Chemical Constituents and Antioxidant Potential of Red Guava (Psidium cattleianum Sabine) from Southern Brazil in Different Edible Ripening Stages.

Ripening and growing location are important factors that can impact fruit quality characteristics. In this study, the influence of these factors on physicochemical characteristics, carbohydrates, aliphatic organic acids, phenolic compounds, and antioxidant capacity of red guava (Psidium cattleianum Sabine) was evaluated. Fruit ripening increased fructose and glucose (up to 22.83 and 16.42 g 100 g- 1 dry matter (DM), respectively), and decreased citric acid, the major organic acid (up to 135.35 mg g- 1 DM). Ripening and growing location also influenced the concentration of phenolic compounds and antioxidant capacity of red guava, in which a dependency between both factors was observed in most cases. Apigenin, galangin, isoquercitrin, among other phenolic compounds were quantified for the first time in red guava, in which isoquercitrin was the major (up to 13409.81 mg kg- 1 DM). The antioxidant potential of red guava was also confirmed by ferric reducing antioxidant power assay (up to 82.63 µmol Fe+ 2 g- 1 DM), Folin-Ciocalteu reducing capacity assay (up to 17.79 mg gallic acid equivalent g- 1 DM), and DPPH free radical scavenging assay (up to 25.36 mg ascorbic acid equivalent g- 1 DM). These results especially demonstrated the bioactive potential of red guava and provided knowledge regarding the influence of ripening and growing location on chemical and bioactive components encouraging its industrial exploitation.

Phenolic compounds profile of optimised green and eco-friendly extracts of Eugenia pyriformis leaves: an alternative for antioxidant and antibacterial applications.

The Eugenia pyriformis Cambess (uvaia) is a well-known source of bioactive compounds. This study investigated the efficiency of Ultrasound-Assisted Extraction (UAE) and Enzyme-Assisted Extraction (EAE) in obtaining uvaia leaf extracts with high antioxidant and antibacterial activity. In a first step, different variables of the leaves were employed to define the best conditions for obtaining the extract with the highest total phenolic content. In a second step, the optimised extracts were characterised. In total, twenty-four phenolic compounds were identified through LC-ESI-MS/MS. The EAE in optimised conditions showed a higher amount of total phenolic compounds and antioxidant potential. It was possible to note an analogous potential of antibacterial activity of the extracts, which showed action mainly against Gram-positive bacteria. These findings suggest that the aqueous extracts of uvaia leaves are feasible, economic, and sustainable alternatives for adding value to uvaia leaves, which are an agricultural residue that is generally underutilised.

Integrated analysis of marine biotoxins and contaminants of emerging concern in bivalve mollusks from Santa Catarina, Brazil.

Santa Catarina is the main producer state of oysters and mussels in Brazil, reaching 98 % of national production. To assure the safety of bivalve mollusks production, control programs of marine biotoxins (MBs) have been continuously performed. Herein, the co-occurrence of MBs and contaminants of emerging concern (CECs) in oyster and mussels from the main production sites of Santa Catarina was reported, covering 178 compounds. Samples of wild and non-cultivated oysters and mussels were also assessed. Chemometric tools were used to evaluate and optimize several sample preparation techniques such as solid-liquid, ultrasound assisted, and pressurized liquid extraction. The optimized protocol was based on ultrasound assisted extraction followed by liquid chromatography coupled to tandem mass spectrometry. The results showed the incidence of several CECs and MBs. In the case of MBs, all results were below the regulatory limits for both cultivated and non-cultivated samples. Wild mollusks have shown a higher number of compounds. Regarding CECs, the more frequent compounds were caffeine, diclofenac, meloxicam, and sertraline. Domoic acid and okadaic acid were the main toxins detected. The results highlighted the need of monitoring for MBs and the potential of oyster and mussels as sentinel organisms to risk analysis of CECs in coastal regions. To the best of our knowledge, this is the first method to describe a simultaneous sample preparation and analysis of CECs and MBs in bivalve mollusks, as well as the first report of meloxicam and florfenicol in mussels and oysters.

Sample pooling and incurred samples improve analytical throughput and quality control of lipophilic phycotoxins screening in bivalve mollusks.

