Integrated Radiometric and Complementary Techniques for Mixed Contaminants and Residues in Foods

Closed for proposals

Project Type

Coordinated Research Project

Project Code

D52041

CRP

2169

Approved Date

12 December 2016

Status

Closed

Start Date

17 March 2017

Expected End Date

31 May 2023

Completed Date

30 August 2023

Participating Countries

Benin
Botswana
Chile
China
Colombia
Ecuador
Italy
Netherlands
North Macedonia
Pakistan
Papua New Guinea
Peru
South Africa
Spain
Uganda

Description

Risk management of contaminants in food and associated matrices such as water and feed is currently based on health risk assessments considering data from studies on individual hazards. However, humans are simultaneously exposed to a large number of contaminants/residues through consumption of food and drinking water (Alexander, et al., 2008) and therefore risk assessment should depend on data on mixed contaminants/residues. However, systematic programmes for monitoring a mixture of contaminants/ residues are still lacking in MSs and their laboratories lack analytical techniques to test such “cocktails” that are individually a food safety and therefore public health, and trade concern.  Use of agricultural inputs such as veterinary drugs and pesticides in food production is inevitable to many MSs due to rampant animal and plants diseases and pests that should be controlled to ensure food security. Residues of these inputs co-occur with incidental contaminants such as mycotoxins, persistent organic pollutants and harmful adulterants such as but not limited to melamine in milk powder and sudan-1 in chili-powder raising consumer concerns.  Open air agricultural production predisposes food commodities to different and possibly unsafe levels of contaminants/ residues and related toxicants. Crops and livestock alike are exposed to industrial and environmental effluents and air pollutants in addition to agrochemicals and naturally occurring toxins such as mycotoxins among others. Levels of air pollutants are increasing especially in urban and peri-urban farming systems worldwide and thus air pollutants are a major source of particulate contaminants that can accumulate to toxic levels in edible portions of plants/crops (Poole et al., 2003).  This implies that products from open environment production may contain a mixture of contaminants/ residues. Monitoring of mixed contaminants/residues is not practiced due to lack of necessary multi-class analytical methods. These hazards are numerous and their physico-chemical properties diverse. Food matrices also vary and are complex. Thus robust, sensitive/selective, precise and cost-effective multi-analyte/class techniques are necessary if the practice of controlling mixed contaminants/residues is to take effect among many FAO/IAEA MSs. Though challenging to laboratories, such techniques, if well researched, as proposed in this CRP with the leveraging the advantages of nuclear, isotopic and complementary techniques, should present numerous benefits such as: (1) ‘information-rich’ measurements covering different classes of residues, contaminants and possibly adulterants; (2) shorter sample preparation/analysis time; (3) high sample throughput; (4) less laboratory consumables. Therefore, the sooner research is done to address these challenges and exploit the benefits, the better it will be for public health and trade in MSs. Through the above mentioned research, this CRP aims at strengthening MS analytical laboratories and national chemical/natural residue monitoring programs thus contributing to the improvement of food safety, public health and where possible international trade. New multi-class analytical methods will be developed (including improved environmentally friendly sample preparation techniques) validated and transferred amongst MS laboratories. The CRP will also contribute to the knowledge-base on risk assessment regarding mixed contaminants as well as work on AMR, through development of some multi-antimicrobial analytical methods that will permit surveillance to ensure their prudent use by MSs 

Objectives

To enhance Member State food and environmental safety control systems and risk assessment programmes through improvement of laboratory capabilities needed to gather reliable data on mixed contaminants/residues in foods as well as antimicrobial use pertaining to the development of antimicrobial resistance

Specific objectives

To investigate the effective application of newly researched methods in the routine surveillance of mixed contaminants/residues in foods and where possible establishment of base/reference “fingerprints” of food matrices that may contain a mixture/cocktail of contaminants and/or residues

To research the development, optimization/adaptation, and validation of analytical methods for mixed contaminants/residues in foods and associated matrices

