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Vagner Bezerra Dos Santos, Daniela Daniel, Melina Singh, Claudimir Lucio do Lago
A capillary electrophoresis-tandem mass spectrometry (CE-MS/MS) method for amphetamine (AM), phentermine (PTM), methamphetamine (MAM), methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA), and methylenedioxyethylamphetamine (MDEA) in commercial samples of homeopathic and phytotherapic medicines and dietary supplements is presented. The samples were submitted to a modified QuEChERS extraction procedure (at apparent pH 13) followed by electrophoretic separation in 0.1molL(-1) formic acid electrolyte (pH 2...
October 17, 2016: Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Jesús Marín-Sáez, Roberto Romero-González, Antonia Garrido Frenich
A new method has been developed for the enantioselective separation of (-) and (+) hyoscyamine in Solanaceaes seeds and contaminated buckwheat. Chromatographic separation was optimized, evaluating two chiral columns, Chirobiotic V and Chiralpal-AY3. Better resolution was obtained using a Chiralpak-AY3 column, utilizing as mobile phase ethanol (0.1% diethanolamine). An extraction procedure based on a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) was applied, using water and acetonitrile containing 1% of acetic acid, and a clean-up step utilizing primary secondary amine (PSA) and graphitized carbon black (GCB) as sorbents...
October 19, 2016: Journal of Chromatography. A
Tianyang Guo, Pingping Fang, Juanjuan Jiang, Feng Zhang, Wei Yong, Jiahui Liu, Yiyang Dong
A rapid method to screen and quantify multi-class analytic targets in red wine has been developed by direct analysis in real time (DART) coupled with triple quadruple tandem mass spectrometry (QqQ-MS). A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for increasing analytical speed and reducing matrix effect, and the multiple reaction monitoring (MRM) in DART-MS/MS ensured accurate analysis. One bottle of wine containing 50 pesticides and 12 adulterants, i.e., preservatives, antioxidant, sweeteners, and azo dyes, could be totally determined less than 12min...
October 1, 2016: Journal of Chromatography. A
Lobna A Hussein, Noha F El Azab, Maha F Abdel-Ghany
A sensitive, selective, and validated HPLC-diode-array detection method was developed for the simultaneous determination of five neonicotinoid insecticides-acetamiprid, imidacloprid, nitenpyram, flonicamid, and thiacloprid-and their primary metabolite, 6-chloronicotinic acid, in cucumbers and soil based on the quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique as a pretreatment procedure. In the QuEChERS procedure, cucumber samples were extracted with acetonitrile and cleaned using C18, whereas soil samples were extracted with an acetonitrile-dichloromethane mixture (1 + 2)...
October 19, 2016: Journal of AOAC International
E Kowalczyk, E Patyra, A Grelik, K Kwiatek
A high performance liquid chromatography combined with fluorescence detection (HPLC-FLD) method was developed for determination of five ergot alkaloids (EA): ergometrine, ergotamine, ergocornine, ergocrypine and ergocristine in animal feedingstuffs. The method was based on the application of QuEChERS salts for extraction and modified QuEChERS dispersive SPE for the cleanup step. Alkaloids separation was performed on a C18, 250 mm x 4.6 mm, 5 μm column with the mobile phase containing ammonium carbonate and acetonitrile...
September 1, 2016: Polish Journal of Veterinary Sciences
Martin Waterstraat, Andreas A Hildebrand, Margit Rosler, Mirko Bunzel
Forage plants of the Poaceae family are grown as pasturage or used for the production of hay, straw, corn stover, etc. Although ferulic acid contents of grasses are generally high, the amount of ingested ferulic acid differs depending on the type of forage resulting in varying contents of ferulic acid and its microbial and hepatic metabolites in milk. Concentrations and patterns of these metabolites may be used as markers to track different forages in livestock feeding. Therefore, we developed a stable isotope dilution assay to quantitate ferulic acid, twelve ferulic acid based metabolites, p coumaric acid, and cinnamic acid in milk...
