About eight years ago, a new automation approach and flow technique called "Lab-In-Syringe" was proposed. It was derived from previous flow techniques, all based on handling reagent and sample solutions in a flow manifold. To date Lab-In-Syringe has evidently gained the interest of researchers in many countries, with new modifications, operation modes, and technical improvements still popping up. It has proven to be a versatile tool for the automation of sample preparation, particularly, liquid-phase microextraction approaches. This article aims to assist newcomers to this technique in system planning and setup by overviewing the different options for configurations, limitations, and feasible operations. This includes syringe orientation, in-syringe stirring modes, in-syringe detection, additional inlets, and addable features. The authors give also a chronological overview of technical milestones and a critical explanation on the potentials and shortcomings of this technique, calculations of characteristics, and tips and tricks on method development. Moreover, a comprehensive overview of the different operation modes of Lab-In-Syringe automated sample pretreatment is given focusing on the technical aspects and challenges of the related operations. We further deal with possibilities on how to fabricate required or useful system components, in particular by 3D printing technology, with over 20 different elements exemplarily shown. Finally, a short discussion on shortcomings and required improvements is given.

• Klíčová slova
• 3D printing of instrument elements, Lab-In-Syringe, automation of sample pretreatment, potentials and troubles, system setup and operation modes, tips and tricks in method development,
• MeSH
• chemické techniky analytické přístrojové vybavení   metody   normy   MeSH
• injekční stříkačky * MeSH
• laboratorní automatizace * MeSH
• limita detekce MeSH
• reprodukovatelnost výsledků MeSH
• Publikační typ
• časopisecké články MeSH

Lab-In-Syringe direct immersion single drop microextraction is proposed as an automated sample pretreatment methodology and coupled online to HPLC with fluorescence detection for the determination of fluoroquinolones in environmental waters. For the first time, a drop of a natural deep eutectic solvent (NADES), synthesized from hexanoic acid and thymol, has been used as an extractant in automated single-drop microextraction. The extraction procedure was carried out within the 5 mL void of an automatic syringe pump. A 9-position head valve served the aspiration of all required solutions, air, waste disposal, and hyphenation with the HPLC instrument. Sample mixing during extraction was done by a magnetic stirring bar placed inside the syringe. Only 60 μL of NADES were required omitting toxic classical solvents and improving the greenness of the proposed methodology. By direct injection, linear working ranges between 0.1 and 5 μg L-1 were achieved for all fluoroquinolones. The limit of quantification values and enrichment factors ranged from 20 ng L-1 to 30 ng L-1 and 35 to 45, respectively. Accuracies obtained from the analysis of spiked surface water and wastewater treatment plant effluent analysis at two concentration levels (0.5 and 4 μg L-1) ranged from 84.6% to 119.7%, with RSD values typically <3%.

• Klíčová slova
• Automation of sample preparation, Directly immersed single drop microextraction, Fluoroquinolone antibiotics, Lab-in-syringe, Natural deep eutectic solvent, Online coupling to HPLC,
• MeSH
• automatizace MeSH
• fluorochinolony * MeSH
• hluboce eutektická rozpouštědla MeSH
• injekční stříkačky MeSH
• limita detekce MeSH
• mikroextrakce kapalné fáze * metody   MeSH
• ponoření MeSH
• rozpouštědla chemie   MeSH
• vysokoúčinná kapalinová chromatografie MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• fluorochinolony * MeSH
• hluboce eutektická rozpouštědla MeSH
• rozpouštědla MeSH

A critical overview on automation of modern liquid phase microextraction (LPME) approaches based on the liquid impregnation of porous sorbents and membranes is presented. It is the continuation of part 1, in which non-dispersive LPME techniques based on the use of the extraction phase (EP) in the form of drop, plug, film, or microflow have been surveyed. Compared to the approaches described in part 1, porous materials provide an improved support for the EP. Simultaneously they allow to enlarge its contact surface and to reduce the risk of loss by incident flow or by components of surrounding matrix. Solvent-impregnated membranes or hollow fibres are further ideally suited for analyte extraction with simultaneous or subsequent back-extraction. Their use can therefore improve the procedure robustness and reproducibility as well as it "opens the door" to the new operation modes and fields of application. However, additional work and time are required for membrane replacement and renewed impregnation. Automation of porous support-based and membrane-based approaches plays an important role in the achievement of better reliability, rapidness, and reproducibility compared to manual assays. Automated renewal of the extraction solvent and coupling of sample pretreatment with the detection instrumentation can be named as examples. The different LPME methodologies using impregnated membranes and porous supports for the extraction phase and the different strategies of their automation, and their analytical applications are comprehensively described and discussed in this part. Finally, an outlook on future demands and perspectives of LPME techniques from both parts as a promising area in the field of sample pretreatment is given.

