Simultaneous screening and quantification of aminoglycoside antibiotics in honey using mixed-mode liquid chromatography with quadrupole time-of-flight mass spectroscopy with heated electrospray ionization

An analytical method based on liquid chromatography with quadrupole time-of-flight mass spectrometry has been developed for the simultaneous determination of six aminoglycoside antibiotics in honey. The sample pretreatment included extraction with aqueous trichloroacetic acid followed by solid-phase extraction on Strata-X polymeric reversed phase cartridges. Liquid chromatography separation was performed on an Obelisc R zwitterionic type mixed-mode column. An ionBooster™ heated electrospray source was used and showed enhanced ionization efficiency in comparison to a conventional electrospray source. The observed signal enhancement ranged from 3- (neomycin) to 16-fold (gentamicin C1). A data…

Mycotoxins in herbal teas marketed in Latvia and dietary exposure assessment

The occurrence of 12 mycotoxins has been analysed by liquid chromatography - time of flight mass spectrometry in the batch of 60 herbal teas purchased from drugstores in Latvia. Among the dry tea samples, 90% were positive for one to eight mycotoxins. Enniatin B and deoxynivalenol (DON) were the most frequently detected mycotoxins in 55% and 45% of the samples, respectively. DON reached the highest level, from 129 µg kg-1 in herbal blend to 5,463 µg kg-1 in wormwood tea. Ochratoxin A (OTA) and aflatoxin B1 (AFB1) were found in 10% and 20% of the samples at the concentrations ranged between 2.99-30.3 µg kg-1 and 3.40-23.7 µg kg-1. Studies of the tea infusion process indicated that 32-100% of…

A reliable screening of mycotoxins and pesticide residues in paprika using ultra-high performance liquid chromatography coupled to high resolution Orbitrap mass spectrometry

Abstract In this study, an ultra-high performance liquid chromatography (UHPLC) coupled to a high resolution Orbitrap mass spectrometry (Orbitrap-HRMS) was demonstrated as a promising technique in high-throughput method development for the routine analysis and contamination control of mycotoxins and pesticide residues in spices. The method was applied for the analysis of fifty ground paprika samples containing blends of sweet and hot paprika harvested in Brazil and China. The efficiency and detection sensitivity of the used UHPLC-Orbitrap-HRMS technique were compared to the results obtained using a triple quadrupole tandem mass spectrometric detector (UHPLC-QqQ-MS/MS). The values of recover…

Effect of lactic acid fermentation of lupine wholemeal on acrylamide content and quality characteristics of wheat-lupine bread

The effect of supplementing wheat flour at a level of 15% with lupine (Lupinus angustifolius L.) wholemeal fermented by different lactic acid bacteria on acrylamide content in bread crumb as well as on bread texture and sensory characteristics was analysed. The use of fermented lupine resulted in a lower specific volume and crumb porosity of bread on an average by 14.1% and 10.5%, respectively, while untreated lupine lowered the latter parameters at a higher level (30.8% and 20.7%, respectively). The addition of lupine resulted in a higher by 43.3% acrylamide content compared to wheat bread (19.4 µg/kg dry weight (d.w.)). Results showed that acrylamide was significantly reduced using proteo…

Recent applications of carbonaceous nanosorbents for the analysis of mycotoxins in food by liquid chromatography: a short review

Carbonaceous nanomaterials (multi-walled carbon nanotubes (MWCNTs), graphene, and graphene oxide (GO)) have attracted attention over the last decade as adsorbents suitable for the analysis of organic and inorganic pollutants. In the present paper we review methods of mycotoxin analysis that involve sample extraction with carbonaceous nanosorbents, reported from 2011 onwards. Recent studies have highlighted the advantages of magnetically modified MWCNTs and GO in mycotoxin analysis, which may enable sample isolation through magnetic separation, reduce the interaction of nanoparticles, and enhance the recovery of analytes. The papers covered in this review point to promising applications of …

The application of phospholipid removal columns and ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry for quantification of multi-class antibiotics in aquaculture samples.

