Determination Of Mycotoxins Research Articles

Improving analytical performance for pesticides and mycotoxins determination in Brazilian table olives: one extraction and one analysis.

This paper describes an extensive study in which a multiclass QuEChERS based approach was optimized for determination of 150 pesticides and 7 mycotoxins in table olives. Three versions of QuEChERS were evaluated and compared (unbuffered, citrate and acetate buffering). A combination of EMR-Lipid cartridges and liquid nitrogen or freezer freezing out were tested for clean-up of the oily olive extracts. Analysis of the extracts were performed by LC-MS/MS triple quadrupole. The best results were achieved using acetate QuEChERS with liquid nitrogen for clean-up. For validation, organic olives were ground and spiked at 4 concentrations with pesticides and mycotoxins (n = 5). The linearity of the calibration curves was assessed by analyzing calibration standards of 7 concentrations which were prepared separately in acetonitrile and in blank olive extract (n = 5). The validation study demonstrated that the calculated r2 was ≥0.99 for 144 pesticides and 6 mycotoxins, when the calibration curves were prepared in matrix extract, showing satisfactory linearity. Matrix effects were within the range of ±20% for only 46 pesticides and one mycotoxin. Then, to ensure reliable quantification, calibration standards had to be matrix-matched. In accuracy experiments 138 pesticides and 6 mycotoxins presented recoveries from 70 to 120% and RSD ≤ 20% for at least 2 of the 4 spike concentrations evaluated, being successfully validated. The integrated QuEChERS and LC-MS/MS method meet MRL for 11 of the 21 pesticides regulated for olives in Brazil and for 132 pesticides which are regulated in the EU law. Eleven commercial table olive samples were analyzed and 4 of them tested positive for pesticides. All the positive samples violate the Brazilian law and one sample violates also the European law.

Ochratoxin A case study: Establish metrological traceability of mycotoxin measurements using certified reference materials.

For the US Food and Drug Administration's (FDA) mycotoxin program, the desired application of certified reference materials (CRMs) is primarily for validating methods for the determination of mycotoxins in foods and establishing metrological traceability of measurement results generated by such validated methods. The latter has been an important but insufficiently addressed challenge due to the lack of appropriate protocols and CRMs. Taking advantage of two recently available mycotoxin CRMs, OTAN-1 and Standard Reference Material (SRM) 1565, a protocol was developed for systematically examining uncertainty and establishing metrological traceability of measurement results of ochratoxin A (OTA) in corn through a series of calibration operations using the two CRMs. Instrument and method calibrations were performed using OTAN-1 and SRM 1565. The OTA value and its standard and expanded (k=2, approximately 95% confidence) uncertainties were estimated from the calibration data and documented. These results demonstrate that the major contributing source of uncertainty is the sample matrix, highlighting the important role of the certified matrix reference material in method calibration. The value of OTA (38.5±7.2µg/g; 95% confidence interval) in the incurred sample was metrologically traceable to the International System of Units through two CRMs using the multi-laboratory validated liquid chromatography-mass spectrometry FDA compendial method. In addition, an alternative estimation of uncertainty was conducted using a one-point calibration, resulting in comparable uncertainty.

A versatile CuCo@PDA nanozyme-based aptamer-mediated lateral flow assay for highly sensitive, on-site and dual-readout detection of Aflatoxin B1

Mycotoxin contaminations in food and environment seriously harms human health. Constructing sensitive and point-of-test early-warning tools for mycotoxin determination is in high demand. In this study, a CuCo@PDA nanozyme-based aptamer-mediated lateral flow assay (Apt-LFA) has been elaborately designed for on-site and sensitive determination of mycotoxin Aflatoxin B1 (AFB1). Benefiting from the rich functional groups and excellent peroxidase-like activity, the CuCo@PDA with original dark color can be conjugated with the specific recognition probe (i.e., aptamer), generating colorimetric signal on the test lines of Apt-LFA via a competitive sensing strategy. The signal can further be amplified in-situ by catalytic chromogenic reaction. Therefore, a visual and dual-readout detection of AFB1 has been realized. The developed Apt-LFA provides a flexible detection mode for qualitative and quantitative analysis of AFB1 by naked-eyes observation or smartphone readout. The smartphone-based LFA platform shows a reliable and ultrasensitive determination of AFB1 with the limit of detection (LOD) of 2.2 pg/mL. The recoveries in the real samples are in the range of 95.11–113.77% with coefficients of variations less than 9.84%. This study provides a new approach to realize point-of-test and sensitive detection of mycotoxins in food and environment using nanozyme-based Apt-LFAs.

