Focused ultrasound solid-liquid extraction and selective pressurised liquid extraction to determine bisphenol A and alkylphenols in sewage sludge by gas chromatography-mass spectrometry

A new method for determining endocrine disrupter compounds (EDCs) in sewage sludge is described in this paper. EDCs studied were bisphenol A (BPA) and alkylphenols (APs). In order to obtain a fast and simple method, selective pressurised liquid extraction (SPLE) and focused ultrasound solid-liquid extraction (FUSLE) were tested. Best results for SPLE were obtained using Florisil as clean-up sorbent and dichloromethane as extraction solvent, while temperature was the only significant variable. Analyte extraction by SPLE was completed in only one extraction cycle of 1 min at 130 °C. FUSLE was carried out in one step of 20 s at 75% power (0.5 cycles) and with 8 mL of ethyl acetate. Although the optimised FUSLE process was faster, simpler and cheaper, SPLE provided higher recovery values (ranging from 81 to 105%) and therefore SPLE-based method was selected and validated. The SPLE and GC-MS method showed an LOD of 10.7 ng/g for BPA and LODs between 1.2 and 41.6 ng/g for APs. Relative standard deviation values lower than 6% were obtained for all analytes. As a result, an efficient, fast and simple method based on SPLE and GC-MS for the determination of BPA and APs in sewage sludge is proposed.     

Design of online solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) hyphenated systems for quantitative analysis of small organic compounds in biological matrices

Three online solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method examples are presented where two different types of chromatographic columns or solvent systems were coupled to meet specific analytical objectives: (i) SPE of target analytes by restricted access media from high ionic strength urine matrix was coupled with reversed phase LC-MS/MS conditions accommodating high ionization potentials of the analytes (urinary bisphenol A and other phenolic derivatives); (ii) strong cation exchange SPE of analytes of diverse polarity and pK(a) was coupled with reversed phase LC-MS/MS analysis (urinary atrazine metabolites); (iii) pre-concentration of low pg per sample analytes by weak anion exchange SPE was hyphenated with ion pair LC-MS analysis (intracellular nucleotide triphosphate analogs). With these examples we suggest a conductive generic work flow for the development of online SPE-LC-MS methods and show how advanced commercial LC devices and software allow for the design of complex yet highly versatile analytical separation systems suited to the unique physicochemical properties of the target analytes.     

Separation and characterization of gold nanoparticle mixtures by flow-field-flow fractionation

We show that using asymmetric flow-field-flow fractionation and UV-vis detector it is possible to separate, characterize, and quantify the correct number size distribution of gold nanoparticle (AuNP) mixtures of various sizes in the 5-60 nm range for which simple dynamic light scattering measurements give misleading information. The size of the collected nanoparticles fractions can be determined both in solution and in the solid state, and their surface chemistry characterized by NMR. This method will find widespread applications both in the process of "size purification" after the synthesis of AuNP and in the identification and characterization of gold-based nanomaterials in consumer products.     

Simultaneous determination of bisphenol A and alkylphenol in plant oil by gel permeation chromatography and isotopic dilution liquid chromatography-tandem mass spectrometry

A simple analytical method was developed for the simultaneous analysis of bisphenol A (BPA), nonylphenol (NP) and octylphenol (OP) in plant oil. The target compounds were extracted by cyclohexane/ethyl acetate (1:1), purified by gel permeation chromatography (GPC), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the negative ion mode. An isolator column was attached in front of the injection valve of the LC to separate background contaminants. Recovery studies were performed at three fortification levels. Mean recoveries were from 92.9% to 119.0%, with an acceptable coefficient of variation (4.4-18.5%, n=6). The limits of quantification of the method were 2, 2 and 0.5 μg/kg for BPA, NP and OP, respectively. This method can be applied for screening and confirming target compounds in plant oil.     

