Green synthesis of MIL53(Al)-modified paper-based analytical device for efficient extraction of neonicotinoid insecticides from environmental water samples.

Background: There is a need to develop low-cost, reliable and portable devices to enhance the efficiency of microextraction techniques in complex samples. Metal-organic frameworks (MOFs) have proven to be promising sorbents due to their well-documented properties. However, their green preparation and combination with paper-based substrates have not been satisfactorily explored to fabricate sustainable sorptive phases.

Aptamer-functionalized stir bar sorptive extraction for selective isolation, identification, and determination of concanavalin A in food by MALDI-TOF-MS.

An aptamer-functionalized stir bar sorptive extraction (SBSE) coating is described for the first time devoted to selective isolation and preconcentration of an allergenic food protein, concavanalin A (Con A), followed by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF-MS) determination. For this purpose, the polytetrafluoroethylene surface of commercial magnetic stir bars was properly modified and vinylized to immobilize a thiol-modified aptamer against Con A via straightforward "thiol-ene" click chemistry. The aptamer-functionalized stir bar was employed as SBSE sorbent to isolate Con A, and several parameters that can affect the extraction efficiency were investigated.

Development of hybrid monoliths incorporating metal-organic frameworks for stir bar sorptive extraction coupled with liquid chromatography for determination of estrogen endocrine disruptors in water and human urine samples.

A novel coating based on hybrid monolith with metal-organic framework (MOF) onto conventional Teflon-coated magnetic stir bars was developed. For this purpose, the external surface of the Teflon stir bar was firstly vinylized in order to immobilize a glycidyl methacrylate (GMA)-based polymer onto the magnet. Then, an amino-modified MOF of type MIL-101 (NH-MIL-101(Al)) was covalently attached to the GMA-based monolith.

Weak anion-exchange mixed-mode materials to selectively extract acidic compounds by stir bar sorptive extraction from environmental waters.

In this study, the first example of a polytetrafluoroethylene (PTFE)-based magnet coated with weak anion exchange (WAX) monolith as novel support for stir bar sorptive extraction (SBSE) is presented. Firstly, the PTFE magnets were properly modified and vinylized in order to immobilize polymer monoliths onto its surface. Then, a glycidyl methacrylate monolith was prepared and modified with ethylenediamine (EDA) to create weak anion exchanger via ring opening reaction of epoxy groups.

Preparation of monolithic polymer-magnetite nanoparticle composites into poly(ethylene-co-tetrafluoroethylene) tubes for uses in micro-bore HPLC separation and extraction of phosphorylated compounds.

This paper describes the fabrication of a novel microbore monolithic column modified with magnetite nanoparticles (MNPs) prepared in a poly(ethylene-co-tetrafluoroethylene) (EFTE) tubing, and its application as stationary phase for the chromatographic separation of phosphorylated compounds. In order to obtain the composite column, a two-step procedure was performed. The formation of a glycidyl methacrylate-based monolith inside the activated ETFE tube was firstly carried out.

Determination of benzomercaptans in environmental complex samples by combining zeolitic imidazolate framework-8-based solid-phase extraction and high-performance liquid chromatography with UV detection.

In this work, the synthesis of zeolitic imidazolate framework-8 (ZIF-8) crystals and their subsequent application as effective sorbents for extraction and preconcentration of several benzomercaptans from environmental complex samples is described. These materials were prepared by solvothermal approach varying the concentration of n-butylamine modulator to modify the surface of the metal-organic framework. The resulting materials were characterized by scanning and transmission electron microscopy, powder X-ray diffraction and Fourier transform infrared spectroscopy.

Influence of photo-initiators in the preparation of methacrylate monoliths into poly(ethylene-co-tetrafluoroethylene) tubing for microbore HPLC.

In this study, poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) polymeric monoliths were in situ developed within 0.75 mm i.d.

Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases.

In this study, porous polymer monoliths were in situ synthesized in fluoropolymers tubing to prepare microbore HPLC columns. To ensure the formation of robust homogeneous polymer monoliths in these housing supports, the inner surface of fluoropolymer tubing was modified in a two-step photografting process. Raman spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the inner poly(ethylene-co-tetrafluoroethylene) (ETFE) wall and the subsequent attachment of a monolith onto the wall.