To research the development of innovative generic sample preparation techniques for mixed contaminants/residues in foods and associated matrices

To investigate the development, optimization/adaptation, validation and application of sensitive and selective multi-antimicrobial analytical methods useful for monitoring residues of substances associated with development of antimicrobial resistance

To investigate the effective application of newly researched methods in the routine surveillance of mixed contaminants/residues in foods and where possible establishment of base/reference “fingerprints” of food matrices that may contain a mixture/cocktail of contaminants and/or residues

To research the development, optimization/adaptation, and validation of analytical methods for mixed contaminants/residues in foods and associated matrices

To research the development of innovative generic sample preparation techniques for mixed contaminants/residues in foods and associated matrices

To investigate the development, optimization/adaptation, validation and application of sensitive and selective multi-antimicrobial analytical methods useful for monitoring residues of substances associated with development of antimicrobial resistance

Impact

Colombia: Four analytical methods were developed and validated. These are suitable for the determination of different classes of chemical hazards such as pesticides, veterinary drugs, mycotoxins, polychlorinated biphenyls, polyaromatic hydrocarbons in different food matrices. The scope of analysis increased from 200 compounds to 460 compounds from different groups which will result in better service-delivery to end users and increasing confidence in the institution’s analytical capabilities. Atrazine-d5, Fenthion D6, 13C g-HCH, Sufapiridina- (Phenyl-13C6), Sulfaquinoxaline (Phenyl-13C6) and flubendazole-d3 were used. Two PhD and six MScs benefited from the CRP. The CSI has initiated work on potential application of artificial intelligence in processing large analytical data.
North Macedonia: Four analytical methods were established enabling the CSI increase food safety testing capabilities. An isotopic confirmatory method for 49 veterinary drugs, organophosphate pesticides and mycotoxins was used to analyze imported and local samples of bovine meat. Another isotopic confirmatory method was established for 69 multiclass antimicrobials, anabolic hormones, lactones, ß-agonists, mycotoxins and organochlorine pesticides in bovine milk. Commercial milk samples were analysed with this method. A third isotopic confirmatory method was established for 72 multiclass antimicrobials, thyreostats, anabolic hormones, lactones, ß-agonists, mycotoxins and organochlorine pesticides in bovine urine. This work has benefited national residue testing for local needs, cutting back on outsourcing of tests; and in serving two neighboring countries, generating revenue. A stable-isotope-supported analytical method was established for residues of five antimicrobials in milk and waste after single dose administration to cows. A correlation was established between the presence of these antimicrobial residues in food and animal waste samples, and of antimicrobial resistance in intestinal microbiota, especially E. coli. More knowledge was gained on AMR testing such as the profiling of E. Coli resistance patterns in dairy cows. The project benefited 1 PhD and 1 MSc students.
Pakistan: Innovative cost-effective radioreceptor assay (RRA) technique using 14C- and 3H-labelled radiotracers for analysis of drug residues and mycotoxins was developed using inhouse receptors. RRA depends on commercial kits, whose procurement, shipping and delivery to end users is a challenge. Member States can produce receptors in-house cutting down the cost of kits. The receptors were packaged into commercial-like tablets and there are plans to scale up and share with other countries. Two MPhil students benefited from the CRP.
Ecuador : The CSI institute is responsible for regulating animal (including products) and plant health but it never had analytical methods to confirm chemical hazards in food before the CRP, let alone methods that can be used for mixed hazards but this has now changed. A method was established for testing residues of both veterinary drugs and pesticides in beef, pork and poultry meat under the country’s national monitoring programmes. Stable isotopes including atrazine-d5; enrofloxacin-d5; sulfamerazine-d4, clenbuterol-d9 and chloramphenical-d5 were used.
