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Capillary liquid chromatography (CLC) with UV-diode array detection has been proposed for the first time to determine fipronil and two metabolites, fipronil-sulfide and fipronil-sulfone in hen egg samples. Under optimum conditions, analytes eluted in less than 12 minutes. Despite the complexity of egg samples, a simple and fast sample preparation method based on salting-out assisted liquid-liquid extraction (SALLE) was developed using acetonitrile as extraction solvent and ammonium sulfate as salting out reagent. To obtain satisfactory extraction efficiencies for the target compounds, several parameters affecting the procedure were optimized, including the nature and amount of the extraction solvent and the type and amount of salting-out reagent, among others. Validation parameters of the proposed SALLE-CLC-UV method yielded satisfactory results with repeatability and intermediate precision, expressed as relative standard deviation (RSD), below 9% and 11%, respectively and recoveries above 80%. Good linearity was obtained (R2>0.990) with limits of detection (LOD) below 5 μg·kg-1. The advantages of a miniaturized technique such as CLC in terms of reduced sample and solvent consumption, combined with simplicity of the SALLE procedure, make this method an attractive green alternative to traditional LC for the monitoring of these residues in egg samples.
M. Mar Aparicio-Muriana; Tereza Jirková; Francisco J. Lara; Ana M. García-Campaña. Simple and efficient method for the determination of fipronil and two main metabolites in eggs by capillary liquid chromatography. Microchemical Journal 2021, 169, 106595 .
AMA StyleM. Mar Aparicio-Muriana, Tereza Jirková, Francisco J. Lara, Ana M. García-Campaña. Simple and efficient method for the determination of fipronil and two main metabolites in eggs by capillary liquid chromatography. Microchemical Journal. 2021; 169 ():106595.
Chicago/Turabian StyleM. Mar Aparicio-Muriana; Tereza Jirková; Francisco J. Lara; Ana M. García-Campaña. 2021. "Simple and efficient method for the determination of fipronil and two main metabolites in eggs by capillary liquid chromatography." Microchemical Journal 169, no. : 106595.
An ultra-high performance liquid chromatography coupled to tandem mass spectrometry method is proposed for the determination of the major ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergokryptine, ergocristine) and their epimers (ergometrinine, ergosinine, ergotaminine, ergocorninine, ergokryptinine, and ergocristinine) in oat-based foods and food supplements. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure was applied as sample treatment, reducing the consumption of organic solvent and increasing sensitivity. This method involved an extraction with acetonitrile and ammonium carbonate (85:15, v/v) and a clean-up step based on dispersive solid-phase extraction, employing a mixture of C18/Z-Sep+ as sorbents. Procedural calibration curves were established and limits of quantification were below 3.2 μg/kg for the studied compounds. Repeatability and intermediate precision (expressed as RSD%) were lower than 6.3% and 15%, respectively, with recoveries ranging between 89.7% and 109%. The method was applied to oat-based products (bran, flakes, flour, grass, hydroalcoholic extracts, juices, and tablets), finding a positive sample of oat bran contaminated with ergometrine, ergosine, ergometrinine, and ergosinine (total content of 10.7 μg/kg).
Laura Carbonell-Rozas; Laura Gámiz-Gracia; Francisco Lara; Ana García-Campaña. Determination of the Main Ergot Alkaloids and Their Epimers in Oat-Based Functional Foods by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry. Molecules 2021, 26, 3717 .
AMA StyleLaura Carbonell-Rozas, Laura Gámiz-Gracia, Francisco Lara, Ana García-Campaña. Determination of the Main Ergot Alkaloids and Their Epimers in Oat-Based Functional Foods by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry. Molecules. 2021; 26 (12):3717.
Chicago/Turabian StyleLaura Carbonell-Rozas; Laura Gámiz-Gracia; Francisco Lara; Ana García-Campaña. 2021. "Determination of the Main Ergot Alkaloids and Their Epimers in Oat-Based Functional Foods by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry." Molecules 26, no. 12: 3717.
The natural occurrence of six major ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers, were investigated in 60 cereal samples (barley and wheat) from Algeria. Ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) and a QuEChERS extraction method were used for sample analysis. The results revealed that 12 out of 60 samples (20%) were contaminated with ergot alkaloids. Wheat was the most contaminated matrix, with an incidence of 26.7% (8 out of 30 samples). The concentration of total ergot alkaloids ranged from 17.8 to 53.9 µg/kg for barley and from 3.66 to 76.0 μg/kg for wheat samples. Ergosine, ergokryptine and ergocristine showed the highest incidences in wheat, while ergometrine was the most common ergot in barley.
Laura Carbonell-Rozas; Choukri Mahdjoubi; Natalia Arroyo-Manzanares; Ana García-Campaña; Laura Gámiz-Gracia. Occurrence of Ergot Alkaloids in Barley and Wheat from Algeria. Toxins 2021, 13, 316 .
AMA StyleLaura Carbonell-Rozas, Choukri Mahdjoubi, Natalia Arroyo-Manzanares, Ana García-Campaña, Laura Gámiz-Gracia. Occurrence of Ergot Alkaloids in Barley and Wheat from Algeria. Toxins. 2021; 13 (5):316.
Chicago/Turabian StyleLaura Carbonell-Rozas; Choukri Mahdjoubi; Natalia Arroyo-Manzanares; Ana García-Campaña; Laura Gámiz-Gracia. 2021. "Occurrence of Ergot Alkaloids in Barley and Wheat from Algeria." Toxins 13, no. 5: 316.