• Klíčová slova
• Automation, Chromatomembrane, Dynamic liquid phase microextraction, Hollow-fibre liquid phase microextraction, Liquid phase microextraction, Miniaturisation, Static liquid phase microextraction, Supported liquid membrane microextraction,
• MeSH
• automatizace * MeSH
• membrány umělé * MeSH
• mikroextrakce kapalné fáze metody   MeSH
• poréznost MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH
• Názvy látek
• membrány umělé * MeSH

This article aims to provide an overview on the transition from earlier laboratory automation using analytical flow approaches toward today's applications of flow methodologies, recent developments, and future trends. The article is directed to flow practitioners while serving as a valuable reference to newcomers in the field in providing insight into flow techniques and conceptual differences in operation across the distinct flow generations. In the focus are the recently developed and complementary techniques Lab-On-Valve and Lab-In-Syringe. In the following, a brief comparison of the different application niches and contributions of flow techniques to past and modern analytical chemistry is given, including (i) the development of sample pretreatment approaches, (ii) the potential applicability for in-situ/on-site monitoring of environmental compartments or technical processes, (iii) the ability of miniaturization of laboratory chemistry, (iv) the unique advantages for implementation of kinetic assays, and finally (v) the beneficial online coupling with scanning or separation analytical techniques. We also give a critical comparison to alternative approaches for automation based on autosamplers and robotic systems. Finally, an outlook on future applications and developments including 3D prototyping and specific needs for further improvements is given. Graphical abstract ᅟ.

• Klíčová slova
• Automation and miniaturization, Flow techniques, Hyphenation, Lab-On-Valve and Lab-In-Syringe, Monitoring and surveillance, Sample pretreatment,
• Publikační typ
• časopisecké články MeSH

Simplicity, effectiveness, swiftness, and environmental friendliness - these are the typical requirements for the state of the art development of green analytical techniques. Liquid phase microextraction (LPME) stands for a family of elegant sample pretreatment and analyte preconcentration techniques preserving these principles in numerous applications. By using only fractions of solvent and sample compared to classical liquid-liquid extraction, the extraction kinetics, the preconcentration factor, and the cost efficiency can be increased. Moreover, significant improvements can be made by automation, which is still a hot topic in analytical chemistry. This review surveys comprehensively and in two parts the developments of automation of non-dispersive LPME methodologies performed in static and dynamic modes. Their advantages and limitations and the reported analytical performances are discussed and put into perspective with the corresponding manual procedures. The automation strategies, techniques, and their operation advantages as well as their potentials are further described and discussed. In this first part, an introduction to LPME and their static and dynamic operation modes as well as their automation methodologies is given. The LPME techniques are classified according to the different approaches of protection of the extraction solvent using either a tip-like (needle/tube/rod) support (drop-based approaches), a wall support (film-based approaches), or microfluidic devices. In the second part, the LPME techniques based on porous supports for the extraction solvent such as membranes and porous media are overviewed. An outlook on future demands and perspectives in this promising area of analytical chemistry is finally given.