A Study of a New Certified Reference Material for Accurate Determination of the Main Fusarium Mycotoxins in Whole-Wheat Flour.

Matrix certified reference materials (CRMs) play a critical role in analytical method validation and the assurance of reliable measurement results. A certified reference material (GBW(E)100813) for whole-wheat flour was developed to ensure an accurate and reliable measurement of the main Fusarium mycotoxins (deoxynivalenol (DON), nivalenol (NIV), deoxynivalenol-3-glucoside (DON-3G), and zearalenone (ZEN)). CRM candidates were prepared using sun-drying, grinding, sieving, homogenising, packaging, and gamma irradiation. The final produced CRM was packaged at 50 g per unit and stored at 20 °C. Certification was performed using isotope dilution-liquid chromatography-tandem mass spectrometry. CRM characterization was performed in eight laboratories in accordance with the requirements of ISO Guide 35. The certified values and expanded uncertainties (at a confidence of 95%, k = 2) for DON, NIV, DON-3G, and ZEN were determined to be 0.98 ± 0.12 mg/kg, 1.37 ± 0.20 mg/kg, 242 ± 35 μg/g, and 382 ± 50 μg/g. The CRM was sufficiently homogeneous between and within bottles, and remained stable for up to 12 months at 20 °C and 9 days below 40 °C for transportation. Thus, CRM can be used for quality control and method validation to ensure the accurate and reliable quantification of the main Fusarium mycotoxins in whole-wheat flour.

The Determination of Mycotoxins in the Composition of Walnut (Juglans Regia L.) Fruits Cultivated in Different Geographical Regions of Uzbekistan by High–Performance Liquid Chromatography Method and Their Comparative Analysis

Mycotoxins are secondary metabolites produced by various fungi and are known to have significant adverse effects on human and animal health. If food products are contaminated with mycotoxins, their toxicity can cause various diseases. In this scientific research work, residual mycotoxins in nutrients were combined with liquid–liquid extraction (LLE) and analyzed through the use of reversed–phase high–performance liquid chromatography (RP–HPLC). These scientific studies were conducted in the experimental biology laboratory of Gulistan State University to determine the amount of aflatoxin (AFB2, AFG1, AFG2) in the samples of walnuts cultivated in six regions of Uzbekistan. The study revealed the detection of aflatoxins AFG1 type 0.003 in the designated region labeled as S20, AFB2 and AFG2 0.001 in J25, and AFG2 0.002 in S30. However, it is important to note that these levels did not above the maximum residue level standards established by the Republic of Uzbekistan. However, the aflatoxins produced by fungi are released based on the development of fungi at a temperature of 25–3000C, therefore it is recommended to store walnut fruits in dry conditions at a temperature of 1500C. All the methods used during scientific analysis can demonstrate high sensitivity and accuracy. All methods are successfully used to identify mycotoxins in the composition of walnut fruits, separate them from fungi and specify the amount of ingredients.

Non-target analysis of livestock products and feed for residues of drugs, pesticides, mycotoxins and their metabolites by high-resolution mass spectrometry (a review)

A review of techniques of non-target analysis for simultaneous identification and determination of veterinary drugs, pesticides, mycotoxins, their metabolites, and substances of chemical transformation in livestock products using liquid chromatography and high-resolution mass spectrometry is presented. Some limitations of the approach are noted, such as the necessity of using common extraction conditions, the possibility of analyte transformations during the sample preparation, false positive results for isobaric and isomeric compounds, and the lack of spectral data for previously unexplored substances. However, the method is the most promising tool for the determination of pollutants not identified in the targeted analysis, as in the case of multicomponent screening of food and raw materials, and in the study of the parent compounds transformation.

Deep Eutectic Solvent-Based Dispersive Liquid-Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum.

