Liquid–liquid microextraction and spectrophotometric determination of anionic surfactants using Astra Phloxine FF

A novel and simple procedure for determination of anionic surfactants has been developed. The method is based on the reaction of sodium dodecyl sulphate (SDS) with Astra Phloxine FF reagent at pH 3–8, followed by liquid–liquid microextraction of the formed ion associate into an organic phase containing a mixture of carbon tetrachloride and dichloroethane (4:1, v/v) and subsequent UV-Vis detection at 555 nm. The calibration plot was linear in the range 0.006–0.29 mg L^?1 of SDS. The limit of detection (LOD), calculated based on 3s, is 0.002 mg L^?1. The method was applied to the determination of anionic surfactants in real wastewater samples.     

喹啉黄中各组分的定性及定量研究

利用高效液相色谱(HPLC)对喹啉黄各组分进行分离并定量,通过液相色谱–串联质谱(LC–MS/MS)对各组分进行定性。以0.01 mol/L乙酸铵溶液和甲醇为流动相进行梯度洗脱,利用Agilent XDB–C18色谱柱对喹啉黄各组分进行分离,峰面积归一化法定量。质谱采用电喷雾负离子(ESI–)模式电离,多反应监测(MRM)模式检测,对喹啉黄各组分进行定性。结果表明,喹啉黄主要成分为喹啉黄一钠盐和喹啉黄二钠盐,分别各有两种同分异构体,各组分质量浓度在5.0~100.0μg/m L范围内与峰面积呈良好的线性关系。加标回收率为98.2%~99.1%,测定结果的相对标准偏差为0.90%~1.58%(n=6)。该方法具有良好的精密度和准确度,可用于喹啉黄中各组分的测定。     

基于色谱–光谱联用和斜投影法分析丹皮酚含量

将色谱–光谱仪联用(HPLC–UV)法与斜投影法结合,建立了丹皮酚含量快速分析方法。通过色谱–光谱联用采集丹皮酚结晶母液的紫外多波长光谱三维数据,构建不含丹皮酚的背景数据库以及丹皮酚光谱数据库,基于斜投影法步骤测定了批量样本中丹皮酚含量。结果表明:该方法计算结果和高效液相色谱分析结果接近,相对误差小于5.0%。测定结果的相对标准偏差为0.4%~1.0%(n=5),回收率为98.8%~101.3%。该方法快速、准确,操作简单,可为丹皮酚结晶产品及各种制剂质量控制提供可行方案。     

New insights into the impact toughness of ASA (acrylonitrile-styrene-acrylate) with controllable core–shell structure synthesized by three-stage seeded emulsion polymerization

Acrylonitrile-styrene-acrylate (ASA) with controllable core–shell structure was prepared through three-stage seeded emulsion polymerization. A series of characterizations had been performed to study the effect of different core–shell ratios on the properties of ASA. The most interesting was that the impact strength of ASA exhibited a “wave” variation instead of a linear variation with the increasing loading content of poly(butyl acrylate) (PBA) core. Moreover, the threshold of impact strength appeared at 49.725?wt% PBA content, nearly 33 kJ/m². To explain this unusual variation, an impact schematic was proposed.     

Study of formation of metal–polymer complexes between copper (I) and polyamic acids by HPLC

Structural, molecular, and hydrodynamic characteristics of thermostable functionalized polymers [polyamic acids (PAAs) with biquinoline chelate groups in the main chain] were studied by high-performance liquid chromatography. Size exclusion mechanism of chromatography in conditions including suppression of polyelectrolyte swelling and ion-exclusion effects was proved. The influence of molecular and structural characteristics of PAAs on their ability to form metal–polymer complexes (MPCs) with copper(I) chloride was studied. The critical polymer concentration at which binding of two PAA macromolecules with Cu⁺ ion takes place to form MPCs was estimated.     

Thermogravimetric characterization of styrene–divinylbenzene copolymers containing alpha-isopropylaminophosphonic acid groups

A commercial styrene–divinylbenzene copolymer was functionalized by multistep reactions with alpha-isopropylaminophosphonic acid groups. Three different functionalized copolymers were obtained in which the phosphonic groups are in meta (1E), para (2E), and ortho (3E) positions. The thermal behavior was studied using the TG/IR hyphenated technique and kinetic analysis of thermo-oxidation under nonisothermal conditions. The evolved gas analysis confirms the partial thermo-oxidative degradation of polymeric materials, with significant preservation of the aromatic ring. The kinetic analysis was performed by three methods: Friedman, Flynn–Wall–Ozawa, and nonparametric kinetic.     

Recent approaches for clickable poly(2-oxazoline)-based functional stimuli-responsive polymers and related applications

Abstract

Poly(2-oxazoline)s (POxs) are well-known thermo-responsive polymers that exhibit reversible hydrophilic–hydrophobic phase transitions at the lower critical solution temperature (LCST). Using living cationic ring-opening polymerisation, various functional groups can be introduced into POxs. Several clickable POxs with propargyl or azide end groups have been designed and subsequently reacted with various functional groups to prepare multifunctional POxs that respond to stimuli such as temperature, pH, chemicals and light. In this article, we briefly review recent approaches for clickable POx-based functional stimuli-responsive polymers and related applications.     

Metal ion-induced H-aggregation of a water-soluble anionic dye Congo red (CR) in Langmuir–Blodgett (LB) film

Present communication reports the preparation of Langmuir monolayer of water-soluble anionic dye Congo red (CR) by allowing it to adsorb from the aqueous subphase onto the preformed Langmuir monolayer of anionic stearic acid using divalent metal cations Mg²⁺ as mediator. Isotherm and compressibility studies of SA-Mg-CR hybrid monolayer gave valuable information about the molecular organisation in the Langmuir monolayer. Absorption spectroscopic studies revealed the formation of H-aggregates in the hybrid Langmuir–Blodgett (LB) films fabricated at lower salt concentration in the subphase. Atomic Force Microscopic image gave visual evidence of distinct nanocrystalline domains in the LB monolayer film.     

Use of biopartitioning micellar chromatography and RP-HPLC for the determination of blood–brain barrier penetration of α-adrenergic/imidazoline receptor ligands,and QSPR analysis

For this study, 31 compounds, including 16 imidazoline/α-adrenergic receptor (IRs/α-ARs) ligands and 15 central nervous system (CNS) drugs, were characterized in terms of the retention factors (k) obtained using biopartitioning micellar and classical reversed phase chromatography (log k_BMC and log k_wRP, respectively). Based on the retention factor (log k_wRP) and slope of the linear curve (S) the isocratic parameter (φ₀) was calculated. Obtained retention factors were correlated with experimental log BB values for the group of examined compounds. High correlations were obtained between logarithm of biopartitioning micellar chromatography (BMC) retention factor and effective permeability (r(log k_BMC/log BB): 0.77), while for RP-HPLC system the correlations were lower (r(log k_wRP/log BB): 0.58; r(S/log BB): –0.50; r(φ₀/P_e): 0.61). Based on the log k_BMC retention data and calculated molecular parameters of the examined compounds, quantitative structure–permeability relationship (QSPR) models were developed using partial least squares, stepwise multiple linear regression, support vector machine and artificial neural network methodologies. A high degree of structural diversity of the analysed IRs/α-ARs ligands and CNS drugs provides wide applicability domain of the QSPR models for estimation of blood–brain barrier penetration of the related compounds.