Lipophilic marine biotoxins (LMBs) are one of the main risks associated with the consumption of mussels and oysters. Sanitary and analytical control programs are developed to detect the occurrence of these toxins in seafood before they reach toxic levels. To ensure quick results, methods must be easy and fast to perform. In this work, we demonstrated that incurred samples were a viable alternative to validation and internal quality control studies for the analysis of LMBs in bivalve mollusks. These samples were used to optimize, validate, and monitor a simple and fast ultrasound-assisted extraction (UAE) procedure. An internal quality control material containing okadaic acid (227 ± 46 µg kg-1) was produced and characterized. This material had its homogeneity and stability verified and was included as a quality control in all batches of analytical routine. Besides, a sample pooling protocol for extracts analysis was developed, based on tests for COVID-19. Up to 10 samples could be analyzed simultaneously, reducing the instrumental time of analysis by up to 80%. The UAE and sample pooling approaches were then applied to more than 450 samples, of which at least 100 were positive for the okadaic acid group of toxins.

Antioxidant effect of blueberry flour on the digestibility and storage of Bologna-type mortadella.

The aim of the study was to add blueberry flour (BF) to Bologna-type mortadella as a natural antioxidant and to evaluate its activity during in vitro digestion and refrigerated storage. Five treatments of mortadella were prepared: without antioxidant, with sodium erythorbate and with the addition of three levels of BF: 0.05 %, 0.075 % and 0.1 %. Twenty-three phenolic compounds were quantified in blueberry fruits and twenty-eight in BF, with prevalence of chlorogenic acid. The presence of BF did not affect the proximal composition of the mortadella, but it had a small effect on pH, hardness (texture profile) and instrumental color, as well as reduced lipid oxidation during refrigerated storage (2-8 °C) for 90 days. During in vitro digestion, the addition of BF increased the content of total phenolic compounds and the antioxidant activity of mortadella (p < 0.05), among all simulated stages. At a concentration of 0.05 %, BF can be used as a synthetic antioxidant substitute in Bologna-type mortadella, enhancing the use of blueberry fruits in the form of flour and enriching the product with natural antioxidants.

Goldenberry flour as a natural antioxidant in Bologna-type mortadella during refrigerated storage and in vitro digestion.

Goldenberry is rich in phenolic compounds; however, no study has been carried out to assess its potential in meat products. The objective of the research was to characterize goldenberry (Physalis peruviana) fruits and flour and investigate its effect on the quality of Bologna-type mortadella, before and after in vitro digestion. Five treatments were performed: without antioxidant, with sodium erythorbate, and with three levels of goldenberry flour. The phenolic profile analysed by LC-MS/MS quantified 10 compounds in the fruit and 23 in the flour. Goldenberry flour did not affect the centesimal composition of the mortadella, but it had an effect on pH, hardness (texture profile) and color, as well as reduced lipid oxidation (peroxide value and TBARS) for 90 days. There was also an increase (P < 0.05) in the antioxidant activity and in the content of phenolic compounds after in vitro digestion. Thus, goldenberry flour can be used as a natural antioxidant to replace sodium erythorbate in Bologna-type mortadella.

Spatial-temporal occurrence of contaminants of emerging concern in urban rivers in southern Brazil.

The widespread use and misuse of antibiotics and pesticides has been linked with several risks to the environment and human health. In the present report, the results of the monitoring of 64 pharmaceuticals and 134 pesticides occurrence in an urban river in Southern Brazil are presented and discussed. Sampling campaigns have covered the period 2016-2018. The identification and determination of the analytes were achieved by high-resolution mass spectrometry. The data were analyzed using chemometric tools to obtain spatial-temporal models. Toxicological evaluation was achieved using acute toxicity (zebrafish standardized protocol), and determination of risk quotient. Within the 198 analytes included in the targeted analysis method for surface water, 33 were identified in an urban river during 2 years of monitoring, being 20 pharmaceuticals and 13 pesticides. Using high-resolution mass spectrometry, a suspect screening approach was established in an un-target analysis. The evaluation was carried out using a data bank built from consumption data of drugs and pesticides, in the metropolitan region of Porto Alegre - RS and their respective metabolites. The suspect screening analysis done with a data bank with more than 1450 compounds results in 27 suspect findings. The target analysis results showed a continuous prevalence of non-steroidal anti-inflammatories, analgesics, antipyretics, beta-blockers, corticoids, and antibiotics. Regarding the pesticides, the main classes were fungicides, especially those from triazol and strobilurin classes.