Ochratoxins, a common class of mycotoxin in capsicum, and techniques and methods for the determination of mycotoxins in spices have been increasingly developed in recent years. An innovative and eco-friendly method of dispersive liquid-liquid microextraction (DLLME) was demonstrated in this study, based on a synthesized deep eutectic solvent (DES) combined with LC-MS/MS, for the quantification and analysis of two ochratoxins in capsicum. The DES-DLLME method parameters entail selecting the DES type (thymol:decanoic acid, molar ratio 1:1) and DES volume (100 μL). The volume of water (3 mL) and salt concentration (0 g) undergo optimization following a step-by-step approach to achieve optimal target substance extraction efficiency. The matrix effect associated with the direct detection of the target substance in capsicum was significantly reduced in this study by the addition of isotopic internal standards corresponding to the target substance. This facilitated optimal conditions wherein quantitative analysis using LC-MS/MS revealed a linear range of 0.50-250.00 µg/mL, with all two curves calibrated with internal standards showing correlation coefficients (r2) greater than 0.9995. The method's limits of detection (LODs) and limits of quantification (LOQs) fell in the ranges of 0.14-0.45 μg/kg and 0.45-1.45 μg/kg, respectively. The method's spiked recoveries ranged from 81.97 to 105.17%, indicating its sensitivity and accuracy. The environmental friendliness of the technique was assessed using two green assessment tools, AGREE and complexGAPI, and the results showed that the technique was more in line with the concept of sustainable development compared to other techniques for detecting ochratoxins in capsicum. Overall, this study provides a new approach for the determination of mycotoxins in a complex food matrix such as capsicum and other spices using DES and also contributes to the application of green analytical chemistry methods in the food industry.

Interconnectable 3D-printed sample processing modules for portable mycotoxin screening of intact wheat

BackgroundThe increasing demand for food and feed products is stretching the capacity of the food value chain to its limits. A key step for ensuring food safety is checking for mycotoxin contamination of wheat. However, this analysis is typically performed by rather complex and expensive chromatographic methods, such as liquid chromatography-tandem mass spectrometry (LC-MS/MS). These costly methods require extensive sample preparation that is not easily carried out at different points along the food supply chain. To overcome such challenges in sample processing, an inexpensive and portable sample preparation device was needed, that required low skill, for rapid sample-to-result mycotoxin screening. ResultsWe describe 3D-printed and interconnectable modules for simple, integrated and on-site sample preparation, including grinding of wheat kernels, and solvent-based extraction. We characterized these 3D-printed modules for mycotoxin screening and benchmarked them against a laboratory mill using commercial lateral flow device(s) (LFD) and in-house validated LC-MS/MS analysis. Different integrated sieve configurations were compared based on grinding efficiency, and we selected a sieve size of 2 mm allowing grinding of 10 g of wheat within 5 min. Moreover, 10 first time-users were able to operate the grinder module with minimal instructions. Screening for deoxynivalenol (DON) in naturally contaminated samples at the regulatory/legal limit (1.25 mg kg−1) was demonstrated using the developed 3D-printed prototype. The whole process only takes 15 min, from sample preparation to screening result. The results showed a clear correlation (R2 = 0.96) between the LFD and LC-MS/MS. SignificanceOur findings demonstrate the potential of 3D-printed sample handling equipment as a valuable extension of existing analytical procedures, facilitating the on-site implementation of rapid methods for the determination of mycotoxins in grains. The presented prototype is inexpensive with material costs of 2.5€, relies on biodegradable 3D printing filament and can be produced with consumer-grade printers, making the prototype readily available. As a future perspective, the modular character of our developed tool kit will allow for adaptation to other hard food commodities beyond the determination of DON in wheat.

Determination of 22 mycotoxins in milk by liquid chromatography-quadrupole/orbitrap mass spectrometry

