scholarly journals DETERMINATION OF SELECTED PESTICIDES IN HONEY BY LC-MS-IT: EFFECTS OF SAMPLE PREPARATION

2012 ◽  
Vol 2 (4) ◽  
Author(s):  
Marija Ilić ◽  
Ljubica Svilar ◽  
Snežana Jovanović ◽  
Aleksandra Đorđević ◽  
Violeta Mitic ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Nutritional Value ◽  
Ion Trap ◽  
Preparation Method ◽  
Solid Phase ◽  
Mass Analyzer ◽  
Liquid Chromatography Mass Spectrometry ◽  
Human Diet ◽  
Liquid Liquid Extraction

Honey is well known in human diet and it is considered to be one of the healthiest foods with high nutritional value. Due to the growing presence of anthropogenic contaminants, with extremely long half-life and prevalence in all environments, some of them may be present in honey. Honey samples were spiked with six pesticides which are commonly used at the time of plant's blooming, in order to develop an efficient method for preparing honey samples for LC-MS-IT analysis. Samples of honey, spiked with soultion containing mixture of six pesticides (pirimicarb, atrazine, prometrine, malation, cyprodinil and famoxadone), were treated applying SPE with Florisil and C18 cartriges, as well as liquid-liquid extraction method. Afterwards, samples were injected in the HPLC with ESI ionisation source, and IT (ion trap) mass analyzer. Methanol solution of pesticides in the same concentrations as in spiked samples, were used as blank. In spiked honey samples, after treatment with Florisil prometrine and famoxadon were detected; with C18, atrazine and prometrine; after LLE famoxedon and pirimicarb. In the specific case, as acceptable sample preparation method SPE with Florisil cartridge may be proposed, since it enables reliable identification of the most examined pesticides. Key words: honey, pesticides, liquid chromatography, mass spectrometry, solid phase extraction

scholarly journals Determination of N-Nitrosamines by Gas Chromatography Coupled to Quadrupole–Time-of-Flight Mass Spectrometry in Water Samples

Separations ◽  
2020 ◽  
Vol 7 (1) ◽  
pp. 3 ◽  
Author(s):  
Benigno José Sieira ◽  
Inmaculada Carpinteiro ◽  
Rosario Rodil ◽  
José Benito Quintana ◽  
Rafael Cela
Keyword(s):  
Mass Spectrometry ◽  
Environmental Protection Agency ◽  
Ion Trap ◽  
Solid Phase ◽  
Classical Method ◽  
Tap Water ◽  
Time Of Flight ◽  
The United States ◽  
Mass Analyzer

An analytical method based on high-resolution quadrupole–time-of-flight (QToF) mass spectrometry has been developed as an alternative to the classical method, using a low-resolution ion trap (IT) analyzer to reduce interferences in N-nitrosamines determination. Extraction of the targeted compounds was performed by solid-phase extraction (SPE) following the United States Environmental Protection Agency (USEPA) -521 method. First, both electron impact (EI) and positive chemical ionization (PCI) using methane as ionization gas were compared, along with IT and QToF detection. Then, parameters such as limits of detection (LOD) and quantification (LOQ), linearity, and repeatability were assessed. The results showed that the QToF mass analyzer combined with PCI was the best system for the determination of the N-nitrosamines, with instrumental LOD and LOQ in the ranges of 0.2–4 and 0.6–11 ng mL−1, respectively, which translated into method LOD and LOQ in the ranges of 0.2–1.3 and 0.6–3.9 ng L−1, respectively. The analysis of real samples showed the presence of 6 of the N-nitrosamines in influent, effluent, and tap water. N-nitrosodimethylamine (NDMA) was quantified in all the analyzed samples at concentrations between 1 and 27 ng L−1. Moreover, four additional nitrosamines were found in tap and wastewater samples.

scholarly journals Determination of Seventeen Polar/Thermolabile Pesticides in Apples and Apricots by Liquid Chromatography/Mass Spectrometry

