorder of the lamellar liquid crystal was, to some extent, enhanced. Surface tension, small-angle X-ray diffraction, viscosity, and fluorescence methods were used to study the properties of the linear copolymer. The linear polymeric surfactant behaves like     

Mechanism of Electrical Percolation of w/o Microemulsions Formed by Nonionic Surfactants

A study was carried out on the mechanism of electrical conductivity percolation of H₂O/C₁₆EO₂₀/n-butanol/heptane microemulsions. Electrical conductivity, UV-vis spectroscopy and FTIR spectra were used to study the diluted “dry” microemulsions with the mass ratio of C₁₆EO₂₀/n-butanol/heptane = 3:3:4. The results of electrical conductivity showed that the percolation occurred around φ_w = 20 wt% and the transition of w/o microemulsions to bicontinueous microemulsions happened when φ_w = 45 wt%. From the UV-vis absorption spectra, it was found that the absorption of methyl orange (MO) in microemulsions shifted red than that of in oil phase, but the maximal absorption peak (λ_max) remained unchanged when φ_w > 20 wt%. It implied that the position of MO solubilized in microemulsions was unvaried after free water appeared in the core. FTIR spectra revealed that the OH band of water in microemulsions moved to high frequency at low φ_w (< 20 wt%) and became broader at high φ_w. It indicated that the added water only caused the hydration of EO at low φ_w, the hydration completed when φ_w > 20 wt% and then the residual water entered into the core with properties similar to bulk water. The presence of free water as ions exchange medium will cause the electrical conductance increased. The percolation appeared after the hydration of EO completed.     

Development of Phosphatidylethanolamine Liposomes That Efficiently Retain Encapsulated Vinorelbine Bitartrate

A hydrophilic and temperature-induced degradation drug, vinorelbine bitartrate (VB)-loaded phosphatidylethanolamin sterically stabilized liposomes (PSLs) were prepared by the thin film hydration method. Liposomes were made of phosphatidylethanolamine: cholesteryl: oleic acid (PE: CHOL: OA, 6:4:3 mass/mass). The mean particle size of the PSLs ranged from 600 to 650 nm. The transmission electron microscope (TEM) images displayed that the shape of the PSLs was multilamellar vesicles with smooth surface. The highest entrapment efficiency (EE) and drug loading capacity (DL) could reach up to 81.2 and 16.6%, respectively. The studies of drug release showed that the drug release could last for much more than 48 hours. The PSLs was evaluated by comparing the rate of release of encapsulated VB in different phosphate buffer solution (PBS).     

免疫亲和柱净化-液相色谱-串联质谱法同时测定猪肉中6种玉米赤霉醇类化合物残留量

建立了猪肉中6种玉米赤霉醇类化合物残留量的免疫亲和柱净化-液相色谱-串联质谱(IAC-LC-MS/MS)分析方法。酶解后的样品用乙醚提取,提取液浓缩后用三氯甲烷溶解,NaOH溶液反萃取,经免疫亲和柱富集和净化后,采用LC-MS/MS进行测定,外标法定量。在Shimadzu Shim-pack VP-ODS C18反相柱上分离,梯度洗脱,流动相为乙腈和2 mmol/L乙酸铵溶液;质谱采集为电喷雾负离子多反应监测模式。6种目标物的线性范围为0.5～200μg/L,相关系数(R)大于0.999,定量限(LOQ)在0.05～0.63μg/kg之间;添加浓度在1.0～5.0μg/kg范围内,方法回收率为71.3%～93.7%,相对标准偏差在3.7%～9.7%之间。该方法灵敏度高、重现性好,适用于猪肉样品中痕量玉米赤霉醇类药物残留的测定。     

Synthesis of aromatic diamine-based benzoxazines and effect of their backbone structure on thermal and flammability properties of polymers

Three kinds of novel aromatic diamine-based benzoxazines containing naphthalene, propane-2,2-diyldibenzene and neopentyl groups in the backbone, respectively (designated as BAPNCP, BAPBACP and BAPNPGCP, respectively), were synthesized and characterized. In addition, the effects of backbone structures on curing behaviors of the monomers and thermal and flammability properties of the resulting polymers were systematically studied. The results indicated that BAPNPGCP displayed the highest enthalpy of the curing reaction associated with the ring-opening of benzoxazine, which was due to the effect of benzoxazine ring content per unit mass. Interestingly, the 5 wt% weight loss temperature and char residue after thermogravimetric test for poly(BAPNPGCP) were 8 °C and 7% higher than those of poly(BAPBACP). Meanwhile, the total heat release of poly(BAPNPGCP) was less than half of that for poly(BAPBACP), indicating the substantial effect of benzoxazine ring content on flammability and char formation. Furthermore, it was found that poly(BAPNCP) gave the best thermal stability and flame retardancy, which was due to the synergistic effect between naphthalene group and benzoxazine ring content. This study provides new insight into the curing behavior of benzoxazine and further understanding on the high performance of polybenzoxazine.     