BACKGROUND Ergot alkaloids are secondary metabolites produced by fungi in the genus Claviceps. They contaminate a large variety of cereals, such as rye, triticale, wheat and barley. The ingestion of contaminated cereals might cause adverse health effects in humans and animals. In fact, pigs, cattle, sheep, and poultry are involved in sporadic outbreaks and, although there are several studies about occurrence of ergot alkaloids in grain cereals, there are scarce studies focused on compound feed. RESULTS Twelve ergot alkaloids have been quantified in 228 feed samples intended for swine. The analytes were extracted using QuEChERS with Z‐Sep+ as sorbent in the clean‐up step, which reduced the matrix effect, allowing limits of quantification between 2.1 and 21.7 μg kg–1. The analytes were subsequently quantified by ultra‐high‐performance liquid chromatography with tandem mass spectrometry (UHPLC–MS/MS). A total of 29 samples (12.7%) revealed contamination by at least one ergot alkaloid, and among contaminated samples, 65% were contaminated by more than one. Only 6 of 12 target ergot alkaloids showed concentrations above the limit of quantification. The concentrations for individual ergot alkaloids ranged between 5.9 μg kg–1 for ergosinine to 145.3 μg kg–1 for ergometrine (the predominant ergot alkaloid), while the total ergot alkaloid content ranged from 5.9 to 158.7 μg kg–1. CONCLUSIONS The occurrence of ergot alkaloids in feed samples in Spain seems to be lower than in other regions of Europe. All the samples fulfilled current recommendations of the feed industry about practical limits for ergot alkaloids in pig feeds. This suggests that the feeds are safe for pig consumption, regarding the presence of ergot alkaloids. © 2021 Society of Chemical Industry.
Natalia Arroyo‐Manzanares; Vicente Rodríguez‐Estévez; Ana M García‐Campaña; Elena Castellón‐Rendón; Laura Gámiz‐Gracia. Determination of principal ergot alkaloids in swine feeding. Journal of the Science of Food and Agriculture 2021, 101, 5214 -5224.
AMA StyleNatalia Arroyo‐Manzanares, Vicente Rodríguez‐Estévez, Ana M García‐Campaña, Elena Castellón‐Rendón, Laura Gámiz‐Gracia. Determination of principal ergot alkaloids in swine feeding. Journal of the Science of Food and Agriculture. 2021; 101 (12):5214-5224.
Chicago/Turabian StyleNatalia Arroyo‐Manzanares; Vicente Rodríguez‐Estévez; Ana M García‐Campaña; Elena Castellón‐Rendón; Laura Gámiz‐Gracia. 2021. "Determination of principal ergot alkaloids in swine feeding." Journal of the Science of Food and Agriculture 101, no. 12: 5214-5224.
The Spanish National Network on Mycotoxins and Toxigenic Fungi and their Decontamination Processes (MICOFOOD) held its V Workshop on 10–11 December 2020. The venue was the University of Valencia, although, due to the pandemic situation, most of the participants followed the event online. Over 100 scientists, researchers, and representatives of the industry followed the Workshop, with the aim of discussing the different aspects of mycotoxin research and their impact on human and animal health, including: Study of mycotoxin-producing fungi, toxicology, analytical methods for the determination of mycotoxins, occurrence studies, reduction, and prevention, among others
Laura Gámiz-Gracia; Ana M. García-Campaña. Report of the Vth Workshop of the Spanish National Network on Mycotoxins and Toxigenic Fungi and Their Decontamination Processes (MICOFOOD), 10–11 December 2020. Toxins 2021, 13, 56 .
AMA StyleLaura Gámiz-Gracia, Ana M. García-Campaña. Report of the Vth Workshop of the Spanish National Network on Mycotoxins and Toxigenic Fungi and Their Decontamination Processes (MICOFOOD), 10–11 December 2020. Toxins. 2021; 13 (1):56.
Chicago/Turabian StyleLaura Gámiz-Gracia; Ana M. García-Campaña. 2021. "Report of the Vth Workshop of the Spanish National Network on Mycotoxins and Toxigenic Fungi and Their Decontamination Processes (MICOFOOD), 10–11 December 2020." Toxins 13, no. 1: 56.
The use of allium extract containing propyl propane thiosulfonate (PTSO) as hen feed supplement was evaluated to demonstrate its positive effect on egg production and intestinal microbiota modulation. The study was carried out on 90 laying hens whose feed was supplemented with allium extract for 28 days. Nutritional properties of eggs were not affected, whereas an improvement in productivity was observed based on the increase weight of eggs. In addition, a modulator effect on intestinal microbiota was confirmed by the increase in Lactobacillus spp. and Bifidobacterium spp., as well as by the reduction in Enterobacteriaceae populations. Finally, the preservation of egg composition was checked by monitoring the content of PTSO, using a new analytical method consisting of the use of solid phase extraction and ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Consequently, based on current results, Allium spp. extract rich in organosulfur compounds such as PTSO added to the diet had a beneficial effect on the microbiota and would seem to be a possible alternative to increase productivity, while not affecting the biochemical composition of egg. However, further studies on the effects of allium extract as feed supplement are necessary.
Paloma Abad; Natalia Arroyo-Manzanares; Juan J. Ariza; Alberto Baños; Ana M. García-Campaña. Effect of Allium Extract Supplementation on Egg Quality, Productivity, and Intestinal Microbiota of Laying Hens. Animals 2020, 11, 41 .