Mycotoxins have carcinogenic, mutagenic, hepatotoxic, nephrotoxic, immunotoxic, neurotoxic, and teratogenic properties. Thus, these substances have attracted significant attention because they pose a threat to human health. As research on mycotoxins deepens, new structural analogues of mycotoxins are constantly being discovered. In this study, a method based on high performance liquid chromatography-quadrupole/orbitrap mass spectrometry was established for the simultaneous determination of 22 mycotoxins in milk. A simple, effective, and rapid pretreatment method was optimized by focusing on the solvent type, extractant volume, and extracting salt based on the characteristics of the mycotoxins and sample matrix. The analytes were extracted using 0.5% formic acid acetonitrile solution and added with sodium chloride to separate fats from water. The samples were centrifuged at 8000 r/min (4 ℃) for 5 min using a centrifuge and then concentrated using nitrogen. The dry residue was dissolved with 50% methanol aqueous solution. Twenty-two mycotoxins were separated on a ZORBAX Eclipse Plus C18 chromatographic column (100 mm×2.1 mm, 1.7 μm), and quantitative analysis was performed using the isotope internal standard method. The analytes were determined by liquid chromatography-quadrupole/orbitrap mass spectrometry in positive electrospray ionization mode. Qualitative analyses of the compounds were performed in full mass spectrometry/data-dependent tandem mass spectrometry (MS/dd-MS2) mode. Good linearities in the range of 0.5-100.0 μg/L were observed for the 22 mycotoxins, and the correlation coefficients (R2) were greater than 0.999. The limits of detection (S/N=3) and quantification (S/N=10) ranged from 0.3 to 0.5 μg/kg and from 1.0 to 1.5 μg/kg, respectively. The average recoveries of the 22 mycotoxins at three spiked levels of 1.5, 5.0, and 15 μg/kg were between 84.7% and 100.8%, with relative standard deviations (RSDs) of 1.2%-9.9%. These findings indicate that the method has high sensitivity and accuracy as well as good precision. Finally, the method was applied to the detection and analysis of mycotoxins in 25 actual commercial milk samples. The results revealed that the selected samples were not contaminated with any of the mycotoxins analyzed. Thus, the proposed method is useful as a quick preprocessing and confirmatory method for the simultaneous determination of mycotoxins in milk.

Simultaneous Determination of Pesticide Residues and Mycotoxins in Storage Pu-erh Tea Using Ultra-High-Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry.

Mycotoxins and pesticides are the most concerning chemical contaminants that can affect the quality of Pu-erh tea during its production and storage. This study presents a method that can simultaneously determine 31 pesticide residues and six mycotoxins in Pu-erh tea within 11 min using ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) after QuEChERS extraction. The lower limit of quantification (LOQ) for all analytes ranged between 0.06 and 50 ppb. Recoveries for each pesticide and mycotoxin ranged between 62.0 and 130.3%, with intra- and inter-day precisions lower than 15%. Good linear relationships were obtained, with correlation coefficients of r2 > 0.991 for all analytes. The established method was applied to 31 Pu-erh tea samples, including raw and ripened Pu-erh tea with different storage times. As a result, pesticide residues were not detected in any of the collected samples, and the mycotoxins detected in the samples were well below the official maximum residue limits (MRLs). Notably, the levels of aflatoxin B1 (AFB1), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2) were lower than 1 ppb in the samples stored for more than 30 years.

Determination of Metals, Fungi and Mycotoxins in Cat Meal Samples used in Saudi Arabia

The cat food samples viz Canned Food, Pouched Food, Raw Food, Lightly Cooked Food, Dry Food were analysed for the presence of essential and non-essential metal ions in addition to fungal infection determination. All the food samples were found to have adequate amount of carbohydrates, proteins, lipids, vitamins and folic acid. The concentration of essential elements in all the analysed samples are within the intake range of cats for their normal growth and development. Although the presence of heavy metals makes some concern about the quality of the food samples, but all these heavy metals are below the toxic level. All the food samples showed the presence of microbial fungi to some extent, but the release of micro-toxin from these fungal species are below the level of their profound health related issues among the cats. Among all the samples analysed the best food samples with very good health quality seems the dry food, followed by pouched food.

Determination of mycotoxins in nuts, cereals, legumes, and coffee beans and effectiveness of a selenium‐based decontamination treatment