Improving the properties of HDPE based separators for lithium ion batteries by blending block with copolymer PE-b-PEG

To improve the performances of HDPE-based separators, polyether chains were incorporated into HDPE membranes by blending with poly(ethylene-block-ethylene glycol) (PE-b-PEG) via thermally induced phase separation (TIPS) process. By measuring the composition, morphology, crystallinity, ion conductivity, etc, the influence of PE-b-PEG on structures and properties of the blend separator were investigated. It was found that the incorporated PEG chains yielded higher surface energy for HDPE separator and improved affinity to liquid electrolyte. Thus, the stability of liquid electrolyte trapped in separator was increased while the interfacial resistance between separator and electrode was reduced effectively. The ionic conductivity of liquid electrolyte soaked separator could reach 1.28 × 10-3 S.cm-1 at 25℃, and the electrochemical stability window was up to 4.5 V (versus Li + /Li). These results revealed that blending PE-b-PEG into porous HDPE membranes could efficiently improve the performances of PE separators for lithium batteries.     

A study of the transition of liquid-crystal alignment from homeotropic to planar on a polyimide layer

The alignment of nematic liquid crystals by rubbed polyimide surfaces has been well-studied and developed. A novel polyimide film which induced a homeotropic alignment of the nematic liquid crystal without rubbing or with weak rubbing strength was presented. However, there was a transition from homeotropic to planar alignment of the nematic liquid crystal after strong rubbing. In order to study the transition, the polyimide surface was investigated by atomic force microscopy, surface free energy measurement and angle-resolved analysis X-ray photo-electron spectroscopy before and after rubbing with a velvet fabric. It was found that both the change of surface polarity and surface morphology were not the reasons for the transition. The droop of the side chain on the polyimide surface after the rubbing treatment was detected by angle-resolved analysis X-ray photo-electron spectroscopy. Owing to the special structure of the novel polyimide, the X-ray photo-electron spectroscopy was successfully used for the first time to analyse the conformational change of the side chain of a polymer. In conclusion, the transition of nematic liquid crystal alignment from homeotropic to planar after rubbing was influenced by the side chain conformation of the polyimide.     

Recombinant Expression and Characterization of an Organic-Solvent-Tolerant α-Amylase from Exiguobacterium sp. DAU5

The enzyme from halophilic microorganisms often has unique properties such as organic-solvent-tolerance. In this study, a novel organic-solvent-tolerant α-amylase gene was cloned from the mild halophile Exiguobacterium sp. DAU5. The open reading frame (ORF) of the enzyme consisted of 1,545 bp and encoded 514 amino acids, the primary sequence revealed that it belongs to the glycoside hydrolase (GH) family 13. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) showed an AmyH monomer of 57 kDa. The enzyme exhibited maximal activity at 40 °C in pH?8.5 glycine–NaOH buffer, and the activity was strongly inhibited by Zn²⁺, Cu²⁺, and Fe²⁺. The α-amylase AmyH exhibited high hydrolysis activity toward soluble starch, and the major hydrolysis products were maltose, maltotriose, and maltopentaose; the AmyH could not efficiently hydrolyze oligosaccharides smaller than maltoheptaose, nor could it act on the β-1,4 or α-1,6 glucosidic bonds in xylan or pullulan, respectively. In addition, the α-amylase exhibited better tolerance to organic solvents, as it was stable in the presence of dimethylsulfoxide (DMSO), methanol, ethanol, and acetone. Base on all of these results, the enzyme could be useful for practical application in the bakery industry and in biotechnological processes that occur in the presence of organic solvents.     

Development of dispersive liquid-phase microextraction based on new ionic liquid 1,3-diisooctylimidazolium hexafluorophosphate as solvent for the extraction and determination of dicofol and its degradation products in water samples

In the current paper we describe a novel sample preparation technique termed dispersive liquid-phase microextraction for the preconcentration and determination of 2,2,2-trichloro-1,1-bis(4-chlorophenyl)ethanol (dicofol) and its degradation products in water samples that includes 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1-dichloroethene(2,4′-DDE), 1,1-dichloro-2,2-bis(4-chlorophenyl)ethane(4,4′-DDE) and 1,1,1-trichloro-2-(2-chlorophenyl)-2-(4-chlorophenyl)ethane (2,4′-DDT) coupled with gas chromatography mass spectrometry (GC-MS), in which a new ionic liquid 1,3-diisooctylimidazolium hexafluorophosphate abbreviated as [D(i-C₈)IM][PF₆] was used as extraction solvent. For each one extraction, 1.00 mL of the methanol solution containing 40 µL of the ionic liquid was sprayed into 25.00 mL of water sample. In the meantime the ionic liquid was finely dispersed into the aqueous phase and analytes were rapidly migrated into the ionic liquid. After the solution was centrifuged for 2 min at 5000 rpm, the droplets of the ionic liquid are subsided in the bottom of the conical test tube (30.0 ± 0.2 µL). Moreover, the factors relevant to extraction efficiencies were investigated and optimised including the volume of the ionic liquid, disperser solvent, extraction time, sample pH and ionic strength. Under optimal conditions, the enrichment factors of the extraction were between 550 and 725 with an extraction efficiency ranging from 66% to 87% for each different analyte. Finally, 1.0 µL of the ionic liquid collected from above extraction was injected into the injector block of GC-MS instrument for analysis. The detection limit (S/N = 3), the relative standard deviations for 2.0 µg L^?1 of the standard analyte (n = 5) and linearity in a calibration range were found to be 3–8 ng L^?1, 1.0–2.7% and 10–3000 ng L^?1, respectively. Good spiked recoveries over the range of 92.0–13.5% were obtained. The proposed method offers the advantages of simplicity of operation, rapidity, good extraction efficiency and enrichment factor; it has been successfully applied to determination of dicofol and its degradation products in environmental water samples.