Peru: Two isotopic confirmatory analytical methods were developed and validated for testing multiple pesticide residues and mycotoxins in paprika and quinoa to support routine food safety control for agroexport or local consumption. Tebuconazole-d6 and dimethoate-d6; 13C-aflatoxin B1, 13C-deoxynivalenol, 13C-Fumonisin B1 and 13C-zearalenone were used. Peru’s agroexportation generates national revenue and creates jobs. In 2022 the exports accounted for 9807 US million dollar, with 102 and 94 US million attributed to paprika and quinoa, respectively. However, this is often affected by rejections at export destinations due to chemical contamination. In 2022, 37 notifications related to mycotoxins and/or pesticides in paprika were issued by EU. Similar concerns were reported about pesticides in quinoa. The CRP findings can help in redressing these challenges. One PhD student benefited from the CRP.
Chile: The stable-isotope dilution and related methodologies were developed and used for the determination of mycotoxins as well as antimicrobial and pesticide residues in broiler chicken droppings and litter. This is a non-invasive sampling method for collecting information on antimicrobial resistance. Residues and genes associated with antimicrobials tetracyclines and fluoroquinolones were detected suggesting release of both into the environment. Isotopic standards (6) used included: tetracycline-d6, enrofloxacin-d5 HCl, 13C6sulfamethazine-phenyl hemihydrate, chloramphenicol-d5, erythromycin-N-methyl-13C, d3 and hexaflumuron-d3. The CSI used the methods to analyze samples from the poultry industry. Samples from untreated birds contained enrofloxacin. The CSI provided guidance on avoiding or treating litter such from such birds. The institution is now part of the World Organization of Animal Health's collaborating centre for antimicrobial stewardship in aquaculture.
Botswana: Two methods validated will be used to enhance the implementation of the national residue monitoring programme and reduce analytical/subcontracting costs and turnaround time. Two PhD and 1 MSc students benefited from the project while the CSI also assisted two other PhD students from local universities. Stable isotope labelled compounds (16) used included tetracycline-d6, sufamethazine-d4, sulfapyridine-d4, lincomycin-d3, spiramycin-d3, enrofloxacin-d5, difloxacin-d5, xylazine-d6, mebendazole-d3, albendazole-d3, triclabendazole-d3, ceftiofur-d3, flunixin-d3, carbaryl-d7, 13C20-ochratoxin A, and 13C18-zearalenone.
China: Stable-isotope (e.g. enrofloxacin-d5, amantadine-d15, chloramphenicol-d5, florfenicol amine-d3, dexamethasone-d4 and 13C6-sulfaphenazole)-analytical methods were developed, validated and used for simultaneous determination of over 244 chemical contaminants/residues including veterinary drugs, mycotoxins and pesticides in eggs, chicken and milk. There are plans to transfer methods to other provinces for application. A database for 245 drugs and 323 pesticides established will facilitate synthesis of laboratory findings. One PhD and two MSc students were trained.
Papua New Guinea: The project enhanced capabilities of the National Agricultural Research Institute to analyze mixtures of chemical hazards in food. A multiresidue isotope-dilution LC-MS/MS method for simultaneous analysis of aflatoxin M1, ochratoxin A, deltamethrin, permethrin, cypermethrin, amitraz, amoxicillin, doramectin, eprinomectin and abamectin in milk was developed. Radioreceptor assay screening of residues/contaminants in milk was enhanced. Offshoot work included analysis of cadmium, lead, copper and zinc in rice by ICP-MS.
Uganda: Two isotope-based mass spectrometric methods were developed and validated for over 100 pesticide residues and mycotoxins in cereals (maize/maize products, rice, wheat/wheat products); and pesticide and mycotoxins in fruits and vegetables. The techniques will support routine testing by Uganda National Bureau of Standards. Twelve stable isotope-labelled compounds: 13C17-AFB1, 13C34-FB1, 13C15-deoxynivalenol, 13C20-OTA, atrazin-d5, dichlorvos-d6, diuron-d6, chlorpyrifos-d10, imidacloprid-d4, 13C6-carbaryl, deltamethrin (phenoxy)-d5, tebuconazole-d9, were used.
Benin: Isotopic-dilution LC-MS/MS method was developed for testing 17 chemicals including acrylamide, poly aromatic hydrocarbons and aflatoxins in roasted coffee, dry/smoked fish and infant formula. The method was successfully used in proficiency testing and will in future be useful for total diet studies to facilitate exposure assessment and risk management of chemical hazards.