AMA StylePaloma Abad, Natalia Arroyo-Manzanares, Juan J. Ariza, Alberto Baños, Ana M. García-Campaña. Effect of Allium Extract Supplementation on Egg Quality, Productivity, and Intestinal Microbiota of Laying Hens. Animals. 2020; 11 (1):41.
Chicago/Turabian StylePaloma Abad; Natalia Arroyo-Manzanares; Juan J. Ariza; Alberto Baños; Ana M. García-Campaña. 2020. "Effect of Allium Extract Supplementation on Egg Quality, Productivity, and Intestinal Microbiota of Laying Hens." Animals 11, no. 1: 41.
A simple and effective method using solid-liquid extraction followed by capillary liquid chromatography with diode array detection (CLC-DAD) has been established for the extraction and determination of seven neonicotinoid insecticides commercially available (imidacloprid, thiacloprid, clothianidin, thiamethoxam, acetamiprid, nitenpyram and dinotefuran) in cereal samples. The separation was achieved in less than 19 min using a Zorbax XDB-C18 column (150 mm x 0.5 mm i.d, 5 µm) at a 25 °C, with a mobile phase consisting of ultrapure water and acetonitrile at a flow rate of 10 µL/min. Detection wavelengths of 254 or 270 nm were used, depending on the analyte. Variables affecting the extraction efficiency were optimized, such as type and volume of extraction solvent, and extraction and centrifugation time. Under the optimal conditions, the proposed method was characterized according to SANTE/12682/2019 guideline, in terms of linearity (R2≥ 0.9901), repeatability (RSD ≤ 7.6%), reproducibility (RSD ≤ 10%) and trueness (recoveries ≥ 80%). The limits of detection and quantification were in the ranges of 3-5 and 9-18 µg/kg, respectively, being adequate for the determination of these compounds in cereal samples at levels below its maximum residue limits (MRLs) established by the European legislation. The advantages of a miniaturized technique such as CLC in terms of high mass sensitivity and reduced solvent consumption, combined with the simplicity of the solid-liquid extraction procedure, make this method a useful alternative for the monitoring of these residues at trace level in cereal samples.
Laura Carbonell-Rozas; Francisco J. Lara; Monsalud Del Olmo Iruela; Ana M. García-Campaña. A novel approach based on capillary liquid chromatography for the simultaneous determination of neonicotinoid residues in cereal samples. Microchemical Journal 2020, 161, 105756 .
AMA StyleLaura Carbonell-Rozas, Francisco J. Lara, Monsalud Del Olmo Iruela, Ana M. García-Campaña. A novel approach based on capillary liquid chromatography for the simultaneous determination of neonicotinoid residues in cereal samples. Microchemical Journal. 2020; 161 ():105756.
Chicago/Turabian StyleLaura Carbonell-Rozas; Francisco J. Lara; Monsalud Del Olmo Iruela; Ana M. García-Campaña. 2020. "A novel approach based on capillary liquid chromatography for the simultaneous determination of neonicotinoid residues in cereal samples." Microchemical Journal 161, no. : 105756.
Mycotoxins are secondary metabolites produced by fungi of different species (mainly Aspergillus, Fusarium, and Penicillium) with toxic effects for humans and animals that can contaminate food and feed
Laura Gámiz-Gracia; Ana M. García-Campaña; Natalia Arroyo-Manzanares. Application of LC–MS/MS in the Mycotoxins Studies. Toxins 2020, 12, 272 .
AMA StyleLaura Gámiz-Gracia, Ana M. García-Campaña, Natalia Arroyo-Manzanares. Application of LC–MS/MS in the Mycotoxins Studies. Toxins. 2020; 12 (4):272.
Chicago/Turabian StyleLaura Gámiz-Gracia; Ana M. García-Campaña; Natalia Arroyo-Manzanares. 2020. "Application of LC–MS/MS in the Mycotoxins Studies." Toxins 12, no. 4: 272.
A survey on 120 cereal samples (barley, maize, rice and wheat) from Algerian markets has been carried out to evaluate the presence of 15 mycotoxins (ochratoxin A, deoxynivalenol, fumonisin B1 and B2, T-2 and HT-2 toxins, zearalenone, fusarenon X, citrinin, sterigmatocystin, enniatins A, A1, B and B1, and beauvericin). With this purpose, a QuEChERS-based extraction and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) were used. Analytical results showed that 78 cereal samples (65%) were contaminated with at least one toxin, while 50% were contaminated with three to nine mycotoxins. T-2 toxin, citrinin, beauvericin and deoxynivalenol were the most commonly found mycotoxins (frequency of 50%, 41.6%, 40.8% and 33.3%, respectively). Fumonisins (B1 + B2), enniatins B and B1, deoxynivalenol and zearalenone registered high concentrations (289–48878 µg/kg, 1.2–5288 µg/kg, 15–4569 µg/kg, 48–2055 µg/kg and 10.4–579 µg/kg, respectively). Furthermore, concentrations higher than those allowed by the European Union (EU) were observed in 21, 8 and 1 samples for fumonisins, zearalenone and deoxinivalenol, respectively. As a conclusion, the high levels of fumonisins (B1 + B2) in maize and deoxynivalenol, zearalenone and HT-2 + T-2 toxins in wheat, represent a health risk for the average adult consumer in Algeria. These results pointed out the necessity of a consistent control and the definition of maximum allowed levels for mycotoxins in Algerian foodstuffs.