2003 ◽  
Vol 86 (3) ◽  
pp. 612-622 ◽  
Author(s):  
Jitka Zrostlíková ◽  
Jana Hajšlová ◽  
Tomáš Kovalczuk ◽  
Radim Štěpán ◽  
Jan Poustka
Keyword(s):  
Liquid Chromatography ◽  
Ion Trap ◽  
Solid Phase ◽  
Reversed Phase ◽  
Simple Liquid ◽  
Liquid Chromatography Mass Spectrometry ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
Mass Spectrome

Abstract A simple liquid chromatography/mass spectrome-try (LC/MS) approach for the determination of widely used representatives of polar/thermolabile pesticides in fruits was developed and validated. The group of pesticides comprised benzimidazoles and azoles (carbendazim, thiabendazole, imazalil, propiconazole, prochloraz, epoxiconazole, flusilazole, tebuconazole, bitertanol); N-methylcarbamates (carbaryl, carbofuran, methiocarb); and phenylureas and benzoylphenylureas (linuron, diflubenzuron, triflumuron, teflubenzuron, flufenoxuron). Matrixes (apple, apricot) were extracted with acetonitrile and crude extracts were cleaned up by solid-phase ex-traction (SPE) using either mixed cation exchange or hydrophilic lipophilic balance cartridges. LC separation of pesticides was performed on a reversed-phase column, Discovery C18. Electrospray ionization and ion trap MS/MS detection were applied. For most pesticides, overall recoveries ranged from 75 to 122%, and repeatability (as relative standard deviation) from 5 repetitive determinations of recovery ranged from 3 to 21%. Carbofuran was the only compound for which recovery was not satisfactory due to its loss in the SPE cleanup step. Limits of detection were 0.1–3 μg/kg for benzimidazole and azole fungicides and carbamate insecticides. For urea insecticides, detection limits were slightly higher (3–10 μg/kg).

scholarly journals Matrix-Induced Sugaring-Out: A Simple and Rapid Sample Preparation Method for the Determination of Neonicotinoid Pesticides in Honey

Molecules ◽  
2019 ◽  
Vol 24 (15) ◽  
pp. 2761 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Jianbo Hou ◽  
...  
Keyword(s):  
Phase Separation ◽  
Sample Preparation ◽  
Preparation Method ◽  
Liquid Extraction ◽  
Subzero Temperature ◽  
Water Mixture ◽  
Sample Preparation Method ◽  
Liquid Liquid Extraction ◽  
Neonicotinoid Pesticides

In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.

Salting-out-assisted liquid–liquid extraction of 5-hydroxymethylfurfural from honey and the determination of 5-hydroxymethylfurfural by high-performance liquid chromatography

2019 ◽  
Vol 11 (37) ◽  
pp. 4835-4841 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Xiaoqing Miao ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
High Performance ◽  
Preparation Method ◽  
Liquid Extraction ◽  
Sample Preparation Method ◽  
Salting Out ◽  
Liquid Liquid Extraction

A simple, rapid, and effective sample preparation method was developed for the recovery of 5-hydroxymethylfurfural from honey samples with negligible co-extracted sugars.

scholarly journals Determination of Chlormequat in Fruit Samples by Liquid Chromatography-Electrospray-Mass Spectrometry/Mass Spectrometry

2001 ◽  
Vol 84 (6) ◽  
pp. 1903-1908 ◽  
Author(s):  
Rocio Castro ◽  
Encarnación Moyano ◽  
Maria Teresa Galceran
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ion Trap ◽  
Solid Phase ◽  
Ion Pair ◽  
Mass Analyzer ◽  
The European Union ◽  
Fruit Samples ◽  
Mass Spectrometry Mass Spectrometry

Abstract An ion-pair liquid chromatography-mass spectrometry/mass spectrometry method was developed for the determination of chlormequat in fruit samples. A solid-phase extraction cleanup procedure with C18 cartridges was used. Sample preparation was simple and the achieved detection limit (0.03 mg/kg) and quantitation limit (0.08 mg/kg) were below the maximum residue levels legislated by the European Union. The chromatographic separation was performed by using a C8 column and heptafluorobutyric acid as ion pair reagent. The detection was conducted with an electrospray source and an ion trap as a mass analyzer. The reproducibility of the method gave good run-to-run (8–9%) and day-to-day (9–13%) precision values, and its applicability to the determination of chlormequat in pears and grapes, purées, and pear, apple, and grape juices was demonstrated.