Extraction and preconcentration of organophosphorus pesticides in water by using a polymethacrylate-based sorbent modified with magnetic nanoparticles.

A polymethacrylate-based sorbent modified with magnetic nanoparticles (MNPs) has been synthesized and used as sorbent for solid-phase extraction (SPE) and magnetic solid-phase extraction (MSPE) of three organophosphorus pesticides (phosmet, pirimiphos-methyl, and chlorpyrifos) in water samples followed by high-performance liquid chromatography-diode array detection. The sorbent was prepared from a glycidyl methacrylate-based polymer, modified with a silanizing agent, followed by immobilization of MNPs on the surface of the material. The sorbent was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy.

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography.

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch), or mixtures of HO and HSO, were tried and compared.

Determination of azoxystrobin and chlorothalonil using a methacrylate-based polymer modified with gold nanoparticles as solid-phase extraction sorbent.

This paper describes a novel and sensitive method for extraction, preconcentration, and determination of two important widely used fungicides, azoxystrobin, and chlorothalonil. The developed methodology is based on solid-phase extraction (SPE) using a polymeric material functionalized with gold nanoparticles (AuNPs) as sorbent followed by high-performance liquid chromatography (HPLC) with diode array detector (DAD). Several experimental variables that affect the extraction efficiency such as the eluent volume, sample flow rate, and salt addition were optimized.

Photoinduced chemiluminescence determination of carbamate pesticides.

A liquid chromatography method with post-column photoinduced chemiluminescence (PICL) detection is proposed for the simultaneous determination of eight carbamate pesticides, namely aldicarb, butocarboxim, ethiofencarb, methomyl, methiocarb, thiodicarb, thiofanox and thiophanate-methyl. After chromatographic separation, quinine (sensitizer) was incorporated and the flow passed through an UV lamp (67 s of irradiation time) to obtain the photoproducts, which reacted with acidic Ce(iv) and provided a CL emission. The PICL method showed great selectivity for carbamate pesticides containing sulphur in their chemical structure.

Selective and Sensitive Chemiluminescence Determination of MCPB: Flow Injection and Liquid Chromatography.

Two new chemiluminescence (CL) methods are described for the determination of the herbicide 4-(4-chloro-o-tolyloxy) butyric acid (MCPB). First, a flow injection chemiluminescence (FI-CL) method is proposed. In this method, MCPB is photodegraded with an ultraviolet (UV) lamp and the photoproducts formed provide a great CL signal when they react with ferricyanide in basic medium.

Development of a Photoinduced Chemiluminescent Method for the Determination of the Herbicide Quinmerac in Water.

A new, simple, and sensitive method, based on photoinduced chemiluminescence, was developed for the determination of quinmerac. The photoproduct, obtained after ultraviolet irradiation in basic medium, was mixed with sodium sulfite (sensitizer), and Ce(IV) (oxidant) in acid medium. A wide linear dynamic range (2-600 ng mL(-1)) and a limit of detection of 0.

Fast determination of thiacloprid by photoinduced chemiluminescence.

A new and sensitive application of chemiluminescence detection has been developed for the determination of the pesticide thiacloprid in water. It was based on the on-line photoreaction of thiacloprid in a basic medium, with quinine acting as the sensitizer of the chemiluminescent response; cerium (IV) in sulfuric acid medium was used as the oxidant. High degrees of automation and reproducibility were achieved using a flow-injection analysis (FIA) manifold.

Determination of organothiophosphorus pesticides in water by liquid chromatography and post-column chemiluminescence with cerium(IV).

A new, fast, selective and sensitive method has been developed for the simultaneous determination of nine organothiophosphorus (OTP) pesticides, namely omethoate, dimethoate, disulfoton-sulfoxide, methidathion, phosmet, malathion, diazinon, pirimiphos-methyl and chlorpyrifos. The pesticides were separated on a Kinetex C18 column by gradient elution with acetonitrile:water. A post-column basic hydrolysis of the pesticides and later a chemiluminescence (CL) reaction with cerium (IV) in acid medium was carried out.

Native vs photoinduced chemiluminescence in dimethoate determination.