Choukri Khelifa Mahdjoubi; Natalia Arroyo-Manzanares; Nisserine Hamini-Kadar; Ana M. García-Campaña; Kihel Mebrouk; Laura Gámiz-Gracia. Multi-Mycotoxin Occurrence and Exposure Assessment Approach in Foodstuffs from Algeria. Toxins 2020, 12, 194 .
AMA StyleChoukri Khelifa Mahdjoubi, Natalia Arroyo-Manzanares, Nisserine Hamini-Kadar, Ana M. García-Campaña, Kihel Mebrouk, Laura Gámiz-Gracia. Multi-Mycotoxin Occurrence and Exposure Assessment Approach in Foodstuffs from Algeria. Toxins. 2020; 12 (3):194.
Chicago/Turabian StyleChoukri Khelifa Mahdjoubi; Natalia Arroyo-Manzanares; Nisserine Hamini-Kadar; Ana M. García-Campaña; Kihel Mebrouk; Laura Gámiz-Gracia. 2020. "Multi-Mycotoxin Occurrence and Exposure Assessment Approach in Foodstuffs from Algeria." Toxins 12, no. 3: 194.
This work proposes a novel Quick, Easy, Cheap, Effective, Rugged, y Safe (QuEChERS) method in combination with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of sulfonylurea residues in edible seeds. The chromatographic separation of nine sulfonylureas was accomplished in less than 5.5 min, using a Luna Omega C18 column (50 × 2.1 mm, 1.6 µm). Mobile phase was supplied at 0.55 mL/min and consisted of 0.01% (v/v) aqueous acetic acid as eluent A and a mixture methanol/acetonitrile (80/20, v/v) as eluent B. Column temperature was established at 25°C. A QuEChERS procedure was investigated as sample treatment for sulfonylureas extraction and sample clean-up. Different clean-up agents (i.e. PSA, Z-Sep+, EMR-Lipid and C18) were evaluated, selecting Z-Sep+ (25 mg) as the best option. The proposed method provided an extraction efficiency greater than 86.2%, while absolute matrix effect was lower than 50.1%. Matrix-matched calibration curves were required for analyte quantification. The analytical method was characterized according to SANTE/11813/2017 guideline, and including limits of detection and quantification, precision, and trueness. Linear dynamic ranges were established from 5 to 150 µg/kg for all analytes. Linearity (R2 ≥ 0.9974) and precision in terms of repeatability and intermediate precision (relative standard deviation ≤ 14.7%) are reported. The reporting limit was established at 5 µg kg−1, which is above the limits of quantification of the proposed method (≤ 1.64 µg kg−1) and below the maximum residue levels currently established by European legislation. In general, trueness is within the range of 70-120%. Despite greater recoveries were obtained at the reporting limit (i.e. 120-138%), relative standard deviations lower than 20% were obtained at this concentration level, so fulfilling the requirements of SANTE/11813/2017 guideline. This work represents the first analytical method intended for the analysis of sulfonylureas in sunflower, pumpkin and chia seeds, which are complex matrices due to their high content of fat as well as of growing interest due to their current commercialization as nutraceuticals.
Maykel Hernández-Mesa; Ana M. García-Campaña. Determination of sulfonylurea pesticide residues in edible seeds used as nutraceuticals by QuEChERS in combination with ultra-high-performance liquid chromatography-tandem mass spectrometry. Journal of Chromatography A 2019, 1617, 460831 .
AMA StyleMaykel Hernández-Mesa, Ana M. García-Campaña. Determination of sulfonylurea pesticide residues in edible seeds used as nutraceuticals by QuEChERS in combination with ultra-high-performance liquid chromatography-tandem mass spectrometry. Journal of Chromatography A. 2019; 1617 ():460831.
Chicago/Turabian StyleMaykel Hernández-Mesa; Ana M. García-Campaña. 2019. "Determination of sulfonylurea pesticide residues in edible seeds used as nutraceuticals by QuEChERS in combination with ultra-high-performance liquid chromatography-tandem mass spectrometry." Journal of Chromatography A 1617, no. : 460831.
A simple, sensitive, and efficient method has been developed for the determination of the seven neonicotinoid insecticides commercially available (imidacloprid, thiacloprid, clothianidin, thiamethoxam, acetamiprid, nitenpyram, and dinotefuran) and the main metabolite 6-chloronicotinic acid. Micellar electrokinetic chromatography (MEKC) mode was applied, using 48.5 cm of total length capillary (50 μm i.d.) with an extended light-path capillary (150 μm). The running electrolyte consisted of 25 mM sodium tetraborate buffer (pH 9.2) containing 120 mM of sodium dodecyl sulfate and 15% of methanol (v/v). A voltage of 27 kV and a temperature of 25 °C were applied. Samples dissolved in deionized water were hydrodynamically injected at 50 mbar for 12 s, achieving the analysis in less than 12 min. Diode array detection (DAD) was performed at 220, 254, and 270 nm, depending on the analyte. Two different methodologies as sample treatments were developed; for water samples, solid-phase extraction was checked using different cartridges (C18, Oasis® HLB, Oasis® HLB Prime, and Strata-X), being the best option Oasis® HLB for preconcentration and cleanup. In the case of soil samples, a simple solid–liquid extraction was applied using a mixture of 1:3 (v/v) acetonitrile/dichloromethane. Satisfactory linearity, trueness, and precision were achieved, with detection limits in the range of 0.1–0.4 μg L−1 for river water and 1.0–2.9 μg kg−1 for soil samples. Recoveries in the range of 80–107% for all of the assayed neonicotinoids in water samples of different origin and 73–92% for soil samples were achieved.