In this study a robust and sensitive method based on a proposed sample purification procedure, using zirconia-coated Phree™ columns and analysis by ultra-high performance liquid chromatography with triple quadrupole tandem mass spectrometry are presented for the assessment of multi-class antibiotics in farmed fish species. The sample preparation procedure benefited from combined precipitation of proteins and selective removal of phospholipids by Phree™ columns, resulting in a high sensitivity of the method (LOQ 0.3-9mgkg(-1)). The in-house validation results (precision, repeatability, decision limit CCα, detection capability CCβ, etc.) indicate that the elaborated method is fully suitable f…

Effect of fermented Helianthus tuberosus L. tubers on acrylamide formation and quality properties of wheat bread

Abstract The main focus in this study was to investigate the effects on wheat bread safety and quality due to addition of Helianthus tuberosus L. (JA) tubers, fermented by different lactic acid bacteria (LAB) strains (Pediococcus acidilactici KTU05-7, Pediococcus pentosaceus KTU05-8, P. pentosaceus KTU05-9, Lactobacillus sakei KTU05-6, P. pentosaceus KTU05-10). We found experimentally that JA tubers fermented with LAB contained more L(+) than D(−) lactic acid, which resulted in safer products than by spontaneous treatment. The concentrations of biogenic amines in all analysed fermented JA products were far below levels causing a health risk, while the products fermented with LAB contained l…

LC-MS/MS characterisation and determination of dansyl chloride derivatised glyphosate, aminomethylphosphonic acid (AMPA), and glufosinate in foods of plant and animal origin.

Abstract Glyphosate and other polar and acidic pesticides have been particularly studied due to the concerns over widespread and intensive use. The chemical properties of these compounds necessitate use of customised methods, such as derivatisation or ion exchange chromatography. These approaches present a compatibility problem with ESI-MS due to presence of salts and non-volatile compounds. For that reason, a simple procedure has been developed for the extraction, pre-column derivatisation with dansyl chloride (5-(dimethylamino)naphthalene-1-sulfonyl chloride), and mass spectrometric detection of glyphosate, AMPA, and glufosinate after the separation on a C18 stationary phase. The dansyl d…

Ultra high performance liquid chromatography-time-of-flight high resolution mass spectrometry in the analysis of hexabromocyclododecane diastereomers: method development and comparative evaluation versus ultra high performance liquid chromatography coupled to Orbitrap high resolution mass spectrometry and triple quadrupole tandem mass spectrometry.

An efficient ultra high performance liquid chromatography (UHPLC)-time-of-flight high resolution mass spectrometry (TOF-HRMS) method was elaborated for the determination of hexabromocyclododecane (HBCD) diastereomers in fish samples and compared against UHPLC-Orbitrap-HRMS and UHPLC-triple quadrupole (QqQ) tandem MS (MS/MS) techniques. The TOF-HRMS analyzer was operated at high resolution (>10000 full width at half maximum (FWHM)) with scanning the m/z range from 600 to 700, to achieve picogram quantitation limits. The effects of various operational parameters on the instrumental response were systematically investigated. Evaluation of the influence of sample clean-up procedure steps on sig…

Improved sensitivity of ochratoxin A analysis in coffee using high-performance liquid chromatography with hybrid triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS)

A novel and sensitive method utilising high-performance liquid chromatography coupled to triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS) was developed in order to analyse the content of ochratoxin A (OTA) in coffee samples. The introduction of the triple-stage MS scanning mode (MS(3)) has been shown to increase greatly sensitivity and selectivity by eliminating the high chromatographic baseline caused by interference of complex coffee matrices. The analysis included the sample preparation procedure involving extraction of OTA using a methanol-water mixture and clean-up by immunoaffinity columns and detection using the MS(3) scanning mode of LC-QqQLIT-MS/MS. The propose…

Effect of heating method on the microbial levels and acrylamide in corn grits and subsequent use as functional ingredient for bread making

Abstract Cereal by-products represent abundant and low-cost resources of nutrients. The study is dedicated to the development of a rapid method for the treatment of corn grits to obtain value added ingredients for breadmaking. The infrared irradiation (IR) at 76 °C and 90 °C and vacuum microwave (VM) heating at 60 °C have been applied for stabilization of corn grits. The corn grit particles were fractionated by size and it was found that the particle size fraction significantly (p

Benzofenona difūzija no papīra un kartona iepakojuma uz pārtiku

Šajā darbā ir pētīta benzofenona difūzija no iepakojuma uz pārtiku. Tika izstrādāta un pārbaudīta metode benzofenona satura noteikšanai papīra un kartona iepakojumos ar AEŠH-MS-MS. Tika veikti pētījumi par benzofenona ekstrakcijas efektivitāti atkarībā no iepakojuma krāsas, laika, temperatūras un šķīdinātāja.