Determination of amino acid content, fatty acid profiles, and phenolic compounds in non-conventional edible fruits of seven species of palm trees (Arecaceae) native to the southern half of South America.

The fruits of palm trees (Arecaceae) are a very important food source for fauna and for humans, despite the still incipient role of these fruits in conventional diet. Seven palm tree species (plus one variety) that are native to the southern half of South America located east of the Andes (Argentina, Paraguay, Uruguay, and the southern states of Brazil) were studied. For the first time, the fatty acid profiles of palm seeds and the content of both amino acids and phenolic compounds present in the pulp (yellowish fleshy mesocarps) of the fruits were determined. High-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was used to screen and quantify thirty-two phenols and HPLC was used to determine the amino acid contents and fatty acids profiles of the species. Twenty-five percent of the fatty acids in the seeds of B. lallemantii, Butia odorata (var. pulposa), B. witeckii, and Syagrus romanzoffiana were found to be unsaturated. One species (B. lallemantii) had a high and well-balanced amino acid content (28,900 mg/kg), while six species (B. odorata, B. catarinensis, B. witeckii, Euterpe edulis, and Syagrus romanzoffiana) contained more than 14,000 mg/kg of amino acids. A high content of the phenolic compounds ferulic acid, luteolin, quercetin-3-rutinoside, isoquercetin, and isorhamnetin were found in many species, most notably in B. odorata, B. catarinensis, and B. witeckii.

Phenolic compounds profile and main nutrients parameters of two underestimated non-conventional edible plants: Pereskia aculeata Mill. (ora-pro-nóbis) and Vitex megapotamica (Spreng.) Moldenke (tarumã) fruits.

Non-conventional edible plants are widely present in Brazil. Several fruits of spontaneous occurrence are underestimated and scarcely used by the population. The increase in the knowledge about these plants, especially regarding the bioactive compounds present in this species, is important to increase its use, cultivation, and propagation. Ora-pro-nóbis (Pereskia aculeata) and tarumã (Vitex megapotamica) fruits are two examples. In the present report, the phenolic compounds profile was determined, using liquid chromatography coupled to tandem mass spectrometry (UHPLC-ESI-MS/MS). Other assays were also performed such as protein content, fat, humidity, and calcium. The results show that tarumã fruits are rich in several phenolic compounds, especially p-coumaric acid (9.3-61.8 mg g-1), isoquercitrin (14.6-55.5 mg g-1), naringenin (7.5-30.1 mg g-1), and caffeic acid (12.7-18.3 mg g-1). Ora-pro-nóbis fruits have showed high contents of caffeic acid (4.9 mg kg-1), rutin (3.9 mg kg-1), and hesperidin (1.7 mg kg-1), and their seeds, specifically, have showed relevant content for galangin (1.1 mg kg-1) and ferulic acid (0.3 mg kg-1).

Simultaneous extraction/derivatization for the analysis of sulfite by capillary electrophoresis: A high-throughput reference method to meet the demand of seafood inspection.

Sulfite is widely used to prevent enzymatic browning in shrimp and lobster processing. However, sulfite may cause allergy in sensitive consumers. Thus, regulatory agencies set limits for its use. Sulfite is usually controlled by the normalized Monier-Williams (MW) titrimetric method that allows a limited number of samples to be analyzed. This manuscript consolidates an innovative method for sulfite inspection in seafood by capillary zone electrophoresis with diode array detector (CZE-DAD). A simple, fast, and simultaneous extraction and derivatization method was developed to provide high throughput for analytical routine. The high instability of the sulfite was suppressed by its derivatization with formaldehyde producing hydroxymethylsulfonate. The evaluation of its analytical performance yielded excellent results in compliance with the strict parameters required for metrological accreditation. The CZE-DAD method was selective and specific when submitted to confirmatory evaluations by liquid chromatography coupled to mass spectrometry. The limit of detection (3.50 mg kg-1), limit of quantitation (11.7 mg kg-1) and recoveries (99-103%) were adequate for sample analysis. The measurement uncertainty was estimated by the propagation of errors and experimental standard uncertainties (precision, accuracy, and analytical curves) and type B uncertainties from traceable measurement instruments. The low relative uncertainty (10%) and the adequate reproducibility demonstrated method suitability. The CZE-DAD results were compared to the MW method through the respective expanded standard uncertainties and normalized error. This new method is promising to be used in seafood inspection and continuous laboratory evaluations using instrumentation not very expensive to acquire and maintain.