Laura Carbonell-Rozas; Francisco J. Lara; Monsalud Del Olmo Iruela; Ana M. García-Campaña. Micellar electrokinetic chromatography as efficient alternative for the multiresidue determination of seven neonicotinoids and 6-chloronicotinic acid in environmental samples. Analytical and Bioanalytical Chemistry 2019, 412, 6231 -6240.
AMA StyleLaura Carbonell-Rozas, Francisco J. Lara, Monsalud Del Olmo Iruela, Ana M. García-Campaña. Micellar electrokinetic chromatography as efficient alternative for the multiresidue determination of seven neonicotinoids and 6-chloronicotinic acid in environmental samples. Analytical and Bioanalytical Chemistry. 2019; 412 (24):6231-6240.
Chicago/Turabian StyleLaura Carbonell-Rozas; Francisco J. Lara; Monsalud Del Olmo Iruela; Ana M. García-Campaña. 2019. "Micellar electrokinetic chromatography as efficient alternative for the multiresidue determination of seven neonicotinoids and 6-chloronicotinic acid in environmental samples." Analytical and Bioanalytical Chemistry 412, no. 24: 6231-6240.
In this study two different analytical approaches have been developed to determine the presence of several cyanotoxins in saline water samples from a continental salt marsh. A salting-out assisted liquid-liquid extraction (SALLE) has been used in combination with ultra-high performance liquid chromatography-tandem mass spectrometry and UV-diode array detection (UHPLC-MS/MS and UHPLC-DAD). The target analytes are eight microcystins named MC-RR, MC-YR, MC-LR, MC-WR, MC-LA, MC-LY, MC-LW, MC-LF and nodularin (NOD), covering a wide range of polarities. The separation was achieved using a Zorbax Eclipse Plus RRHD C18 column (50 × 2.1 mm, 1.8 μm) in less than 7.5 and 5.5 min for UV and MS/MS detection, respectively. The mobile phase used consisted of water (solvent A) and acetonitrile (MeCN) (solvent B), both containing 0.01% of formic acid for DAD and 0.4% of formic acid for MS/MS detection, at a flow rate of 0.4 mL min-1. The temperature of the column was set at 25 °C and 20 μL of sample were injected. The main parameters affecting the SALLE procedure were studied and the following optimum values were obtained: neutral pH, 2 mL of acetonitrile as extraction solvent and 1.2 g of ammonium sulfate as salting-out agent for 4 mL of water sample. The validation protocols for both methods were accomplished with real water samples obtaining LODs ranging from 1.0 to 3.4 μg L-1 and 0.02 to 0.11 μg L-1 for DAD and MS/MS respectively. Although the SALLE-UHPLC-DAD methodology is easier and cheaper than UHPLC-MS/MS significantly better detection limits were achieved with tandem mass spectrometry as well as allowing for unambiguous identification. Extraction recoveries were higher than 77.0% (except for MC-RR and NOD which were 53.2% and 54.3, respectively) with satisfactory inter-day and intra-day precisions (RSD below 13.3%).
Maryam Hemmati; Carmen Tejada-Casado; Francisco J. Lara; Ana M. García-Campaña; Maryam Rajabi; Monsalud del Olmo-Iruela. Monitoring of cyanotoxins in water from hypersaline microalgae colonies by ultra high performance liquid chromatography with diode array and tandem mass spectrometry detection following salting-out liquid-liquid extraction. Journal of Chromatography A 2019, 1608, 460409 .
AMA StyleMaryam Hemmati, Carmen Tejada-Casado, Francisco J. Lara, Ana M. García-Campaña, Maryam Rajabi, Monsalud del Olmo-Iruela. Monitoring of cyanotoxins in water from hypersaline microalgae colonies by ultra high performance liquid chromatography with diode array and tandem mass spectrometry detection following salting-out liquid-liquid extraction. Journal of Chromatography A. 2019; 1608 ():460409.
Chicago/Turabian StyleMaryam Hemmati; Carmen Tejada-Casado; Francisco J. Lara; Ana M. García-Campaña; Maryam Rajabi; Monsalud del Olmo-Iruela. 2019. "Monitoring of cyanotoxins in water from hypersaline microalgae colonies by ultra high performance liquid chromatography with diode array and tandem mass spectrometry detection following salting-out liquid-liquid extraction." Journal of Chromatography A 1608, no. : 460409.
Mycotoxins have become one of the most common contaminants reported worldwide. Current legislation has established maximum levels only for some well-known mycotoxins; however, there are many other “emerging mycotoxins” for which there is no regulation, as enniatins and beauvericin. An analytical method based on salting-out assisted liquid-liquid extraction followed by ultra-high performance liquid chromatography tandem mass spectrometry is proposed for determination of enniatin A, A1, B, B1, and beauvericin in different plant-based milks, as a possible source of these contaminants, is proposed. The method showed good precision and trueness (RSD <8% and recoveries between 84-97%) with a moderate matrix effect. From a total of 32 samples of plant-based milks of different compositions (including 8 rice milks, 8 oat milks and 16 soy milks), 3 samples were contaminated with the five mycotoxins, while 5 samples were contaminated with four of them, being oat milk the most susceptible for contamination.