AbstractLiquid chromatography‐tandem mass spectrometry (LC‐MS/MS) was used for the rapid quantification of multiple mycotoxins, specifically aflatoxins B1, B2, G1, and G2 (AFB1, AFB2, AFG1, and AFG2), ochratoxin A (OTA), deoxynivalenol (DON), and zearalenone (ZEN), in walnuts, pistachios, peanuts, coffee beans, rice, and chickpeas from various countries. Total counts of fungi, Aspergillus flavus, and Aspergillus parasiticus were also assessed, along with the effectiveness of a decontamination treatment with inorganic selenium to reduce mycotoxin levels. Of the 78 samples tested, 69% were contaminated with mycotoxins. ZEN, the predominant mycotoxin contaminant, was detected in all the contaminated samples in concentrations often exceeding the maximum level, followed by AFG1 (28% of the contaminated samples), DON (22%), AFG2 (11%), and AFB1 (5.5%). The occurrence of aflatoxins was associated with high proportions of A. flavus and A. parasiticus. Complete removal of AFB1 from walnuts and DON from roasted coffee beans was achieved by treatment with aqueous selenium, while the levels of ZEN and AFG1 were respectively lowered by 65% to 89% depending on the commodity and by about 56% in roasted coffee beans. While this novel treatment is a promising approach for mycotoxin decontamination, it is not intended to replace safe practices upstream.

Multi-class/residue method for determination of veterinary drug residues, mycotoxins and pesticide in urine using LC-MS/MS technique

BackgroundVeterinary drugs are widely used in animals to prevent diseases and are a complex set of drugs with very different chemical properties. Multiclass and multi-residue methods for simultaneous detection of residues from veterinary drugs and contaminants in urine are very rare or non-existent. Therefore, the aim of this study was to develop and validate a sensitive and reliable quantitative LC-MS/MS method for simultaneous determination of a wide range of veterinary drug and pesticide residues and mycotoxins in bovine urine. This involved 42 veterinary drug residues (4 thyreostats, 6 anabolic hormones, 2 lactones, 10 beta agonists, 15 antibiotics, 5 sulphonamides), 28 pesticides and 2 mycotoxins. Stable isotopically labelled internal standards were used to facilitate effective quantification of the analytes. Analysis was performed in both positive and negative ionization modes with multiple reaction monitoring transitions over a period of 12 min.ResultsThe parameters validated included linearity, limit of detection (LOD), limit of quantification (LOQ), detection capability (CCβ), decision limit (CCα), stability, accuracy and precision. The process followed guidelines of the regulation 2021/808/EC. The calibration curves were linear with coefficient of correlation (R2) from 0.991 to 0.999. The LODs were from 0.01 to 2.71 µg/L, while the LOQs were from 0.05 to 7.52 µg/L. The CCα and CCβ were in range 0.05–12.11 µg/L and 0.08–15.16 µg/L. In addition, the average recoveries of the spiked urine samples were from 71.0 to 117.0% and coefficient of variation (CV) < 21.38% (intraday and interday).ConclusionA new isotopic LC-MS/MS method has been developed, validated and applied for identification and quantification of 72 residues of veterinary drugs and pesticides and other contaminants such as mycotoxins in bovine urine. The most appropriated sample preparation procedures involved sodium acetate buffer, enzymatic hydrolysis using β-glucuronidase and cleanup solid phase extraction with OASIS SPE cartridges. The parameters were satisfactorily validated fulfilling requirements under Regulation 2021/808/EC. Consequently, the method could be used in routine analysis of bovine urine samples for simultaneous detection of veterinary drug and pesticide residues as well as contaminants such as mycotoxins.

Mycotoxins and Maize Value Chain: Multi-Matrix and Multi-Analyte Tools towards Global Feed and Food Safety

Maize value chains represent invaluable end-consumer products in food systems worldwide. Mycotoxin contamination along these chains causes severe economic and health impacts from the plant, animal and human safety points of view. This work aimed to develop a single standardized methodology that fulfilled extraction and detection procedures for 22 mycotoxins in maize chain matrices. The main goal concerned the validation of a QuEChERS-based ultra-high-performance liquid chromatography coupled to the tandem mass spectrometry (UHPLC-MS/MS) method in compliance with established performance criteria for mycotoxin determination. Validation parameters encompassing specificity/selectivity, linearity, precision, recovery, Limits of Detection (LOD) and Limits of Quantification (LOQ) were evaluated, and acceptable data were found for all the mycotoxins in the matrices under study, namely, seeds, flowering plants, silage and feed. The applied method presented LODs and LOQs lower than 40.3 and 42.1 ng g−1, respectively, and recoveries ranging from 80.7 to 118.1%, with precision values below 20.5%. A first-time full analytical procedure in a multi-matrix and multi-analyte approach was successfully validated, representing a valuable control tool for mycotoxin monitoring in maize chains. This approach will ultimately allow a response to the need for integrated risk assessments encompassing full, comprehensive analysis of whole food chains in compliance with the maximum levels established in European regulations, and the establishment of accurate solutions in each chain-specific critical point, helping to provide more sustainable, safer and healthy food systems.