Reference LC-MS/MS method to detect fresh cheeses adulteration with whey.

This study evaluated the potential of a reference method to detect fresh cheeses adulteration with whey by liquid chromatography coupled to mass spectrometry (LC-MS/MS). Qualitative results were expressed as presence or absence of the marker peptide TPEVDDEALEK, obtained by tryptic hydrolysis of ß-lactoglobulin. Sample preparation was based on defatting with cold acetone and protein solubilization in ammonium bicarbonate and urea buffer (pH = 8.0). Reversed phase liquid chromatography used a C18 column for separation of the analyte, whose retention time was 4.12 min. Mass spectrometry was carried out with positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode for the precursor ion (m/z 624) and the quantitation (m/z 573) and confirmation transitions (m/z 820; m/z 920) of the peptide. Method validation was carried out in quantitative terms, to set the baseline concentration of the marker peptide in 69 authentic samples, and in qualitative terms, to set the action level that distinguish authentic from adulterated cheeses (350 mg kg-1). Sensitivity was enough to detect cheeses with 10% adulteration and the detection limit was set to 21 mg kg-1. The simple extraction procedure allowed high-throughput analysis of 33 real samples. Results were compared to SDS-PAGE electrophoresis, whose limitations for accurate quantitation were easily overcome by LC-MS/MS. The developed method ensured precision, accuracy, sensitivity, and specificity needed for the unequivocal detection of non-compliant cheeses made with cow or buffalo milk, without dealing with the highly toxic chemical species required for SDS-PAGE. This method can be extended in the future to detect similar adulterations in fresh cheeses prepared with milk from other animal species, as well as in other dairy products.

Disasters with oil spills in the oceans: Impacts on food safety and analytical control methods.

More than 5.8 million tonnes of oil have been spilled into the oceans. Some oil disasters marked history, causing multiple social and economic consequences in addition to catastrophic environmental impacts. Recently, Brazil and Mauritius faced oil disasters that have severely impacted seafood sanitary credibility. One of the components of the oil composition are the polycyclic aromatic hydrocarbons (PAH), which are the main contamination markers of petrogenic origin. There is enough evidence to correlate the intake of food contaminated with PAH with increased risks of developing cancer. The set PAH4, composed of benzo[a]anthracene, benzo[a]pyrene, benzo[b]fluoranthene, and chrysene, and the set PAH8, composed of benzo[a]anthracene, benzo[a]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[ghi]perylene, chrysene, dibenzo[a,h]anthracene, and indeno[1,2,3-cd]pyrene are recognized as markers of food chemical contamination. After oil disasters in the oceans, the risk to the health of seafood consumers tends to be of special concern, Countries like the European Union set maximum levels for benzo[a]pyrene (5 µg kg-1) and PAH4 (30 µg kg-1) in bivalve mollusks. Levels of concern established by countries that have faced oil disasters are given special attention in this review. Laboratory analysis of PAH in food samples is very challenging because it deals with quite different kinds of matrices. Furthermore, analytical results are usually related to the closure or reopening of cultivated areas and fishing points. Therefore, the progress of the analytical methods for PAH in seafood is covered in detail. Chemical laboratory measurements provide essential data to assess the potential risks to human health due to consumption of seafood contaminated with PAH. The main human health risk assessment approaches in a seafood contamination scenario with PAH are reviewed and discussed, providing an insightful and guiding tool to each step of the risk assessment framework.

Cassava-based materials for matrix solid phase dispersion: An alternative for sample preparation in food analysis.

Cassava-based food ingredients were evaluated as candidate materials to be used as matrix solid phase dispersion (MSPD) for sample preparation. Cassava starch, tapioca, and tapioca pearls (TP) were applied in MSPD sample preparation of several food matrices such as mussels, fish, cooked ham, sausages, and animal feed (laying mash) for the determination of pharmaceuticals, preservatives, and polycyclic aromatic hydrocarbons by liquid chromatography coupled to tandem mass spectrometry or capillary electrophoresis. The performance of the new cassava-based solid phases was compared to other materials, such as diatomaceous earth, cellulose, cork powder, and a commercial polymer (Q-matrix® Hydra). The following parameters were used to select the most appropriate solid phases for each assay: fat removal, accuracy for certified reference material analysis, interferents presence in blank samples extract, signal to noise ratio, signal enhancement, and signal suppression. Best results were observed for cassava starch, except for nitrite and nitrate analysis, where the use of cellulose have led to the best sample preparation performance. Electronic microscopy of the materials and the mixture matrix and solid phase confirmed the adequate dispersion of the matrix on cassava starch. In conclusion, cassava-based solid phases were suitable for MSPD, allowing cheaper, greener, and abundant alternatives to sample preparation.