Natalia Arroyo-Manzanares; Ahmed M. Hamed; Ana M. García-Campaña; Laura Gámiz-Gracia. Plant-based milks: unexplored source of emerging mycotoxins. A proposal for the control of enniatins and beauvericin using UHPLC-MS/MS. Food Additives & Contaminants: Part B 2019, 12, 296 -302.
AMA StyleNatalia Arroyo-Manzanares, Ahmed M. Hamed, Ana M. García-Campaña, Laura Gámiz-Gracia. Plant-based milks: unexplored source of emerging mycotoxins. A proposal for the control of enniatins and beauvericin using UHPLC-MS/MS. Food Additives & Contaminants: Part B. 2019; 12 (4):296-302.
Chicago/Turabian StyleNatalia Arroyo-Manzanares; Ahmed M. Hamed; Ana M. García-Campaña; Laura Gámiz-Gracia. 2019. "Plant-based milks: unexplored source of emerging mycotoxins. A proposal for the control of enniatins and beauvericin using UHPLC-MS/MS." Food Additives & Contaminants: Part B 12, no. 4: 296-302.
In the last decade, ion mobility spectrometry (IMS) has reemerged as an analytical separation technique, especially due to the commercialization of ion mobility mass spectrometers. Its applicability has been extended beyond classical applications such as the determination of chemical warfare agents and nowadays it is widely used for the characterization of biomolecules (e.g., proteins, glycans, lipids, etc.) and, more recently, of small molecules (e.g., metabolites, xenobiotics, etc.). Following this trend, the interest in this technique is growing among researchers from different fields including food science. Several advantages are attributed to IMS when integrated in traditional liquid chromatography (LC) and gas chromatography (GC) mass spectrometry (MS) workflows: (1) it improves method selectivity by providing an additional separation dimension that allows the separation of isobaric and isomeric compounds; (2) it increases method sensitivity by isolating the compounds of interest from background noise; (3) and it provides complementary information to mass spectra and retention time, the so-called collision cross section (CCS), so compounds can be identified with more confidence, either in targeted or non-targeted approaches. In this context, the number of applications focused on food analysis has increased exponentially in the last few years. This review provides an overview of the current status of IMS technology and its applicability in different areas of food analysis (i.e., food composition, process control, authentication, adulteration and safety).
Maykel Hernández-Mesa; David Ropartz; Ana M. García-Campaña; Hélène Rogniaux; Gaud Dervilly-Pinel; Bruno Le Bizec. Ion Mobility Spectrometry in Food Analysis: Principles, Current Applications and Future Trends. Molecules 2019, 24, 2706 .
AMA StyleMaykel Hernández-Mesa, David Ropartz, Ana M. García-Campaña, Hélène Rogniaux, Gaud Dervilly-Pinel, Bruno Le Bizec. Ion Mobility Spectrometry in Food Analysis: Principles, Current Applications and Future Trends. Molecules. 2019; 24 (15):2706.
Chicago/Turabian StyleMaykel Hernández-Mesa; David Ropartz; Ana M. García-Campaña; Hélène Rogniaux; Gaud Dervilly-Pinel; Bruno Le Bizec. 2019. "Ion Mobility Spectrometry in Food Analysis: Principles, Current Applications and Future Trends." Molecules 24, no. 15: 2706.
A survey including 228 pig feed samples from Spain has been developed, exploring the occurrence of 19 mycotoxins (aflatoxins B1, B2, G1 and G2, ochratoxin A, fumonisins B1 and B2, citrinin, zearalenone, deoxynivalenol, fusarenon X, sterigmatocystin, T-2 toxin, HT-2 toxin, enniatins A, A1, B and B2, and beauvericin). The samples were analysed by solid-liquid extraction followed by liquid chromatography coupled with fluorescence or mass spectrometry detection. Enniatin B was found in 100% of the samples (up to 1200 µg/kg) and beauvericin in more than 90%. Moreover, 40% of samples were contaminated with more than five mycotoxins. This high occurrence is insurmountable and surpasses all previous studies, probably due to the inclusion of emerging mycotoxins, scarcely explored. The majority of the samples (96.9%) were in accordance with EU regulations, which do not address emerging mycotoxins or co-occurrence. These results show that in order to ensure mycotoxin absence, emerging mycotoxins should always be considered.
Natalia Arroyo-Manzanares; Vicente Rodríguez-Estévez; Plácido Arenas-Fernández; Ana M. García-Campaña; Laura Gámiz-Gracia. Occurrence of Mycotoxins in Swine Feeding from Spain. Toxins 2019, 11, 342 .
AMA StyleNatalia Arroyo-Manzanares, Vicente Rodríguez-Estévez, Plácido Arenas-Fernández, Ana M. García-Campaña, Laura Gámiz-Gracia. Occurrence of Mycotoxins in Swine Feeding from Spain. Toxins. 2019; 11 (6):342.
Chicago/Turabian StyleNatalia Arroyo-Manzanares; Vicente Rodríguez-Estévez; Plácido Arenas-Fernández; Ana M. García-Campaña; Laura Gámiz-Gracia. 2019. "Occurrence of Mycotoxins in Swine Feeding from Spain." Toxins 11, no. 6: 342.