The determination of dimethoate using either its native chemiluminescent (CL) properties or its photoinduced chemiluminescence obtained by irradiation with a 15 W low-pressure mercury lamp was studied. Thereby, two flow injection systems (FIA) with and without irradiation were exhaustively optimized and their analytical characteristics studied. Better sensitivity and selectivity was found in absence of irradiation, due to the enhancing effect of hexadecylpyridinium chloride (HPC), which acted as a sensitizer.

FI-photoinduced chemiluminescence method for diuron determination in water samples.

A new method for the determination of the herbicide diuron, using a flow injection manifold and photoinduced chemiluminescence detection, is presented. The pesticide, in basic medium, was irradiated on-line with UV light (254 nm) for 53 s. A short discussion about the possible irradiation products is included.

Determination of diquat by flow injection-chemiluminescence.

A simple, economic, sensitive and rapid method for the determination of the pesticide diquat was described. This new method was based on the coupling of flow injection analysis methodology and direct chemiluminescent detection; to the authors' knowledge, this approach had not been used up to now with this pesticide. It was based on its oxidation with ferricyanide in alkaline medium; significant improvements in the analytical signal were achieved by using high temperatures and quinine as sensitiser.

A tandem-flow assembly for the chemiluminometric determination of hydroquinone.

A direct chemiluminescent procedure for determination of hydroquinone based on the emergent flow methodology known as multicommutation or tandem-flow is presented for first time. The manifold was based on a set of three channels and three solenoid valves; and, the determination was performed at 60 degrees C and at flow-rate of 7.5mlmin(-1).

Flow injection-photoinduced-chemiluminescence determination of ziram and zineb.

A simple, sensitive and rapid method for the determination of the pesticides ziram and zineb was described. This new method was based on the coupling of FIA methodology and direct chemiluminescent detection; this approach had not been used up to now with these pesticides. The additional use of an 'on line' photochemical reaction, which was performed by using a photoreactor consisting of a long piece of PTFE helically coiled around a 15W low-pressure lamp, increased by a factor >20 the chemiluminometric response of the pesticides.

Chemiluminescent determination of the pesticide bromoxynil by on-line photodegradation in a flow-injection system.

A new, robust and simple method is proposed for the chemiluminescent determination of the pesticide Bromoxynil. The empirical procedure is performed with the aid of a flow-injection manifold provided with an on-line photo-reactor to obtain chemiluminescent photofragments. After a period of 12 s of irradiation with an 8 W low-pressure mercury lamp, a chemiluminescent oxidation was performed with the system potassium permanganate in a polyphosphoric acid medium.

Fluorescence determination of the pesticide asulam by flow injection analysis.

This paper presents the analytical determination of the pesticide Asulam based on its native fluorescence. The method was optimized in either a flow injection analysis (FIA) assembly or in batch. The maximum fluorescence intensity was observed for basic pH solutions and at a lamda(ex) of 258 nm and a lamda(em) of 342 nm.

Automated simultaneous triple dissolution profiles of two drugs, sulphamethoxazole-trimethoprim and hydrochlorothiazide-captopril in solid oral dosage forms by a multicommutation flow-assembly and derivative spectrophotometry.

This article deals with the simultaneous determination of three dissolution profiles with the aid of the new and emerging continuous-flow methodology known as multicommutation. This methodology is based on a flow network of a set of solenoid valves controlled by the computer and acting as independent multicommutators to allow the easy and automated control of flowing solutions. The obtained three dissolution profiles from one dosage form are the whole formulation profile or "global profile" recommended by pharmacopoeias, and, at same time, are recorded two "individual" profiles from two drugs present in the formulation.

Three simultaneous dissolution profiles on a solid pharmaceutical formulation by a FIA manifold provided with a single spectrophotometric detector.

This article deals with the simultaneous determination of three dissolution profiles in the same pharmaceutical formulation. The officially proposed procedure from the pharmacopoeias is adapted to the FIA methodology to obtain the officially recommended profile or "global profile", and two "individual" profiles, corresponding to dissolution rate of two different active principles present in the formulation; both drugs have overlapped UV-vis spectra. The simultaneous determination of several profiles is based on the derivative spectra and the zero crossing mathematical procedure for the "individual" profiles of an active principle; the "global" profile of the formulation is obtained from the order zero derivative.