Mycotoxin Determination in Peaches and Peach Products with a Modified QuEChERS Extraction Procedure Coupled with UPLC-MS/MS Analysis.

Peaches are the most significant temperate fruit crop worldwide. However, peach fruits are susceptible to fungal and mycotoxin contamination. Consequently, monitoring the residual levels of multiple mycotoxins in peaches and related products is essential. In this study, a novel method based on QuEChERS extraction, followed by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection, was developed for analyzing 14 mycotoxins in peaches and peach products from China. Matrix-matched calibrations were employed to accurately quantify the mycotoxins and compensate for matrix effects. Recoveries for the target analytes ranged from 84.6% to 117.6%, with intra-day and inter-day precision below 20%. The limits of quantification were 2 or 5 μg/L for the 14 mycotoxins. This method was utilized to detect the presence of target mycotoxins in 109 fresh peaches, 100 diseased peaches, and 89 peach products from China. Six mycotoxins were identified in the rotten parts of the diseased peaches, with concentrations ranging from 5.2 to 1664.3 µg/kg. In the remaining parts of the diseased peach samples, only two toxins, alternariol (AOH) and alternariol monomethyl ether (AME), were quantified at levels of 15.3 µg/kg and 15.5 µg/kg, respectively. No mycotoxins were detected in fresh peaches. For peach products, all contamination levels were below the quantitative limits and significantly lower than the maximum legal limits established for the products.

Fusarium Mycotoxins and OTA in Beer from Shanghai, the Largest Megacity in China: Occurrence and Dietary Risk Assessment.

Beer is susceptible to mycotoxin contamination originating from infected grains. It could be that mycotoxins are not completely removed during the brewing process and remain in the final product. Nevertheless, there have been no surveys of exposure to mycotoxin for Chinese inhabitants through beer consumption. This study aimed to investigate the presence of eight mycotoxins in 158 beer samples purchased in Shanghai, the largest megacity in China. The multiple mycotoxins determination was carried out using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Our findings revealed that 48.1% (76/158) of the beer samples were contaminated with Fusarium toxins. Deoxynivalenol-3-glucoside (D3G) and zearalenone (ZEN) were detected in 34.81% and 16.46% of the total samples, respectively. The significant differences between D3G/ZEN contamination and various beer types were performed. Furthermore, this study performed a health risk assessment for Shanghai residents based on data for Fusarium toxins and ochratoxin A (OTA) present in beer for the first time. The results revealed that the 95th percentile dietary exposures of Shanghai residents did not pose any chronic or acute health risks, either individually or in combination. Dietary exposures to Fusarium toxins revealed different risk levels among residents. The cumulative health risk for women is higher than that for men at the same beer consumption. In addition, the acute risk of DONs exposure for adults deserves concern. The insights obtained from this study may be of assistance for beer manufacturers and governmental regulators to further develop beer monitoring and guarantee public health.

Recent advances in rare earth ion-doped upconversion nanomaterials: From design to their applications in food safety analysis.

The misuse of chemicals in agricultural systems and food production leads to an increase in contaminants in food, which ultimately has adverse effects on human health. This situation has prompted a demand for sophisticated detection technologies with rapid and sensitive features, as concerns over food safety and quality have grown around the globe. The rare earth ion-doped upconversion nanoparticle (UCNP)-based sensor has emerged as an innovative and promising approach for detecting and analyzing food contaminants due to its superior photophysical properties, including low autofluorescence background, deep penetration of light, low toxicity, and minimal photodamage to the biological samples. The aim of this review was to discuss an outline of the applications of UCNPs to detect contaminants in food matrices, with particular attention on the determination of heavy metals, pesticides, pathogenic bacteria, mycotoxins, and antibiotics. The review briefly discusses the mechanism of upconversion (UC) luminescence, the synthesis, modification, functionality of UCNPs, as well as the detection principles for the design of UC biosensors. Furthermore, because current UCNP research on food safety detection is still at an early stage, this review identifies several bottlenecks that must be overcome in UCNPs and discusses the future prospects for its application in the field of food analysis.