This paper evaluates the bioavailability of allium derivative propyl propane thiosulfonate (PTSO) in the pig gastrointestinal tract by means of an in vitro dynamic gastrointestinal tract simulator system (GITSS). The GITSS is based on a membrane bioreactor comprising a continuous stirred-tank reactor connected in series to a continuous plug-flow tubular reactor. Bioavailability values have been evaluated for different vehiculization strategies, including mere carriers such as polyethylene glycol sorbitan monooleate (a nonionic surfactant also known as Tween 80) and encapsulation matrices (β-cyclodextrin vs. mono- and di-glycerides of edible fatty acids mixed with hydrogenated sunflower oil) and compared with the absorption of free PTSO. The net absorbed amount of PTSO in the GITSS when Tween 80 was used as a carrier was over 3.5 times higher than the one for free PTSO. Neither the encapsulated PTSO in β-cyclodextrin nor by means of mono- and di-glycerides of fatty acids plus a vegetable oil succeeded to improve absorption values for free PTSO. These promising results indicate that Tween 80 provides an interesting and high resistance to the PTSO molecule against the simulated digestive conditions in the stomach, and thus it enables favorably the subsequent absorption process of PTSO along the intestine.
Paloma Abad; Natalia Arroyo-Manzanares; Ernesto Rivas-Montoya; Javier M. Ochando-Pulido; Enrique Guillamon; Ana M. Garcia-Campaña; Antonio Martinez-Ferez. Effects of different vehiculization strategies for the allium derivative propyl propane thiosulfonate during dynamic simulation of the pig gastrointestinal tract. Canadian Journal of Animal Science 2019, 99, 244 -253.
AMA StylePaloma Abad, Natalia Arroyo-Manzanares, Ernesto Rivas-Montoya, Javier M. Ochando-Pulido, Enrique Guillamon, Ana M. Garcia-Campaña, Antonio Martinez-Ferez. Effects of different vehiculization strategies for the allium derivative propyl propane thiosulfonate during dynamic simulation of the pig gastrointestinal tract. Canadian Journal of Animal Science. 2019; 99 (2):244-253.
Chicago/Turabian StylePaloma Abad; Natalia Arroyo-Manzanares; Ernesto Rivas-Montoya; Javier M. Ochando-Pulido; Enrique Guillamon; Ana M. Garcia-Campaña; Antonio Martinez-Ferez. 2019. "Effects of different vehiculization strategies for the allium derivative propyl propane thiosulfonate during dynamic simulation of the pig gastrointestinal tract." Canadian Journal of Animal Science 99, no. 2: 244-253.
In the context of human and veterinary drugs identification, ion mobility spectrometry (IMS) in combination with mass spectrometry (MS) may provide a relevant complementary piece of information to mass-to-charge ratio (m/z), the so-called collision-cross-section (CCS). Up to now, however, the application of CCS as identification parameter has not been fully investigated due to the reduced number of these drugs that have being characterized in terms of CCS. This work proposes a CCS database for 92 human and veterinary drugs, including eighteen benzimidazoles, eleven 5-nitroimidazoles, eleven aminoglycosides, nineteen quinolones, eighteen β-lactams, ten sulfonamides and five tetracyclines. Among them, 37 drugs have been characterized in terms of CCS for the first time. The CCS values of the other 55 compounds have been compared with those from a recently published database in order to evaluate inter-laboratory reproducibility, which is crucial for the implementation of the CCS as identification parameter. CCS values were measured by traveling wave ion mobility spectrometry (TWIMS) under positive ionization conditions. Nitrogen was used as drift gas in the ion mobility cell. The proposed database covers 173 ions including [M+H]+ and [M+Na]+ species. High correlation between m/z and CCS has been observed for [M+H]+ (R2 = 0.9518, n = 91) and [M+Na]+ (R2 = 0.9135, n = 82) ions. As expected, CCS values for sodium adducts are generally greater than for protonated molecules because they exhibit higher molecular weight. However, sodium adducts of aminoglycosides, β-lactams, and of several quinolones and benzimidazoles, were characterized as more compact ions than their related protonated molecule. In addition, this work describes the fragmentation pattern observed for the studied molecules. For the first time, the main fragment ions for most of the compounds have also been characterized in terms of CCS, involving a total of 238 ions. As proof of concept, for the application of this database to biological matrices, eleven veterinary drugs in bovine urine samples were characterized in terms of CCS, showing that this parameter was not influenced by the matrix.
Carmen Tejada-Casado; Maykel Hernández-Mesa; Fabrice Monteau; Francisco J. Lara; Monsalud del Olmo-Iruela; Ana M. García-Campaña; Bruno Le Bizec; Gaud Dervilly-Pinel. Collision cross section (CCS) as a complementary parameter to characterize human and veterinary drugs. Analytica Chimica Acta 2018, 1043, 52 -63.
AMA StyleCarmen Tejada-Casado, Maykel Hernández-Mesa, Fabrice Monteau, Francisco J. Lara, Monsalud del Olmo-Iruela, Ana M. García-Campaña, Bruno Le Bizec, Gaud Dervilly-Pinel. Collision cross section (CCS) as a complementary parameter to characterize human and veterinary drugs. Analytica Chimica Acta. 2018; 1043 ():52-63.
Chicago/Turabian StyleCarmen Tejada-Casado; Maykel Hernández-Mesa; Fabrice Monteau; Francisco J. Lara; Monsalud del Olmo-Iruela; Ana M. García-Campaña; Bruno Le Bizec; Gaud Dervilly-Pinel. 2018. "Collision cross section (CCS) as a complementary parameter to characterize human and veterinary drugs." Analytica Chimica Acta 1043, no. : 52-63.