• Klíčová slova
• Automation, Dynamic liquid phase microextraction, In-syringe liquid phase microextraction, Liquid phase microextraction, Microfluidic-based liquid phase microextraction, Miniaturisation, Single drop microextraction, Solvent plug microextraction, Static liquid phase microextraction, Wetting film microextraction,
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH

BACKGROUND: Alkylphenols are water contaminants of strong endocrine disruptive potential. Sample preparation is generally imperative to improve sensitivity and minimize matrix effects. Dispersive solid phase extraction is a powerful alternative to cartridge-based sorbent extraction omitting backpressure problems and reducing procedural time. Herein, solvent-dissolvable sorbents offer the advantages of easy and cost-efficient production, efficiency, and full analyte recovery, while eluates can be directly submitted to instrumental determination. Despite the potential to reduce environmental impact and enhance reproducibility, there is a lack of automation attempts. RESULTS: A fully automated solvent-assisted dispersive solid phase extraction method was developed for selected alkylphenols based on the technique Lab-In-Syringe. The void of automatic bidirectional syringe pump was used as mixing and extraction vessel. The iron(III) thenoyltrifluoroacetonate complex was used as novel dissolvable sorbent. 40 μL complex solution was dispersed in the sample, leading to the precipitation of 0.4 mg sorbent. Extraction occurred within 40 s and was accelerated by in-syringe magnetic stirring. The sorbent was retained on a melamine foam packing in the syringe inlet, dissolved in a methanolic solution of ascorbic acid, and injected into online-coupled HPLC. Linear working ranges were achieved from 1 to 1000 μg/L with sub-ppb detection limits and accuracies ranging from 98.3 to 110 %. SIGNIFICANCE: In this work, we explored for the first time automated in-syringe automated dispersive SPE based on a dissolvable sorbent. Parallel operation of sample pretreatment and separation enabled throughputs of 4.5/h with typically <5 % RSD and preconcentrations of 16.4-21.2. AGREE greenness evaluation yielded a score of 0.59.

• Klíčová slova
• Alkylphenols, High performance liquid chromatography, Iron(III) thenoyltrifluoroacetonate complex, Lab-in-syringe automation, Solvent-assisted dispersive solid phase Extraction,
• MeSH
• adsorpce MeSH
• automatizace MeSH
• chemické látky znečišťující vodu * analýza   izolace a purifikace   MeSH
• chromatografie kapalinová MeSH
• fenoly * analýza   izolace a purifikace   chemie   MeSH
• injekční stříkačky MeSH
• limita detekce MeSH
• mikroextrakce na pevné fázi * přístrojové vybavení   metody   MeSH
• vysokoúčinná kapalinová chromatografie MeSH
• železité sloučeniny * chemie   MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• chemické látky znečišťující vodu * MeSH
• fenoly * MeSH
• železité sloučeniny * MeSH

A simple and automated HPLC column-switching method with rapid sample pretreatment has been developed for quantitative determination of β-carotene in food supplements. Commercially samples of food supplements were dissolved in chloroform with help of saponification with 1M solution of sodium hydroxide in ultrasound bath. A 20-min sample dissolution/extraction step was necessary before chromatography analysis to transfer β-carotene from solid state of food supplements preparations (capsules,tablets) to chloroform solution. Sample volume - 3μL of chloroform phase was directly injected into the HPLC system. Next on-line sample clean-up was achieved on the pretreatment precolumn Chromolith Guard Cartridge RP-18e (Merck), 10×4.6mm, with a washing mobile phase (methanol:water, 92:8, (v/v)) at a flow rate of 1.5mL/min. Valve switch to analytical column was set at 2.5min in a back-flush mode. After column switching to the analytical column Ascentis Express C-18, 30×4.6mm, particle size 2.7μm (Sigma Aldrich), the separation and determination of β-carotene in food supplements was performed using a mobile phase consisting of 100% methanol, column temperature at 60°C and flow rate 1.5mL/min. The detector was set at 450nm. Under the optimum chromatographic conditions standard calibration curve was measured with good linearity - correlation coefficient for β-carotene (r(2)=0.999014; n=6) between the peak areas and concentration of β-carotene 20-200μg/mL. Accuracy of the method defined as a mean recovery was in the range 96.66-102.40%. The intraday method precision was satisfactory at three concentration levels 20, 125 and 200μg/mL and relative standard deviations were in the range 0.90-1.02%. The chromatography method has shown high sample throughput during column-switching pretreatment process and analysis in one step in short time (6min) of the whole chromatographic analysis.