Parameters of rye, wheat, barley, and oat sourdoughs fermented withLactobacillus plantarumLUHS135 that influence the quality of mixed rye-wheat bread, including acrylamide formation

A Lactobacillus plantarum strain was used for the production of rye, wheat, barley, and oat sourdoughs, and the influence of different sourdoughs on mixed rye–wheat bread quality parameters and acrylamide formation was evaluated. L. plantarum LUHS135 demonstrated versatile carbohydrate metabolism, good growth and acidification rates, and the ability to excrete amylolytic and proteolytic enzymes in various cereal sourdoughs. The same starter and different cereal substrates allow to produce sourdoughs showing different characteristics. The type of sourdough and its quantity had significant influence on acrylamide content in bread (P ≤ 0.0001), and using 5% or 10% of wheat sourdough, 5%, 15%, …

Mycotoxins in cereals and pulses harvested in Latvia by nanoLC-Orbitrap MS

Twenty-seven mycotoxins in unprocessed cereals (n = 110) and pulses (n = 23) harvested in Latvia were analysed by nanoflow liquid chromatography combined with Orbitrap high-resolution mass spectrometry. One or more mycotoxins were found in 99% of the cereals and 78% of the pulses. Deoxynivalenol, zearalenone and T-2 and HT-2 toxins were prevalent in 9 to 86% of the cereals, mostly below their maximum levels as set by the European regulations. Non-regulated type A and B trichothecenes were prevalent in 5 to 87% of the cereals, at concentrations of 0.27–83 µg kg−1 and 1.7–4,781 µg kg−1, respectively. Quantification of emerging mycotoxins was also provided. Enniatins were detected in 94% of th…

The contribution of P. acidilactici, L. plantarum, and L. curvatus starters and L-(+)-lactic acid to the acrylamide content and quality parameters of mixed rye - Wheat bread

Abstract Lactic acid bacteria (LAB) from spontaneous rye sourdough were isolated, identified, and characterized by their growth, acidification rate, and carbohydrate metabolism. The isolated LAB were used for production of rye sourdough, and the influence of sourdough on mixed rye - wheat bread quality and acrylamide formation was evaluated. In addition, comparative studies by using acidification with L-(+)-lactic acid for mixed rye – wheat bread production were performed. Isolated LAB (P. acidilactici, L. plantarum, L. curvatus) demonstrated versatile carbohydrate metabolism, grown at 30 °C and 37 °C, and acidic tolerance. When the isolated strains were used for rye sourdough production, t…

Determination of pharmaceutical residues and assessment of their removal efficiency at the Daugavgriva municipal wastewater treatment plant in Riga, Latvia

Pharmaceutical products (PPs) belong to emerging contaminants that may accumulate along with other chemical pollutants in wastewaters (WWs) entering industrial and/or urban wastewater treatment plants (WWTPs). In the present study, the technique of ultra-high-performance liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (Orbitrap-HRMS) was applied for the analysis of 24 multi-class PPs in WW samples collected at different technological stages of Daugavgriva WWTP located in Riga, Latvia. Caffeine and acetaminophen levels in the range of 7,570–11,403 ng/L and 810–1,883 ng/L, respectively, were the predominant compounds among 19 PPs determined in the WW. The results i…

Application of Wastewater-Based Epidemiology for Tracking Human Exposure to Deoxynivalenol and Enniatins