三维荧光结合化学多维校正快速灵敏测定环境水样中的噻菌灵和双酚A

随着经济的高速发展,环境问题正在日益引起人们的广泛关注。在实际生产中,农药和塑化剂长期存在滥用的问题,使其成为最为广泛的环境污染源并对生态环境、食品、人畜等造成严重的危害。针对环境中农药和塑化剂的残留问题,开发一种灵敏、快速的高效检测分析方法,采用三维荧光结合化学计量学方法用于环境水样中噻菌灵（TBZ）与双酚A（BPA）的快速灵敏分析。兼顾了三维荧光分析的灵敏度高、信息丰富及化学多维校正方法“数学分离”的显著优势,仅需要简单的预处理过程即可实现TBZ和BPA的痕量检测。即使分析物之间以及分析物和水样中未知背景干扰之间的光谱存在严重的重叠,基于交替三线性分解（ATLD）算法的二阶校正方法仍能借助其显著的“二阶优势”对其进行解析,并获得可靠的定性定量结果。其中,TBZ在20~200 ng·mL-1范围内线性关系良好（r=0.9999）,而BPA在40~280 ng·mL-1范围内线性关系良好（r=0.999 1）。TBZ和BPA在两种水样中的平均加标回收率分别为96.3%~99.1%和90.0%~90.8%,且标准偏差均低于7.2%。另外,计算品质因子,如灵敏度（SEN）、选择性（SEL）、检测限（LOD）和定量限（LOQ）,评估了该方法的准确性。所得结果均令人满意,表明所提出的方法能够用于环境水样中TBZ和BPA的准确、快速定量分析,为环境中农药和塑化剂的残留问题提供了一种科学有效的监测手段。     

On character groups arising from dimension groups

Character groups associated with certain dimension groups are considered. It is shown how these character groups can be used to construct an AF groupoid whose dimension group is isomorphic to the original dimension group.

     

Bisphenol A-recognition polymers prepared by covalent molecular imprinting

A specific recognition material for bisphenol A (BPA) was prepared by using a covalent imprinting technique. A chloroform solution containing bisphenol A dimethacrylate as a template, ethylene glycol dimethacrylate as a cross-linking agent and 2,2′-azobis(isobutyronitrile) as an initiator was polymerized by UV initiation. When BPA was removed from the resulting polymer by hydrolysis of the ester bonds with aqueous sodium hydroxide, carboxylic acid residues were generated in the polymer. After the polymer was packed into a stainless steel column, retention factors of BPA and related compounds were measured. The imprinted polymer adsorbed BPA and structurally related compounds such as 4,4′-dihydroxybenzophenone, bis(4-hydroxyphenyl)sulfone and 4,4′-dihydroxybiphenyl. A typical association constant (K_a) was calculated to be 1.72×10⁵ M⁻¹ by Scatchard analysis. Interestingly, 17α- and 17β-estradiol were also bound to the imprinted polymer (K_a=1.68×10⁵ M⁻¹), indicating that the polymer could be used as artificial receptors for screening the compounds having estrogenic action.     

Review of near-field optical microscopy

This review has introduced a new near-field optical microscope (NOM)—atomic force microscope combined with photon scanning tunneling microscope (AF / PSTM). During scanning, AF/PSTM could get two optical images of refractive index image and transmissivity image, and two AFM images of topography image and phase image. A reflected near-field optical microscope (AF/RSNOM) has also been developed on AF/PSTM platform. The NOM has been reviewed in this paper and the comparison between AF/PSTM & RSNOM and the commercial A-SNOM & RNOM has also been discussed. The functions of AF/PSTM & RSNOM are much better than A-SNOM & RNOM.     

二步法合成低分子量双酚A环氧

对二步法合成低分子量双酚A环氧的反应历程进行了分析,指出了降低环氧氯丙烷与双酚A克分子比的途径和方法。     

Sample preparation including sol-gel immunoaffinity chromatography for determination of bisphenol A in canned beverages, fruits and vegetables

The paper describes the development of a very simple method to prepare samples of canned food (beverages, fruits and vegetables) for the determination of bisphenol A by isocratic HPLC with fluorescence detection. The new sample preparation method makes use of the selectivity of bisphenol A antibodies immobilized in a silica matrix by an inexpensive and simple sol-gel technique. In spite of applying highly complex food matrices, immunoaffinity columns could be used for clean-up of at least 15 real samples. Limits of detection (S/N=3) ranged from 0.1 ng/ml for beverages to 4.3 ng/g for vegetables.