Relevance

Safety of food remains a major concern to Members States and laboratories must play a central role. These laboratories need support with research and transfer of analytical methods and innovative solutions to challenges in testing.Nuclear/isotopic techniques as well as complementary techniques offer solutions. The CRP findings will help Member States improve performance of their laboratories and facilitate routine surveillance programmes to safeguard consumers and enhance trade. Normally laboratories use individual analytical methods to test different groups of chemical hazards such as mycotoxins, pesticides and veterinary drug residues. With the outputs of this CRP, now laboratories can use a single method to test groups of these hazards. This helps laboratories reduce the cost and time of analysis as well as resources in developing/validation of single-group methods. This also contributes to quick turnaround of test results.

Miniaturized sample preparation methods whose performance was enhanced using stable isotopes and involving low quantities of chemicals have a significant benefit to the laboratories. These will spend less resources on chemicals and discharge minimal amounts into the environment. Some of the inputs for such 'green' chemistry techniques are cheap and easily accessible.

The technology and approach used to produce receptors (in-house) to support radioreceptor biding assay and tested, are available for transfer to Member States. Their adoption of the protocol can enable laboratories reduce dependence on commercial receptors. This will also reduce analytical costs and time spent sourcing and procuring the receptors; promote innovation in research and testing laboratories to facilitate routine cost-effective testing and monitoring of a range of chemical hazards in food.

Some of the information and findings generated in the CRP are relevant to global efforts on combating antimicrobial resistance (AMR).

CRP Publications

Type

Conference proceedings

Year

2018

Description

Quantification of Chlortetracycline Residues and Determination of Antimicrobial Activity in Therapeutically Treated Broiler Chickens’ Dejections. VDRA, 8th International symposium on Hormone and Veterinary Drug Residue Analysis. Ghent, Belgium

Country/Organization

Chile

Type

Drafted and due for peer review

Year

For submission in 2020

Description

A new isotopic LC-MS/MS method for multiple residues/contaminants in bovine meat

Country/Organization

North Macedonia

Type

Conference proceedings

Year

2020

Description

Determination of mixed contaminants (mycotoxins, pesticides and veterinary) in food by green microextraction-Orbitrap HRMS; ASMS Conference on Mass Spectrometry and Allied Topics; abstract #304664

Country/Organization

South Africa

Type

Peer review

Year

2019

Publication URL

https://www.mdpi.com/1420-3049/23/6/1264

Description

Determination of Chlortetracycline Residues, Antimicrobial Activity and Presence of Resistance Genes in Droppings of Experimentally Treated Broiler Chickens

Country/Organization

Chile

Type

Peer review

Year

2019

Publication URL

https://pubmed.ncbi.nlm.nih.gov/30738613/

Description

A multianalyte, multi class method for residues in eggs

Country/Organization

China PR

Type

Conference proceedings

Year

2020

Description

Determination of mixed contaminants (mycotoxins, pesticides and veterinary) in food by green microextraction-Orbitrap HRMS; ASMS Conference on Mass Spectrometry and Allied Topics; abstract #304664

Country/Organization

South Africa

Type

Conference proceedings

Year

2020

Description

Determination of mixed contaminants (mycotoxins, pesticides and veterinary) in food by green microextraction-Orbitrap HRMS; ASMS Conference on Mass Spectrometry and Allied Topics; abstract #304664

Country/Organization

South Africa

Type

Peer reviewed

Year

2022

Publication URL

https://www.mdpi.com/2077-0472/12/6/869

Description

Multi-Residue Determination of 244 Chemical Contaminants in Chicken Eggs by Liquid Chromatography-Tandem Mass Spectrometry after Effective Lipid Clean-Up