October 15, 2016: Journal of Agricultural and Food Chemistry
Mouna Necibi, Laurent Lanceleur, Nadia Mzoughi, Mathilde Monperrus
A new analytical method for the simultaneous determination of eight synthetic musks compounds (SMs) including five polycyclic musks (PCMs) and three nitro musks (NMs) was validated for sediment samples based on a simple QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation procedure followed by gas chromatography-mass spectrometry (GC-MS). Good analytical performances were obtained for all the target compounds. For the validation of the method, internal calibration (IC) and internal calibration with QuEChERS (ICQ) were compared...
October 14, 2016: Bulletin of Environmental Contamination and Toxicology
Qingxin Zhou, Fenghua Li, Leilei Chen, Dafeng Jiang
A simple and sensitive analytical method for quantitative analysis of 10 mycotoxins was developed and validated by a combination of modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure with ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Sample preparation involved QuEChERS with dispersive solid phase extraction for clean-up, and analysis was performed by reversed-phase UHPLC-MS/MS using electrospray negative ionization and multiple reaction monitoring...
October 12, 2016: Journal of Food Science
Jian Du, Zoya Gridneva, Melvin C L Gay, Robert D Trengove, Peter E Hartmann, Donna T Geddes
Persistent organic pollutants in human milk (HM) at high levels are considered to be detrimental to the breastfed infant. To determine the pesticide concentration in HM, a pilot cross-sectional study of 40 Western Australian (WA) women was carried out. Gas chromatography-tandem mass spectrometry (GC-MS/MS) with a validated QuEChERS was used for the analysis of 88 pesticides in HM. p,p'-dichlorodiphenyldichloroethylene (p,p'-DDE) with a mean concentration of 62.8 ± 54.5 ng/g fat was found, whereas other organochlorines, organophosphates, carbamates and pyrethroids were not detected in HM...
October 8, 2016: Chemosphere
Mário Paz, Luísa Correia-Sá, Carla B Vidal, Helena Becker, Elisane Longhinotti, Valentina F Domingues, Cristina Delerue-Matos
The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was applied to the extraction of 14 organochlorine pesticides (OCPs) residues from commercial fruit pulps available in supermarkets in Fortaleza, Northeastern Brazil. The analyses were carried out by gas chromatography (GC), coupled to an electron-capture detector (ECD), and were confirmed by GC-tandem mass spectrometry (MS). The parameters of the analytical method, such as accuracy, precision, linear range, limits of detection and quantification, were determined for each pesticide...
October 11, 2016: Journal of Environmental Science and Health. Part. B, Pesticides, Food Contaminants, and Agricultural Wastes
Hongping Chen, Jesús Marín-Sáez, Roberto Romero-González, Antonia Garrido Frenich
A method was developed for the determination of atropine and scopolamine in buckwheat and related products. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure was evaluated. Dispersive solid phase extraction (d-SPE) was studied as clean-up step, using graphitized black carbon (GBC) and primary secondary amine (PSA). The extract was diluted with water (50:50, v/v) prior to chromatographic analysis. The method was validated and recoveries (except chia samples spiked at 10μg/kg) ranged from 75% to 92%...
March 1, 2017: Food Chemistry
Leonardo Mariño-Repizo, Raquel Gargantini, Humberto Manzano, Julio Raba, Soledad Cerutti
BACKGROUND: The assessment of ochratoxin A (OTA) in wine is relevant for food safety and its continuous control allows to reduce the risk of intake. Thus, a novel sensitive QuEChERS-SPE (Quick, Easy, Cheap, Effective, Rugged, and Safe - Solid Phase Extraction) pretreatment prior to liquid chromatography coupled to tandem mass spectrometry was developed for the determination of OTA in red wine samples from different grape-growing regions in Argentine. RESULTS: A sensitive methodology was achieved, thus limits of detection and quantification were 0...
October 4, 2016: Journal of the Science of Food and Agriculture
Vera Alves, Carlota Conceição, João Gonçalves, Helena M Teixeira, José S Câmara
This paper reports, for the first time, the development of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) combined with a dispersive SPE (d-SPE) based clean-up procedure as a new and powerful strategy for the simultaneous and efficient isolation of two different antidepressants, fluoxetine and clomipramine, and their active metabolites in human urine samples. A univariate experimental design with four independent variables such as sample volume, extraction solvent, buffered salts and clean-up step, was performed and used to investigate the effect of process variables on the extraction efficiency...