A green and simple multiresidue method using capillary liquid chromatography (CLC) with UV-diode array detection (DAD) has been developed for the determination of sixteen benzimidazoles (BZs) and its metabolites in milk samples. The separation was achieved in 0.9985 for all BZs) with limits of detection (LOD) between 1.0 and 2.8 μg kg−1. Relative standard deviations of repeatability and intermediate precision were below 1.6 and 14.2%, respectively. Satisfactory recoveries between 79.1 and 99.6% were also obtained for three types of milk samples (cow, sheep and goat). The advantages of a miniaturized technique such as CLC in terms of better efficiencies and reduced solvent consumption, combined with the simplicity of the SALLE procedure, make this method a useful alternative for the monitoring of these residues at trace level.
Carmen Tejada-Casado; Monsalud del Olmo-Iruela; Ana M. García-Campaña; Francisco J. Lara. Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography. Journal of Chromatography B 2018, 1091, 46 -52.
AMA StyleCarmen Tejada-Casado, Monsalud del Olmo-Iruela, Ana M. García-Campaña, Francisco J. Lara. Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography. Journal of Chromatography B. 2018; 1091 ():46-52.
Chicago/Turabian StyleCarmen Tejada-Casado; Monsalud del Olmo-Iruela; Ana M. García-Campaña; Francisco J. Lara. 2018. "Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography." Journal of Chromatography B 1091, no. : 46-52.
QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology in combination with UHPLC–MS/MS is proposed for the determination of 5-nitroimidazole (5-NDZ) residues in infant milk-based products. Chromatographic separation was accomplished in a C18 Zorbax Eclipse Plus RRHD (50 × 2.1 mm, 1.8 μm) column under gradient elution conditions. Mobile phase consisted of 0.025% (v/v) aqueous formic acid (eluent A) and MeOH (eluent B), and was supplied at a flow rate of 0.5 mL/min. Under these conditions, eleven 5-NDZs including three metabolites were separated in less than 4 min. A novel QuEChERS method was optimized, and primary-secondary amine (PSA) sorbent was selected as clean-up agent. In addition, the proposed QuEChERS procedure was compared with other sample preparation methodologies, which are usually used in the analysis of 5-NDZs, namely solid phase extraction (SPE) using mixed cation exchange (MCX) cartridges and molecularly imprinted solid phase extraction (MISPE). Method comparison was carried out in terms of process efficiency, which includes matrix effect and extraction recovery. Higher process efficiency was generally achieved for QuEChERS and MISPE than for SPE. However, matrix effect was more significant for the non-selective QuEChERS method than for the selective MISPE. Higher extraction recoveries (63.2–94.1%) were observed for QuEChERS. The studied methods were validated in terms of linearity, detection limits (CCα), detection capabilities (CCβ) and precision, observing similar performance characteristics independently of the proposed sample treatment. CCα and CCβ ranged between 0.05 and 1.69 μg/L for all analytes and extraction techniques. QuEChERS-UHPLC–MS/MS method was also validated in terms of precision (relative standard deviations < 10.3%), trueness (recovery > 70.2%) and selectivity according to Regulation 2002/657/EC. It is proposed as a good alternative for the monitoring of 5-NDZ residues in enriched infant-milk based products and other similar milk based-products.
Maykel Hernández-Mesa; Ana M. García-Campaña; Carmen Cruces-Blanco. Development and validation of a QuEChERS method for the analysis of 5-nitroimidazole traces in infant milk-based samples by ultra-high performance liquid chromatography-tandem mass spectrometry. Journal of Chromatography A 2018, 1562, 36 -46.
AMA StyleMaykel Hernández-Mesa, Ana M. García-Campaña, Carmen Cruces-Blanco. Development and validation of a QuEChERS method for the analysis of 5-nitroimidazole traces in infant milk-based samples by ultra-high performance liquid chromatography-tandem mass spectrometry. Journal of Chromatography A. 2018; 1562 ():36-46.
Chicago/Turabian StyleMaykel Hernández-Mesa; Ana M. García-Campaña; Carmen Cruces-Blanco. 2018. "Development and validation of a QuEChERS method for the analysis of 5-nitroimidazole traces in infant milk-based samples by ultra-high performance liquid chromatography-tandem mass spectrometry." Journal of Chromatography A 1562, no. : 36-46.
In this article capillary electrophoresis (CE) is presented as a well-established separation technique, applied in food analysis because of its advantages related with the high separation efficiency, short analysis time and low cost. Its applications in the field of food analysis cover the determination of major compounds such as proteins, carbohydrates, lipids or bioactive substances, as well as the control of relevant contaminants, such as natural toxins or residues of pesticides or veterinary drugs, among others. In this contribution, general strategies to face the analysis of these compounds, considering the nature of the analyzed compounds, the different CE modes, the coupled detection techniques and the samples treatments, are summarized.
Maykel Hernández-Mesa; David Moreno-González; Francisco J. Lara; Ana M. García-Campaña. Capillary Electrophoresis | Food Chemistry Applications. Reference Module in Chemistry, Molecular Sciences and Chemical Engineering 2018, 1 .
AMA StyleMaykel Hernández-Mesa, David Moreno-González, Francisco J. Lara, Ana M. García-Campaña. Capillary Electrophoresis | Food Chemistry Applications. Reference Module in Chemistry, Molecular Sciences and Chemical Engineering. 2018; ():1.
Chicago/Turabian StyleMaykel Hernández-Mesa; David Moreno-González; Francisco J. Lara; Ana M. García-Campaña. 2018. "Capillary Electrophoresis | Food Chemistry Applications." Reference Module in Chemistry, Molecular Sciences and Chemical Engineering , no. : 1.