• MeSH
• beta-karoten analýza   izolace a purifikace   MeSH
• extrakce na pevné fázi MeSH
• potravní doplňky analýza   MeSH
• senzitivita a specificita MeSH
• vysokoúčinná kapalinová chromatografie přístrojové vybavení   metody   MeSH
• Publikační typ
• časopisecké články MeSH
• hodnotící studie MeSH
• práce podpořená grantem MeSH
• Názvy látek
• beta-karoten MeSH

Enhanced sensitivity for determination of basic drugs in body fluids was achieved by in-line coupling of extraction across supported liquid membrane (SLM) to large electrokinetic injection and transient isotachophoresis-capillary zone electrophoresis (tITP-CZE) in commercial CZE instrument. Twelve cm long tITP plug of 300mM ammonium acetate was formed in the separation capillary just before the electrokinetic injection of acceptor solution containing nortriptyline, haloperidol and loperamide extracted across the SLM. The tITP plug ensured efficient stacking and preconcentration of the injected basic drugs due to the tITP action of ammonium and the drugs were then separated by CZE using 5.2M acetic acid as background electrolyte. No interferences were observed from highly-abundant body fluid species (NaCl and human serum albumin) due to the excellent clean-up properties of SLMs and analytical sensitivity increased up to 340 times compared to SLM extractions coupled in-line to CZE with standard hydrodynamic injections. The SLM-tITP-CZE method was characterized by good repeatability (RSDs of peak areas below 7.8%), linearity over two orders of magnitude (r(2) better than 0.994) and limits of detection (defined as 3×S/N) between 3 and 45μg/L. Interfacing of SLM extractions to CZE instrumentation was achieved by low-cost, disposable micro-extraction devices, which can be routinely prepared in every analytical laboratory. These devices eliminated sample carry-over, minimized the need for manual sample handling and ensured fully automated determination (including extraction, injection, preconcentration and separation) of the three basic drugs in 20μL of untreated body fluids.

• Klíčová slova
• Capillary electrophoresis, Complex samples, In-line sample pretreatment, Supported liquid membranes, Transient isotachophoresis,
• MeSH
• chemické techniky analytické přístrojové vybavení   metody   MeSH
• elektroforéza kapilární * MeSH
• izotachoforéza * MeSH
• lidé MeSH
• membrány umělé MeSH
• tělesné tekutiny chemie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• membrány umělé MeSH

For the pretreatment of wood, charcoal and collagen from bone micro samples using the Acid-Base-Acid (ABA) method, we have assembled an automated computer-controlled unit in our laboratory CRL. The sample is placed in a glass single-necked cuvette. The machine consists of prepared solutions which are guided through capillaries, switching valve and peristaltic pump into the cuvette with the sample according to the currently selected program. The automat can be used for the pretreatment of charcoal, wood and also collagen from bones.

• MeSH
• alkálie chemie   MeSH
• dřevěné a živočišné uhlí chemie   MeSH
• dřevo chemie   MeSH
• kolagen chemie   MeSH
• kosti a kostní tkáň chemie   MeSH
• kyseliny chemie   MeSH
• laboratorní automatizace metody   MeSH
• lidé MeSH
• radioaktivní datování metody   MeSH
• radioizotopy uhlíku analýza   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• alkálie MeSH
• dřevěné a živočišné uhlí MeSH
• kolagen MeSH
• kyseliny MeSH
• radioizotopy uhlíku MeSH

Over the last five decades, many methods to analyze thiamine (vitamin B1) and its phosphorylated forms in urine, whole blood, serum, plasma and erythrocytes have been proposed. Some of the methods are presently used in routine practice, but analytical problems regarding reproducibility, standardization, lack of automation, time consuming procedures for pretreatment and analysis are often discussed. With modern approaches to bioanalysis in clinical research of vitamins, whole processes can be automated, making analysis less time consuming, with reduced consumption of solvents and samples. This review critically discusses various analytical techniques, their advantages and disadvantages that are used for determination of thiamine and its derivatives in clinical practice, with emphasis on accurate, reliable and fast analytical procedures.

• Klíčová slova
• Bioanalysis, Blood, Chromatography, Sample preparation, Thiamine, Vitamin B,
• MeSH
• erytrocyty chemie   MeSH
• klinická chemie normy   trendy   MeSH
• lidé MeSH
• referenční standardy MeSH
• reprodukovatelnost výsledků MeSH
• thiamin analýza   krev   moč   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• přehledy MeSH
• Názvy látek
• thiamin MeSH