Development and validation of a QuEChERS-LC-MS/MS method for determination of multiple mycotoxins in maize and sorghum from Botswana.

Climatic conditions such as drought, high temperatures, and pre-harvest rainfalls promote the occurrence of mycotoxins in grains. Contamination of staple food sources such as maize and sorghum means that many populations are at risk of being poisoned by mycotoxins. Hence the need for sensitive methods for their simultaneous analysis. Herein, a quick, easy, cheap, effective, rugged, and safe liquid chromatography tandem mass spectrometry (QuEChERS-LC-MS/MS) method for the simultaneous determination of ten mycotoxins in maize and sorghum is presented. The QuEChERS extraction procedure was optimized to maximize extraction recovery and minimize matrix effects while using relatively small quantities of organic solvents and acids. This method was validated according to Commission Implementing Regulation (EU) 2021/808, Commission Regulation (EC) No 1881/2006, and Regulation (EC) no. 401/2006. The developed method met the specified requirements. Recoveries of 80.77% to 109.83% and CVs below 15% were obtained. The correlation coefficient values (R2) were all above 0.98, and low limits of quantification ranging from 0.53 to 89.28 µg/Kg were recorded. The method was applied to 10 maize and 10 sorghum samples collected from markets in Botswana. Half of the samples had detectable mycotoxins, Aflatoxins, Fumonisins, T2-toxin, HT2-toxin, and Zearalenone. Two maize samples had levels of aflatoxin B1 above the maximum permitted level (2.55, 4.07 µg/Kg). These findings point to the necessity of more stringent monitoring of mycotoxins, particularly AFB1 in maize, as well as the value of regular assessment using LC-MS/MS.

Ultra-sensitive determination of Ochratoxin A in coffee and tea samples using a novel semi-automated in-syringe based coagulant-assisted fast mycotoxin extraction (FaMEx) technique coupled with UHPLC-MS/MS.

In this study, we demonstrated a novel semi-automated in-syringe-based coagulant-assisted liquid-liquid microextraction (IS-CGA-LLME) as fast mycotoxin extraction (FaMEx) technique coupled with ultra-high-performance liquid chromatography connected with a tandem-mass spectrometer (UHPLC-MS/MS) for the quantification of mycotoxin (Ochratoxin A, OT-A) in coffee and tea samples. IS-CGA-LLME is a three-step extraction process that includes extraction of OT-A from sample matrix using low-volume solvent extraction, then the extractant was cleaned-up using a coagulation process, and finally, the decolorized/matrix removed sample solution was processed for LLME for target analyte's pre-concentration. The final extractant was analyzed using UHPLC-MS/MS for OT-A quantification. Under the optimized experimental conditions, highly sensitive detection and quantification limits were obtained at 0.001 and 0.003ngg-1 for OT-A with excellent extraction recovery (93-111%) and precision <10%. These results proved that the developed method is a simple, highly sensitive, semi-automated, low-matrix effect and efficient procedure for the determination of mycotoxins in food samples.

Honey analysis in terms of nicotine, patulin and other mycotoxins contamination by UHPLC-ESI-MS/MS - method development and validation

Fifty-seven samples of honey of different types and origins were screened for nicotine and nine mycotoxins (aflatoxin B1, aflatoxin B2, fusarenon X, ochratoxin A, penicillic acid, zearalenone, sterigmatocystin, gliotoxin, and patulin). The sample set consisted of monofloral, multifloral, nectar, honeydrew, cream, and artificial honey originating mainly from Poland. The physicochemical characterization of honey was performed by determining colour (by Pfund method), water content (by refractometry), total phenolics and flavonoids content (by spectrophotometry). For nicotine and mycotoxins determination a QuEChERS-based UHPLC-ESI-MS/MS method was developed and validated. Analyses were carried out in alkaline conditions to ensure patulin-methanol adduct formation and facilitate this mycotoxin detection. About 33% of tested honey samples were contaminated by nicotine or/and mycotoxins. However, the presence of mycotoxins was not related to herein evaluated physicochemical parameters of honey samples.