Country/Organization

China PR

Type

Peer reviewed

Year

2023

Publication URL

https://onlinelibrary.wiley.com/doi/full/10.1002/fsn3.3568

Description

Ionic liquid-based dispersive liquid–liquid microextraction of anthelmintic drug residues in small-stock meat followed by LC-ESI-MS/MS detection

Country/Organization

Botswana

Type

Peer reviewed

Year

2022

Publication URL

https://doi.org/10.1016/j.foodchem.2021.130714

Description

Development and validation of qualitative screening, quantitative determination and post-targeted pesticide analysis in tropical fruits and vegetables by LC-HRMS

Country/Organization

Colombia

Type

Conference proceedings

Year

2021

Description

34th Latin American Congress of Chemistry in Cartagena de Indias, Colombia, 11-15 October 2021; Poster: Evaluación instrumental para la determinación de residuos de antibióticos en músculo e hígado de pollo por cromatografía líquida acoplada a espectrometría de masas de alta resolución-Orbitrap

Country/Organization

Colombia

Type

Peer reviewed

Year

2022

Publication URL

https://www.tandfonline.com/doi/abs/10.1080/03601234.2022.2120318

Description

Radiotracer studies to isolate in-house receptors from poultry liver for multi-chemical hazard analysis in selected food and feed

Country/Organization

Pakistan

Type

Conference proceedings

Year

2019

Description

Development, Validation and Application of Isotope Based Chromatographic/Spectrometric Techniques for Mixed Contaminants and Some Veterinary Drug Residues in Bovine Meat. Book of Abstracts. 8. National/2. International Veterinary Food Hygiene Congress 24-27th October 2019 Antalya, p.108

Country/Organization

North Macedonia

Type

Peer review

Year

2019

Publication URL

https://www.mdpi.com/1660-4601/16/1/24

Description

Assessment of Residues in poultry tissue and potential public health effects

Country/Organization

Chile

Type

Conference proceedings

Year

2018

Description

Validation of a methodology for determination of pesticides residues in Green coffee beans by Liquid Chromatography couple to High Resolution (Orbitrap) Mass Spectrometry”. 12th European Pesticide Residue Workshop, in Munich

Country/Organization

Colombia

Type

Conference proceedings

Year

2021

Description

Evaluation of the effect of OTC residue persistence on the selection of resistant bacteria in poultry by-products. XXVI PAN AMERICAN CONGRESS OF VETERINARY SCIENCES. 24-26 November 2021

Country/Organization

Chile

Type

Peer review

Year

2019

Publication URL

https://www.mdpi.com/1660-4601/16/1/24

Description

Assessment of Residues in poultry tissue and potential public health effects

Country/Organization

Chile

Type

Peer review

Year

2019

Publication URL

https://www.mdpi.com/1420-3049/23/6/1264

Description

Determination of veterinary drug Residues, Antimicrobial Activity and Presence of Resistance Genes

Country/Organization

Chile

Type

Peer review

Year

2019

Publication URL

https://pubmed.ncbi.nlm.nih.gov/30738613/

Description

A multianalyte, multi class method for residues in eggs

Country/Organization

China PR

Type

Peer reviewed

Year

2023

Publication URL

https://www.mdpi.com/2304-8158/12/13/2594

Description

Simultaneous Determination of Multiple Contaminants in Chicken Liver Using Dispersive Liquid-Liquid Microextraction (DLLME) Detected by LC-HRMS/MS

Country/Organization

South Africa

Type

Peer review

Year

2021

Publication URL

https://doi.org/10.1186/s13065-021-00788-5

Description

A new LC–MS/MS method for multiple residues/contaminants in bovine meat

Country/Organization

North Macedonia

Type

Peer reviewed

Year

2021

Publication URL

https://doi.org/10.1016/j.psj.2021.101313

Description

Determination of five antimicrobial families in droppings of therapeutically treated broiler chicken by high-performance liquid chromatography-tandem mass spectrometry