Residues of antibiotics in yeasts from ethanol production: a possible contamination route for feedingstuffs.

Sugarcane yeast and brewer's yeast from ethanol production are widely used as ingredients of animal feed formulations in Brazil. To avoid the contamination of the must in ethanol production refineries, the use of antibiotics is one of the main preventive treatments. Thus, there is a risk of antibiotic residues carry over from yeast to animal feed. This unintentional addition of antibiotics can produce non-compliant feed products, due to regulatory aspects and their toxicity for animals. The results of an exploratory program to assess the occurrence of over 60 antibiotics and other pharmaceuticals in 27 sugarcane yeast and brewer's yeast samples were described. Monensin was present in seven samples with concentrations ranging from 0.47 to 263.5 mg kg-1. Other antibiotics quantitated were virginiamycin (2.25 mg kg-1) and amprolium (0.25 mg kg-1). Monensin in sugarcane yeast may represent a risk for further feeds production, especially for those products intended for sensible species such as equines and rabbits, for which monensin has toxic effects.

Analysis of sulfonamide residues in bovine liver by liquid chromatography- tandem mass spectrometry without chemical extraction or clean-up procedures.

A new procedure for direct extraction and analysis of sulfonamides residues in bovine liver was developed. Briefly, an amount of homogenized sample was mixed with sand and incubated in an ultrasonic bath to promote tissue disruption. After, samples are centrifuged in an empty cartridge with a fritted glass filter. The filtrate was diluted with acetonitrile to precipitate proteins and centrifuged again. The final supernatant was diluted with HPLC mobile phase (ammonium acetate 10 mM: methanol, 85:15) and analyzed with a LC-MS/MS system with electrospray ionization in positive mode. Six sulfonamides were studied, and the procedure showed good recoveries values for all analytes, except for sulfamethoxazole and sulfaquinoxaline. Sulfapirydine was used as internal standard. Consumption of organic solvents was restricted to 2 mL of acetonitrile per sample.

Determination of 62 veterinary drugs in feedingstuffs by novel pressurized liquid extraction methods and LC-MS/MS.

A fast and simple method for the determination of 62 veterinary drugs in feedingstuffs was developed, optimized, validated, and applied to real samples. Sample preparation was based on a pressurized liquid extraction method using a hard cap coffee machine, which was compared to a commercial pressurized liquid extraction system. Extraction was performed with diatomaceous earth, acetonitrile (20%), and formic acid (0.1%). A central composite design was used to optimize the composition of the extraction solvent. The extracts were analyzed using two chromatographic modes (reversed phase with C18 and HILIC). Analytical limits were set to 25 (limit of detection) and 75 µg kg-1 (limit of quantitation). For banned substances, a salting-out step was included, achieving LOQ lower as 1 µg kg-1 for ractopamine. Other figures of merit such as precision, trueness, decision limit (CCα), method capability (CCß), matrix effects, stability, recovery, and measurement uncertainty were also reported for analytical validation. The method was successfully applied to hundreds of real samples demonstrating its fitness-for-purpose for the analysis of sulfonamides, tetracyclines, fluoroquinolones, avermectins, quinolones, beta-agonists, beta-lactams, amphenicols, benzimidazoles, coccidiostats, lincosamides, macrolides, nitrofurans, quinoxalines, melamine, and trimethoprim.

Presence of antibiotic resistance genes and its association with antibiotic occurrence in Dilúvio River in southern Brazil.