September 27, 2016: Journal of Analytical Toxicology
Sisi Zhang, Jiwei Lu, Shaomin Wang, Dan Mao, Shui Miao, Shen Ji
A sensitive and high-throughput method was established and validated for the simultaneous determination of 22 mycotoxins in Pheretima aspergillum (E.Perrier) and Pheretima guillelmi (Michaelsen). A modified Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method was used for sample preparation with recoveries ranging from 73% to 105% with relative standard deviations (RSDs) <8.0% for all target analytes. Ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-MS/MS) was applied for separation and detection in ESI (+) and ESI (-) modes with the limits of detection (LOD) in the range of 0...
November 1, 2016: Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Khaoula Toumi, Christiane Vleminckx, Joris van Loco, Bruno Schiffers
In order to assess the prevalence of pesticide contamination and the risk of florists' exposure when handling cut flowers, sampling and analysis of 90 bouquets of the most commonly sold cut flowers in Belgium (50 bouquets of roses; 20 of gerberas, and 20 of chrysanthemums) were carried out. The bouquets were collected from 50 florists located in the seven largest cities of Belgium (Antwerp, Brussels, Charleroi, Ghent, Leuven, Liege, and Namur) and from five supermarkets located in the different regions. To have a better understanding of the route of exposure and professional practices a questionnaire was also addressed to a group of 25 florists who volunteered to take part in the survey...
2016: International Journal of Environmental Research and Public Health
Tomasz Rejczak, Tomasz Tuzimski
In this study, a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique was adapted to develop a simple sample treatment for multi-residue pesticide analysis in milk samples. The proposed method is based on liquid-liquid partitioning with acetonitrile followed by dispersive solid phase extraction clean-up using primary secondary amine along with zirconia-coated silica particles for extract purification. Identification and quantification of 30 pesticides was conducted via high performance liquid chromatography with diode-array detection (HPLC-DAD)...
February 15, 2017: Food Chemistry
Eleonora Laura De Paola, Giuseppe Montevecchi, Francesca Masino, Davide Garbini, Martino Barbanera, Andrea Antonelli
Acrylamide is a carcinogenic and neurotoxic process contaminant that is generated from food components during heat treatment, while it is absent in raw foodstuffs. Its level in food arouses great concern. A method for acrylamide extraction and determination in dried fruits (dried prunes and raisins) and edible seeds (almonds, hazelnuts, peanuts, pine nuts, pistachios, and walnuts) using a QuEChERS-LC-ESI-MS-Triple Quadrupole approach was set up. Linearity, sensitivity, accuracy, and precision of the method were satisfactory...
February 15, 2017: Food Chemistry
Nannan Pang, Yu Cui, Jiye Hu
A dynamic model of dynamiCROP was applied to study environmental fate and behavior of four herbicides in wheat including florasulam, carfentrazone-ethyl, fluroxypyr-meptyl, and fluroxypyr. Meantime, their residue in wheat and dissipation half-lives in plant determined by field trials using QuEChERS liquid chromatography tandem mass spectrometry were used to verify modelling results. The combination of experimental verification and modelling prediction deciphered the fate of four pesticides in wheat field ecosystem...
December 2016: Chemosphere
De-Gao Wang, Shane R de Solla, Michel Lebeuf, Tommy Bisbicos, Glenn C Barrett, Mehran Alaee
We measured the concentrations of linear and cyclic volatile methylsiloxanes (VMS) concentrations in the blood plasma of turtles, cormorants, and seals collected from Canadian freshwater and marine ecosystems. A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was developed to quantify the levels of linear and cyclic VMS in the plasma samples. The cyclic VMS of hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6) were present in the plasma of all three species...
September 20, 2016: Science of the Total Environment
Peng Wei, Yanan Liu, Wenzhuo Li, Yuan Qian, Yanxia Nie, Dongyeop Kim, Mengcen Wang
Fluopyram, a typical phenylamide fungicide, was widely applied to protect fruit vegetables from fungal pathogens-responsible yield loss. Highly linked to the ecological and dietary risks, its residual and metabolic profiles in the fruit vegetable ecosystem still remained obscure. Here, an approach using modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction combined with GC-MS/MS analysis was developed to investigate fluopyram fate in the typical fruit vegetables including tomato, cucumber, pepper under the greenhouse environment...
2016: Scientific Reports
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