Wastewater-based epidemiology (WBE) is a promising biomonitoring approach with the potential to provide direct information on human intake and exposure to food contaminants and environmental chemicals. The aim of this study was to apply WBE while employing the normalization method for exploring human exposure to selected mycotoxins according to population biomarker 5-hydroxyindoleacetic acid (5-HIAA). This type of normalization technique has been previously used to detect various other compounds. However, to the best of our knowledge, this is the first study tracking human exposure to mycotoxins. A sensitive analytical methodology was developed to achieve reliable quantification of deoxyniv…

Determination of pharmaceutical residues in wastewater using high performance liquid chromatography coupled to quadrupole-Orbitrap mass spectrometry

Abstract A multi-class method for the determination of 24 emerging pharmaceutical residues has been developed and validated. The method is based on solid-phase extraction of wastewater samples using Strata-X cartridges followed by high performance liquid chromatography coupled to hybrid quadrupole − Orbitrap high resolution mass spectrometry (HPLC-Q-Orbitrap-HRMS). A single-laboratory validation procedure showed satisfactory analytical performance. The analysis of 21 samples collected at the wastewater treatment plant in Riga revealed the occurrence of 20 compounds of different therapeutic classes. The highest concentration was found for the central nervous system stimulator caffeine − up t…

Lactic Acid Bacteria Isolation from Spontaneous Sourdough and Their Characterization Including Antimicrobial and Antifungal Properties Evaluation

This research effort aimed at isolating and phenotypically characterizing lactic acid bacteria (LAB) isolates from a spontaneous rye sourdough manufactured following traditional protocols, as well as at evaluating their antimicrobial and antifungal properties as key features for future industrial applications. Thirteen LAB strains of potential industrial interest were isolated and identified to species-level via PCR. Most of the sourdough isolates showed versatile carbohydrate metabolisms. The Leuconostoc mesenteroides No. 242 and Lactobacillus brevis No. 173 demonstrated to be gas producers

Occurrence of glyphosate in beer from the Latvian market.

A sensitive LC-MS/MS method for the determination of glyphosate in beer has been developed, validated, and applied to analyse 100 beer samples from 24 different producers and distributors in Latvia. The selected samples represented most beer brands and varieties sold in local supermarkets. Different procedures for sample preparation and chromatographic separation were compared. The final version of the method consisted of solid phase extraction, chromatographic separation on aminopropyl stationary phase, and detection using tandem mass spectrometry. The concentration of glyphosate in beer varied from below the LOD of 0.2 μg kg-1 up to 150 μg kg-1, higher than previously reported. Significan…

Occurrence and risk assessment of mycotoxins, acrylamide, and furan in Latvian beer.

This work reports data on the occurrence of nine mycotoxins and two food processing contaminants - acrylamide and furan - in a total of 100 beers produced in Latvia. Mycotoxins were detected by high-performance liquid chromatography (HPLC) coupled with time-of-flight mass spectrometry, acrylamide by HPLC coupled with quadrupole-Orbitrap mass spectrometry, and furan by headspace gas chromatography-mass spectrometry. The most frequently occurring mycotoxins were HT-2 and deoxynivalenol (DON), which were detected in 52% and 51% of the analysed samples. The highest content was observed for DON, reaching the maximum of 248 µg kg-1. Furan was ubiquitous, and 74% of the samples contained acrylamid…

Two-dimensional liquid chromatography - high resolution mass spectrometry method for simultaneous monitoring of 70 regulated and emerging mycotoxins in Pu-erh tea

Lactic Acid Bacteria Combinations for Wheat Sourdough Preparation and Their Influence on Wheat Bread Quality and Acrylamide Formation

Different lactic acid bacteria (LAB) from spontaneous wheat sourdough were isolated, identified, and characterized by their growth, acidification rate, and carbohydrate metabolism. The combinations of isolated LAB (Pediococcus pentosaceus LUHS183 and Leuconostoc mesenteroides LUHS242, P. pentosaceus LUHS183 and Lactobacillus brevis LUHS173, P. pentosaceus LUHS183 and Enterococcus pseudoavium LUHS 234, P. pentosaceus LUHS183 and Lactobacillus curvatus LUHS51, Lactobacillus plantarum LUHS135 and L. curvatus LUHS51, L. plantarum LUHS135 and P. pentosaceus LUHS183) were used for wheat sourdough production, and the effects of LAB fermentation in sourdoughs on wheat bread quality parameters and a…

