Search results for "sample preparation"
showing 10 items of 343 documents
Pressurized liquid extraction combined with capillary electrophoresis–mass spectrometry as an improved methodology for the determination of sulfonami…
2007
A new analytical method, based on capillary electrophoresis and tandem mass spectrometry (CE-MS2), is proposed and validated for the identification and simultaneous quantification of 12 sulfonamides (SAs) in pork meat. The studied SAs include sulfathiazole, sulfadiazine, sulfamethoxypyridazine, sulfaguanidine, sulfanilamide, sulfadimethoxyne, sulfapyridine, sulfachloropyridazine, sulfisoxazole, sulfasalazine, sulfabenzamide and sulfadimidine. Different parameters (i.e. separation buffer, sheath liquid, electrospray conditions) were optimized to obtain an adequate CE separation and high MS sensitivity. MS2 experiments using an ion trap as analyzer, operating in the selected reaction monitori…
An effective negative pressure cavitation-microwave assisted extraction for determination of phenolic compounds in P. calliantha H. Andr.
2013
A novel negative pressure and microwave assisted extraction technique (NMAE) was first proposed and applied for extraction of phenolic compounds from pyrola. [C₄MIM]BF₄ aqueous solution was selected as extraction solvent. Optimal extraction conditions were microwave power 700 W, negative pressure -0.07 MPa, temperature 40 °C, liquid-solid ratio 20 : 1, ionic liquid (IL) concentration 0.5 M, extraction time 15 min. The predominance of NMAE was investigated by comparing with microwave-assisted extraction (MAE) and negative pressure cavitation extraction (NPCE) using a first-order kinetics equation. The C∞ values of the target compounds by NMAE were from 0.406 to 5.977 mg g⁻¹ higher than these…
Rapid analysis of effluents generated by the dairy industry for fat determination by preconcentration in nylon membranes and attenuated total reflect…
2014
Abstract This paper describes a new approach for the determination of fat in the effluents generated by the dairy industry which is based on the retention of fat in nylon membranes and measurement of the absorbances on the membrane surface by ATR-IR spectroscopy. Different options have been evaluated for retaining fat in the membranes using milk samples of different origin and fat content. Based on the results obtained, a method is proposed for the determination of fat in effluents which involves the filtration of 1 mL of the samples through 0.45 µm nylon membranes of 13 mm diameter. The fat content is then determined by measuring the absorbance of band at 1745 cm −1 . The proposed method c…
On-line extraction coupled to liquid chromatographic analysis of hydrophobic organic compounds from complex solid samples-Application to the analysis…
2019
This work investigates the applicability of on-line extraction (OLE) directly coupled to liquid chromatography (LC) for the dynamic extraction of hydrophobic organic compounds from complex solid samples. The method operates within the existing apparatus of the LC by replacing the valve loop with an extraction vessel comprised of an empty guard column loaded with the sample. In this manner, extraction is accomplished by the mobile phase as it flows through the extraction vessel under high pressure without the need for additional apparatus other than those comprising the LC system or additional sample pretreatment steps. The experimental parameters affecting the extraction efficiency of the m…
Rugged Large Volume Injection for Sensitive Capillary LC-MS Environmental Monitoring
2017
A rugged and high throughput capillary column (cLC) LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL) solid phase extraction (SPE) for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g. injection of 100 non-filtrated water samples would did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 µm). In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for …
Trace analysis by ion mobility spectrometry: From conventional to smart sample preconcentration methods. A review.
2018
Ion mobility spectrometry (IMS) is a rapid and high sensitive technique widely used in security and forensic areas. However, a lack of selectivity is usually observed in the analysis of complex samples due to the scarce resolution of the technique. The literature concerning the use of conventional and novel smart materials in the pretreatment and preconcentration of samples previous to IMS determinations has been critically reviewed. The most relevant strategies to enhance selectivity and sensitivity of IMS determinations have been widely discussed, based in the use of smart materials, as immunosorbents, aptamers, molecularly imprinted polymers (MIPs), ionic liquids (ILs) and nanomaterial. …
Determination of total ribonucleotide pool in plant materials by high-pH anion-exchange high-performance liquid chromatography following extraction w…
2005
A new, improved method that only requires a potassium hydroxide extraction procedure is presented for the analysis of a full nucleotide pool in plant materials. Quantification was performed by high-pH anion-exchange chromatography (HPAEC) with UV detection after a potassium hydroxide extraction, and allowed the quantification of 13 linear ribonucleotides in a single run. The method has been validated by comparison of six extraction methods and also by measurement of the intracellular nucleotide levels of three plant species (cell cultures and leaves). The evolution of the nucleotide pool of Nicotiana tabacum cell culture during growth has also been measured, and showed an increase in the po…
Evaluation of mycotoxins and their metabolites in human breast milk using liquid chromatography coupled to high resolution mass spectrometry
2014
Humans can be exposed to mycotoxins through the food chain. Mycotoxins are mainly found as contaminants in food and could be subsequently excreted via biological fluids such as urine or human breast milk in native or metabolised form. Since breast milk is usually supposed as the only food for new-borns, the occurrence of mycotoxins in thirty-five human milk samples was evaluated by a newly developed method based on QuEChERS extraction and UHPLC-HRMS detection. The method described here allows the detection of target mycotoxins in order to determine the quality of this initial feeding. The method has been fully validated, with recoveries ranging from 64% to 93% and relative standard deviatio…
Alteration of the structural properties of inulin gels
2019
Abstract In this work, inulin particle gels, prepared with a type of long chain inulin, were examined in terms of their structural properties and mechanical response, depending on the applied shear rates and temperature during gel preparation. The results are interpreted on the basis of a particle gel model, which takes into account the varying gel structure, depending on the sample preparation parameters. X-ray measurements of the inulin powder, used for the experiments, revealed a mostly amorphous powder. The temperature profiles for the sample preparation, chosen from 25 °C to 60 °C with constant stirring at 600 rpm, yielded viscoelastic particle gels with decreasing hardness. By applica…
Manual packing and soil reuse effects on determination of saturated hydraulic conductivity of a loam soil
2022
Abstract Performing laboratory measurement of saturated hydraulic conductivity, Ks, of sieved soil is important for many scientific purposes such as testing theories and methods to determine Ks. A given soil mass can be used only once or it can be reused after a previous use. Little is known on the dependence of the Ks measurements on both the applied packing method and the reuse of the same soil mass. This lack of knowledge makes comparisons among different investigations more or less uncertain. Four packing methods were tested on an initially dry loam soil by measuring Ks with the simplified falling head (SFH) technique. The four methods differed by the used compacting procedure (dropping…