Recent Trends in the Development of Green Microextraction Techniques for the Determination of Hazardous Organic Compounds in Wine

2019 ◽  
Vol 15 (7) ◽  
pp. 788-800 ◽  
Author(s):  
Natasa P. Kalogiouri ◽  
Victoria F. Samanidou
Keyword(s):  
Sample Preparation ◽  
Solid Phase Extraction ◽  
Organic Compounds ◽  
Method Development ◽  
Solid Phase ◽  
Stir Bar Sorptive Extraction ◽  
Phase Extraction ◽  
Microextraction Techniques ◽  
Hazardous Organic Compounds

Background:The sample preparation is the most crucial step in the analytical method development. Taking this into account, it is easily understood why the domain of sample preparation prior to detection is rapidly developing. Following the modern trends towards the automation, miniaturization, simplification and minimization of organic solvents and sample volumes, green microextraction techniques witness rapid growth in the field of food quality and safety. In a globalized market, it is essential to face the consumers need and develop analytical methods that guarantee the quality of food products and beverages. The strive for the accurate determination of organic hazards in a famous and appreciated alcoholic beverage like wine has necessitated the development of microextraction techniques.Objective:The objective of this review is to summarize all the recent microextraction methodologies, including solid phase extraction (SPE), solid phase microextraction (SPME), liquid-phase microextraction (LPME), dispersive liquid-liquid microextraction (DLLME), stir bar sorptive extraction (SBSE), matrix solid-phase dispersion (MSPD), single-drop microextraction (SDME) and dispersive solid phase extraction (DSPE) that were developed for the determination of hazardous organic compounds (pesticides, mycotoxins, colorants, biogenic amines, off-flavors) in wine. The analytical performance of the techniques is evaluated and their advantages and limitations are discussed.Conclusion:An extensive investigation of these techniques remains vital through the development of novel strategies and the implication of new materials that could upgrade the selectivity for the extraction of target analytes.

scholarly journals A Toolbox for the Determination of Nitroaromatic Explosives in Marine Water, Sediment, and Biota Samples on Femtogram Levels by GC-MS/MS

Toxics ◽  
2021 ◽  
Vol 9 (3) ◽  
pp. 60
Author(s):  
Tobias Hartwig Bünning ◽  
Jennifer Susanne Strehse ◽  
Ann Christin Hollmann ◽  
Tom Bötticher ◽  
Edmund Maser
Keyword(s):  
Sample Preparation ◽  
Freeze Drying ◽  
Solid Phase ◽  
Phase Extraction ◽  
Direct Extraction ◽  
Time Saving ◽  
Marine Samples ◽  
Volume Method ◽  
Biota Samples

To determine the amount of the explosives 1,3-dinitrobenzene, 2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and its metabolites in marine samples, a toolbox of methods was developed to enhance sample preparation and analysis of various types of marine samples, such as water, sediment, and different kinds of biota. To achieve this, established methods were adapted, improved, and combined. As a result, if explosive concentrations in sediment or mussel samples are greater than 10 ng per g, direct extraction allows for time-saving sample preparation; if concentrations are below 10 ng per g, techniques such as freeze-drying, ultrasonic, and solid-phase extraction can help to detect even picogram amounts. Two different GC-MS/MS methods were developed to enable the detection of these explosives in femtogram per microliter. With a splitless injector, limits of detection (LODs) between 77 and 333 fg/µL could be achieved in only 6.25 min. With the 5 µL programmable temperature vaporization—large volume method (PTV-LVI), LODs between 8 and 47 fg/µL could be achieved in less than 7 min. The detection limits achieved by these methods are among the lowest published to date. Their reliability has been tested and confirmed by measuring large and diverse sample sets.

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