Influence of the addition ofHelianthus tuberosusL. fermented with different lactobacilli on acrylamide content in biscuits

Summary The aim of the study was to investigate the effect of the addition of Helianthus tuberosus L. fermented with different lactobacilli (Lactobacillus sakei KTU05-6, Pediococcus acidilactici KTU05-7 and Pediococcus pentosaceus KTU05-9) on acrylamide content in biscuits. Results of study indicated that submerged fermented Helianthus tuberosus L. tubers had the significantly (P ≤ 0.05) lower pH, higher total titratable acidity and from 1.2 to 1.3 times higher protease and from 1.2 to 2.0 higher alpha-amylase activities compared with treated by solid-state fermentation. The acrylamide content in all biscuit samples enriched with submerged fermented Helianthus tuberosus L. was measured lowe…

The quality of wheat bread with ultrasonicated and fermented by-products from plant drinks production

During plant-based drinks production a significant amount of valuable by-products (BPs) is obtained. The valorization of BPs is beneficial for both the environment and the food industry. The direct incorporation of the fermented and/or ultrasonicated almond, coconut, and oat drinks production BPs in other food products, such as wheat bread (WB) could lead to the better nutritional value as well as quality of WB. Therefore, in this study, various quantities (5, 10, 15, and 20%) of differently treated [ultrasonicated (37 kHz) or fermented with Lacticaseibacillus casei LUHS210] almond, coconut, and oat drinks preparation BPs were used in wheat bread (WB) formulations. Microbiological and other…

Application of Pediococcus acidilactici LUHS29 immobilized in apple pomace matrix for high value wheat-barley sourdough bread

The aim of this study was to evaluate the potential use of Pediococcus acidilactici LUHS29 immobilized in apple pomace in case to apply in barley sourdough fermentation for functional bread production. The strain was phenotypically characterized by the growth and acidification rate, carbohydrate metabolism and resistance to acidic conditions. The effect of immobilized bacterial cells on antioxidant properties of barley sourdough and on the acrylamide content in wheat-barley bread was analyzed. The phenotypic and molecular testing indicates the P. acidilactici having a versatile carbohydrate metabolism and acid resistance, showing 42.7% of viable cells surviving after incubation at low pH as…

The effects of woodchip- and straw-derived biochars on the persistence of the herbicide 4-chloro-2-methylphenoxyacetic acid (MCPA) in soils

Sorption and degradation are the primary processes controlling the efficacy and runoff contamination risk of agrochemicals. This study assessed the influence of two biochars, made from woodchips and straw at a pyrolysis temperature of 725°C and applied to a loamy sand and a sandy soil in the concentration of 5.3 g 100 g(-1) sandy soil and 4.1 g 100 g(-1) loamy sand soil, or 53 t ha(-1) for both soil types, on degradation of the herbicide 4-chloro-2-methylphenoxyacetic acid (MCPA). Soils were spiked with 50 mg MCPA kg(-1) soil. In the sandy soil, significantly more MCPA remained after 100 days if amended with straw-derived biochar in comparison to wood-derived biochar. Both biochars types si…

The effects of ultrasonication, fermentation with Lactobacillus sp., and dehydration on the chemical composition and microbial contamination of bovine colostrum.

The aim of this study was to evaluate the influence of ultrasonication, fermentation with Lactobacillus plantarum LUHS135 and Lactobacillus paracasei LUHS244, and different methods of dehydration on the chemical composition of bovine colostrum (BC), including the fatty acid and free amino acid profile and the content of micro- and macroelements. In addition, we analyzed the changes in lactic acid bacteria count, microbial contamination (aerobic mesophilic spore-forming bacteria, enterobacteria including Escherichia coli, and fungi/yeasts), the abundance of biogenic amines, and the concentration of nucleotide monophosphates. Significant effects of different treatments on the free amino acid …

The application of headspace gas chromatography coupled to tandem quadrupole mass spectrometry for the analysis of furan in baby food samples.

