INTRODUCTION: The analysis of plant and herbal samples is a challenging task for analytical chemists due to the complexity of the matrix combined with the low concentration of analytes. In recent years different liquid-phase microextraction (LPME) techniques coupled with a variety of analytical equipment have been developed for the determination of both organic and inorganic analytes. OBJECTIVE: Over the past few years, the number of research papers in this field has shown a markedly growing tendency. Therefore, the purpose of this review paper is to summarise and critically evaluate research articles focused on the application of LPME techniques for the analysis of plant and herbal samples. RESULTS: Due to the complex nature of the samples, the direct application of LPME techniques to the analysis of plants has not often been done. LPME techniques as well as their modalities have been commonly applied in combination with other pretreatment techniques, including a solid-liquid extraction technique supported by mechanical agitation or auxiliary energies for plant analysis. Applications and the most important parameters are summarised in the tables. CONCLUSION: This review summarises the application of the LPME procedure and shows the major benefits of LPME, such as the low volume of solvents used, high enrichment factor, simplicity of operation and wide selection of applicable detection techniques. We can expect further development of microextraction analytical methods that focus on direct sample analysis with the application of green extraction solvents while fully automating procedures for the analysis of plant materials.
- MeSH
- Liquid Phase Microextraction * MeSH
- Plants MeSH
- Solvents MeSH
- Publication type
- Journal Article MeSH
- Review MeSH
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.
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
- Alkalies chemistry MeSH
- Charcoal chemistry MeSH
- Wood chemistry MeSH
- Collagen chemistry MeSH
- Bone and Bones chemistry MeSH
- Acids chemistry MeSH
- Automation, Laboratory methods MeSH
- Humans MeSH
- Radiometric Dating methods MeSH
- Carbon Radioisotopes analysis MeSH
- Check Tag
- Humans MeSH
- Publication type
- Journal Article 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.
- Publication type
- Journal Article MeSH
Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail.
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.
- MeSH
- Erythrocytes chemistry MeSH
- Chemistry, Clinical standards trends MeSH
- Humans MeSH
- Reference Standards MeSH
- Reproducibility of Results MeSH
- Thiamine analysis blood urine MeSH
- Check Tag
- Humans MeSH
- Publication type
- Journal Article MeSH
- Review MeSH
This work presents the development of a fully automated flow-batch analysis (FBA) system as a new approach for on-line preconcentration, photodegradation and fluorescence detection in a lab-constructed mixing chamber that was designed to perform these processes without sample dispersion. The system positions the mixing chamber into the detection system and varies the instrumental parameters according to the required photodegradation conditions. The developed FBA system is simple and easily coupled with any sample pretreatment without altering the configuration. This FBA system was implemented to photodegrade and determine the fluorescence of the degradation products of metsulfuron methyl (MSM), a naturally non-fluorescent herbicide of the sulfonylurea׳s family. An on-line solid phase extraction (SPE) and clean up procedure using a C18 minicolumn was coupled to the photodegradation-detection mixing chamber (PDMC) that was located in the spectrofluorometer. An enrichment factor of 27 was achieved. Photodegradation conditions have been optimized by considering the influence of the elution solvent on both the formation of the photoproduct and on the fluorescence signal. Under optimal conditions, the calibration for the MSM determination was linear over the range of 1.00-7.20 µg L(-1). The limit of detection (LOD) was 0.28 µg L(-1); the relative standard deviation was 2.0% and the sample throughput for the entire process was 3h(-1). The proposed method was applied to real water samples from the Bahía Blanca׳s agricultural region (Bahía Blanca, Buenos Aires, Argentina). This method obtained satisfactory recoveries with a range of 94.7-109.8%.
- MeSH
- Arylsulfonates analysis MeSH
- Solid Phase Extraction MeSH
- Spectrometry, Fluorescence MeSH
- Photochemistry methods MeSH
- Photolysis MeSH
- Herbicides analysis MeSH
- Calibration MeSH
- Hydrogen-Ion Concentration MeSH
- Water Pollutants analysis MeSH
- Limit of Detection MeSH
- Reproducibility of Results MeSH
- Sulfonylurea Compounds analysis MeSH
- Light MeSH
- Green Chemistry Technology MeSH
- Water chemistry MeSH
- Publication type
- Journal Article MeSH
- Research Support, Non-U.S. Gov't MeSH