It is known that antibiotics are widely used in human and veterinary medicine. In some countries the use is controlled, however few restrictions to their use are enforced in many countries. Antibiotics and their metabolites can reach the water bodies through sewage systems, especially in those countries with partial or absent wastewater treatment systems. The overuse and misuse of antibiotics has been linked with the increase of antibiotic resistant bacteria. The relation between the occurrence of antibiotics and resistance genes in surface waters has been widely studied worldwide evincing the great importance of this subject. In this work, a methodology for quantification of 40 antibiotics of 5 different classes, in river water, by SPE-LC-MS/MS was validated. Samples were taken during a two-year period from Dilúvio River, a stream that crosses the city of Porto Alegre (RS - Brazil) and receives in nature domestic effluent. The methodology met the requirements of validation, with Limit of Quantification varying from 20 ng L-1 to 100 ng L-1. A total of 48 samples was analyzed for the presence of antibiotics for two years. From the 40 antibiotics analyzed, 8 of them (Azithromycin, Cephalexin, ciprofloxacin, clindamycin, norfloxacin, sulfadiazine, sulfamethoxazole and trimethoprim) were present in all sampling points in the range of

Assessing the mutagens ethylnitrolic acid and 2-methyl-1,4-dinitro-pyrrole in meat products: Sample preparation and simultaneous analysis by LC-MS/MS.

The simultaneous use of nitrite and sorbate as preservatives in meat products may produce mutagenic compounds such as the ethylnitrolic acid and 2-methyl-1,4-dinitro-pyrrole. We developed a sensitive analytical method with high metrological reliability. After assessing several extraction approaches and chromatographic separation modes, a modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) approach was chosen for sample preparation, which were analyzed by reversed-phase liquid chromatography (with C18 as stationary phase) coupled to tandem mass spectrometry. After validation, we confirmed that this method is fit-for-purpose, since it was applied to the analysis of several meat products. Limits of detection were set from 5 to 20 µg kg-1. Satisfactory results were obtained for both compounds, such as precision (CV > 20%) and recoveries (77-92%). This method determine these carcinogenic compounds in processed meats, contributing to the preservation of public health and the improvement of food regulation and control.

Efficiency of a low-cost pyramid-shaped solar still for pesticide removal from highly contaminated water.

Water pollution by pesticides and other chemical contaminants is a subject of major importance due to the risk for human health and the environment. The search for remediation processes able to withdraw chemical contaminants from water and to allows water reuse is an urgent need. Herein, a simple and cheap system for pesticides removal was constructed and evaluated using water samples contaminated with two widely used herbicides (imazapic and imazethapyr, at g L-1 level). Operation parameters and process efficiency, in terms of removal rate in the reclaimed water and degradation rate of pesticides in the dry residue, were quantitatively determined. The model was tested in real-world field experiments and was able to remove more than 99.95% of both contaminants from a 10 L solution containing 4.16 ±â€¯0.94 g of imazethapyr and 1.31 ±â€¯0.17 g of imazapic, generating reusable water with minimum volume loss (<2.5%). Liquid chromatography coupled to mass spectrometry was used to determine the herbicides content in all samples and to estimate the degree of degradation of the substances as well as the occurrence of transformation products of imazapic and imazethapyr. The system efficiency in removing contaminants of emerging concern from surface water was also evaluated. The process have generated output water with undetected levels for two fungicides present in a local river in Southern Brazil.

Cost-Effective and High-Reliability Analytical Approach for Multitoxin Screening in Bivalve Mollusks by Liquid Chromatography Coupled to Tandem Mass Spectrometry.

A fast, less expensive, analytical approach with high metrologic reliability was developed to assist an official program for 21 marine biotoxins, monitoring in bivalve mollusks. The simultaneous analysis of lipophilic and hydrophilic marine biotoxins was achieved using a sample preparation protocol based on solid-liquid extraction and low-temperature cleanup, followed by liquid chromatography coupled to tandem mass spectrometry. Samples were extracted with acidified methanol/water (90:10), followed by low-temperature cleanup. Chromatographic separation was obtained using a cyano-bonded silica phase. The mobile phase was composed of water and acetonitrile, with both 0.1% formic acid and 2.5 mmol L-1 ammonium formate. Electrospray ionization was used in both negative and positive modes. The single-laboratory validation approach enabled method performance assessment, and the necessary data to design a model for result expression were yielded. With this purpose, a systematic study of errors and uncertainties was performed. This new analytical approach aimed to minimize the use of highly expensive analytical standards, promoting economic viability to be applied by high-throughput routine laboratories. After its implementation on the Brazilian official monitoring program, positive results near the regulatory limits were obtained, demonstrating the fit for purpose of the method as a surveillance tool.