Abstract Selective methodology employing a tandem quadrupole mass spectrometer coupled to a gas chromatograph with headspace autosampler (HS-GC–MS/MS) was elaborated in this study. Application of the elaborated procedure resulted in a limit of detection of 0.021 μg kg −1 and a limit of quantification of 0.071 μg kg −1 . The mean recoveries during in-house validation ranged from 89% to 109%, and coefficients of variation for repeatability ranged from 4% to 11%. The proposed analytical method was applied for monitoring the furan content of 30 commercial baby food samples available on the Latvian retail market. The level of furan found in these samples varied from 0.45 to 81.9 μg kg −1 , indic…

Challenges of Lactobacillus fermentation in combination with acoustic screening for deoxynivalenol and deoxynivalenol conjugates reduction in contaminated wheat - based products

Abstract This study was dedicated to apply biological treatment using Lactobacillus (LAB) fermentation separately or in combination with an acoustic screening method for the prevention of mycotoxins in Fusarium spp. contaminated wheat-based products. Wheat samples of different contamination were treated separately using antimicrobial LAB strains (L. casei, L. plantarum, L. paracasei, and L. uvarum) and the changes on the level of deoxynivalenol (DON) and its conjugates such as 3-acetyldeoxynivalenol (3-ADON), 15-acetyldeoxynivalenol (15-ADON), and DON-3-β-D-glucoside (D3G)) were evaluated using UHPLC-QqQ-MS/MS and UHPLC-Orbitrap-HRMS. Additionally, an acoustic device was used to analyse DON…

Challenges Associated with Byproducts Valorization—Comparison Study of Safety Parameters of Ultrasonicated and Fermented Plant-Based Byproducts

In order to promote the efficient use of byproducts from the production of plant-based beverages, which still contain a large amount of nutritional and functional compounds, microbiological and chemical safety characteristics should be evaluated and, if needed, improved. Many challenges are associated with byproducts valorization, and the most important ones, which should be taken into account at the further steps of valorization, are biological and chemical safety. For safety improving, several technological treatments (biological, physical etc.) can be used. In this study, the influence of low-frequency ultrasonication (US) and fermentation with Lactobacillus casei LUHS210 strain, as phys…

Determination of Fungi and Multi-Class Mycotoxins in Camelia sinensis and Herbal Teas and Dietary Exposure Assessment

In this paper, a study of fungal and multi-mycotoxin contamination in 140 Camellia sinensis and 26 herbal teas marketed in Latvia is discussed. The analysis was performed using two-dimensional liquid chromatography with time-of-flight mass spectrometry (2D-LC-TOF-MS) and MALDI-TOF-MS. In total, 87% of the tea samples tested positive for 32 fungal species belonging to 17 genera, with the total enumeration of moulds ranging between 1.00 &times

The Influence of Scalded Flour, Fermentation, and Plants Belonging to Lamiaceae Family on the Wheat Bread Quality and Acrylamide Content

The aim of this study was to investigate the influence of additives such as plants belonging to Lamiaceaefamily (Thymus vulgaris, Carum carvi, Origanum vulgare, Ocimum basilicum, and Coriandrum sativum), scalded flour (SF) or scalded flour fermented with Lactobacillus plantarumLUHS135 (SFFLp) on the quality and acrylamide formation in wheat bread. The formation of acrylamide and bread quality significantly depended on the king of plants used and the amount of SF and SFFLp used. The additives of T. vulgarisand SF increased the content of acrylamide by 3.4-fold in comparison with bread prepared without SF, whereas the addition of SFFLp significantly reduced the content of acrylamide in bread,…

Development of a Rapid Method for the Determination of Phenolic Antioxidants in Dark Chocolate Using Ultra Performance Liquid Chromatography Coupled to Orbitrap Mass Spectrometry

Development of a new comprehensive method based on one-step liquid-liquid extraction (LLE) combined with ultra-high-performance liquid chromatography-Orbitrap high resolution mass spectrometry (UHPLC-Orbitrap-HRMS) for the determination of eight phenolic compounds in dark chocolate is demonstrated. The study focuses on the optimization of sample preparation, chromatographic separation and Orbitrap-HRMS detection parameters to adjust selectivity and sensitivity of the method. The LLE mixture of formic acid-water-acetonitrile (2:58:40, v/v) and hexane at the component ratio of 1:1 (v/v) was applied for sample preparation. The inter-day and intra-day precision expressed from the relative stand…

Occurrence of polybrominated diphenyl ethers, perfluorinated compounds, and nonsteroidal anti-inflammatory drugs in freshwater mussels from Latvia.

Abstract The occurrence of polybrominated diphenyl ethers (PBDE), perfluorinated compounds (PFC), and nonsteroidal anti-inflammatory drugs (NSAID) in Latvian freshwater ecosystems was evaluated by using filter-feeding mussels as bioindicators. Twenty four samples of mussels were collected from freshwater bodies throughout the territory of Latvia during the summer of 2017. PBDE contamination was ubiquitous, reaching the highest total concentration of 193.2 pg g−1 w.w. BDE-209 was the most abundant compound, followed by penta-BDE components BDE-49, -100, −99, −153, −154, and −47 in decreasing order. The levels of PFCs in Latvian mussels were generally lower than those reported from other regi…

Development and application of mass spectrometric methods for the determination of Maillard reaction products in foodstuffs

Tika izstrādātas jaunas analītiskā s metodes divu pārtikas produktos sastopamo toksikantu noteikšanai, kuri rodas produktos Maijāra reakcijas rezultātā. Pirmo reizi zinātniskajā literatūrā Orbitrap masspektr o metra analītiskās spējas tika piemērotas akrilamīda noteikšanai kafijas paraugos. Izstrādātā metode uzrādīja selektīvu un precīzu detektēšan as spēju mazu molekulu, kā akrilamīds, kvantitatīv ai noteikšan ai sarežģītās matricās, piemēram, kafijā. Instruments nodrošina augstu izšķirtspēju, ļoti labu jūtību, lineāru diapazonu un labu atkārtojamību. Izstrādātā s m etodes salīdzinājums ar tandēma kvadrupola detektēšanas metodi uzrādīja pārākumu šim konkrētajam analīzes veidam. Kafijas par…

Development and optimization of confirmatory liquid chromatography—Orbitrap mass spectrometry method for the determination of 17 anticoccidials in poultry and eggs

A new sensitive and selective multi-residue method based on liquid chromatography - Orbitrap high resolution mass spectrometry (LC-Orbitrap-HRMS) was developed and validated for the determination of 17 anticoccidials in poultry and eggs. Instrumental parameters were optimized by the means of statistical experimental designs to improve the sensitivity, precision, and repeatability of the method. Further optimization of auto-tuned MS parameters led to an increase of signal intensity by 10% to 99% for 16 out of 17 analytes. The sample preparation procedure included extraction from muscle tissue and egg samples with acetonitrile, followed by preconcentration, reconstitution, and filtration. Val…

A concept of mould spoilage prevention and acrylamide reduction in wheat bread: application of lactobacilli in combination with a cranberry coating

In this study, a concept for wheat bread moulding prevention and acrylamide reduction has been developed. It includes various lactic acid bacteria (LAB), selected according to their technological, antifungal and acrylamide-lowering properties, in combination with an antifungal cranberry coating for wheat bread surface treatment. All the tested strains (Pediococcus pentosaceus LUHS183, Pediococcus acidilactici LUHS29, Lactobacillus paracasei LUHS244, Lactobacillus brevis LUHS173, Lactobacillus plantarum LUHS135 and Leuconostoc mesenteroides LUHS242) showed antifungal activities against Aspergillus nidulans, Penicillium funiculosum and Fusarium poae. However, L. brevis LUHS173 and Leu. mesent…

Study on the reduction of acrylamide in mixed rye bread by fermentation with bacteriocin-like inhibitory substances producing lactic acid bacteria in combination with Aspergillus niger glucoamylase

Abstract This study mainly focuses on a strategy for reducing of acrylamide in cereal products, predominantly in bakery products. The effect of mesophilic lactic acid bacteria (LAB) strains as well as a novel fermentation media on the bases of extruded rye wholemeal on the acrylamide formation in mixed rye bread of different weight of loaf was studied. The LC–MS/MS method for acrylamide determination in bread crumb has been applied. Addition of 15% low pH (pH 3.4–4.3) fermented product to bread dough, which were produced by using commercial strain Lactobacillus casei and bacteriocin-like inhibitory substances (BLIS) producing strains Lactobacillus sakei KTU05-6 , Pediococcus acidilactici KT…

The Occurrence and Dietary Exposure Assessment of Mycotoxins, Biogenic Amines, and Heavy Metals in Mould-Ripened Blue Cheeses

The occurrence and dietary exposure assessment of 16 mycotoxins, 6 biogenic amines (BAs), and 13 metallic elements in blue-veined cheeses (n = 46) is reported. Co-occurrence of mycophenolic acid (&le

Recent Applications of Carbonaceous Nanosorbents in Solid Phase Extraction for the Determination of Pesticides in Food Samples

This article covers recent trends of carbonaceous nanomaterial supported solid phase extraction for the liquid and gas chromatography analysis of pesticides in food samples. Several advanced carbonaceous nanosorbents have been reported over the previous decade for pesticide extraction, such as graphene derivatives modified by combination with silica, amines, polymers, and/or magnetic nanoparticles. The advances in this field have opened possibilities for using neat or modified carbon nanotubes or graphene-type sorbents for the pre-concentration of polar or nonpolar pesticides by solid phase extraction (SPE) or micro-SPE methods or to apply such nanomaterials for the removal of matrix compon…

Evaluation of selected buffers for simultaneous determination of ionic and acidic pesticides including glyphosate using anion exchange chromatography with mass spectrometric detection

Ion chromatography coupled with mass spectrometry is an established technique for determination of ionic analytes, however, sophisticated buffer removal equipment is required to eliminate inorganic compounds from the eluate before introduction into the ion source of mass spectrometer. A standard high-performance liquid chromatography coupled with tandem mass spectrometry setup using an ion exchange column (Metrosep® A Supp 5) is proposed as an alternative approach. For that reason, some buffers including non-volatile carboxylic acid based solutions have been evaluated for simultaneous trace determination of ionic and acidic pesticides including glyphosate in the same extract without a need …

Development of a sensitive method for the determination of acrylamide in coffee using high-performance liquid chromatography coupled to a hybrid quadrupole Orbitrap mass spectrometer

The emerging trend towards high-resolution mass spectrometry (MS) alternatives was evaluated by the application of Orbitrap MS for the determination of acrylamide in coffee samples. The high resolving power of the Orbitrap MS provided the high selectivity and sensitivity that enabled quantitative analysis of acrylamide in complex matrices, such as coffee. Several sample preparation methods and scanning modes of the MS (full MS, t-SIM, t-MS2) were assessed in order to optimise parameters of the analytical method. The final procedure involved the extraction of acrylamide with acetonitrile, solid-phase extraction with dispersive primary secondary amine (PSA) and amino columns, and the detectio…

Reducing of acrylamide formation in wheat biscuits supplemented with flaxseed and lupine

Abstract The use of pseudo-cereals for wheat products making is to fortify the deficiency of nutritional value in wheat flour. However rich in proteins plant additives could increase acrylamide content in baked products. The present study was focused on acrylamide reduction in wheat flour biscuits supplemented with lupine and defatted flaxseed flour treated by solid state (SSF) and submerged (SMF) fermentations by Lactobacillus sakei , Pediococcus pentosaceus and Pediococcus acidilactici strains. After fermentation the decrease in asparagine was on average of 67.6 and 80.6%, and reducing sugar contents were reduced by 18 and 79.4% in flaxseed and lupine, respectively. The most effective acr…

Occurrence of glyphosate in beer from the Latvian market

A sensitive LC-MS/MS method for the determination of glyphosate in beer has been developed, validated, and applied to analyse 100 beer samples from 24 different producers and distributors in Latvia. The selected samples represented most beer brands and varieties sold in local supermarkets. Different procedures for sample preparation and chromatographic separation were compared. The final version of the method consisted of solid phase extraction, chromatographic separation on aminopropyl stationary phase, and detection using tandem mass spectrometry. The concentration of glyphosate in beer varied from below the LOD of 0.2 μg kg−1 up to 150 μg kg−1, higher than previously reported. Significan…