Country/Organization

Chile

Type

Peer reviewed

Year

2021

Publication URL

https://doi.org/10.3390/ani11051399

Description

Detection of Antimicrobial Residues in Poultry Litter: Monitoring a Risk through a Selective and Sensitive HPLC–MS/MS Method

Country/Organization

Chile

Type

Conference proceedings

Year

2020

Publication URL

https://www.eprw2020.com/wp-content/uploads/2020/03/eprw-2020-list-of-accepted-a…

Description

Simultaneous target and non-target screening method for pesticide residue analysis in tropical fruits and vegetables by liquid chromatography high resolution mass spectrometry-Orbitrap”. A poster presentation PD-50 at the 13th European Pesticide Residue Workshop, virtual in May 2020 where we presented the poster

Country/Organization

Colombia

Type

Conference proceedings

Year

2020

Description

Determination of mixed contaminants (mycotoxins, pesticides and veterinary) in food by green microextraction-Orbitrap HRMS; ASMS Conference on Mass Spectrometry and Allied Topics; abstract #304664

Country/Organization

South Africa

Type

Peer review

Year

2019

Publication URL

https://www.mdpi.com/1660-4601/16/1/24

Description

Assessment of Three Antimicrobial Residue Concentrations in Broiler Chicken Droppings as a Potential Risk Factor for Public Health and Environment

Country/Organization

Chile

Type

Drafted and due for peer review

Year

For submission in 2020

Description

A new isotopic LC-MS/MS method for multiple residues/contaminants in bovine meat

Country/Organization

North Macedonia

Type

Peer review

Year

2019

Publication URL

https://pubmed.ncbi.nlm.nih.gov/30738613/

Description

A multianalyte, multi class method for residues in eggs

Country/Organization

China PR

Type

Peer reviewed

Year

2023

Description

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

Country/Organization

North Macedonia

Type

Peer reviewed

Year

2021

Publication URL

https://pubmed.ncbi.nlm.nih.gov/33802994

Description

Evaluation of Antibiotic Dissemination into the Environment and Untreated Animals, by Analysis of Oxytetracycline in Poultry Droppings and Litter

Country/Organization

Chile

Type

Conference proceedings

Year

2022

Description

Multi-residue LC-MS/MS Method for Veterinary Drug Residues, Mycotoxins and Pesticides in Urine. Proceedings Book, 24-27.02.2022. pp.165-187, on-line, Oral presentation-invited lecturer

Country/Organization

North Macedonia

Type

China PR

Year

2022

Publication URL

https://pubmed.ncbi.nlm.nih.gov/35159483/

Description

Multiclass Comparative Analysis of Veterinary Drugs, Mycotoxins, and Pesticides in Bovine Milk by Ultrahigh-Performance Liquid Chromatography-Hybrid Quadrupole-Linear Ion Trap Mass Spectrometry

Type

Conference

Year

2022

Description

10. 14th EPRW in Bolognia, Italy, September 2022: Evaluation of two methodologies for the analysis of the mancozeb and propineb fungicide residues in fruits and vegetables

Country/Organization

Colombia

Type

Conference proceedings

Year

2021

Publication URL

https://www.laprw2021.com/programa

Description

Direct, sensitive and broad scope multiresidue analysis in water via SPE-HRMS” – Oral presentation at the 8th Latin American Pesticide residue workshop;

Country/Organization

Colombia

Type

Peer reviewed

Year

2022

Publication URL

https://doi.org/10.2478/jvetres-2022-0027

Description

Determination of veterinary drug residues, mycotoxins and pesticide residues in bovine milk by liquid chromatography electrospray ionization–tandem mass spectrometry

Country/Organization

North Macedonia

Type

Peer reviewed

Year

2020

Publication URL

https://doi.org/10.1007/s42452-020-03361-2

Description

Development and validation of confirmatory LC–MS/MS method for multi-residue analysis of antimicrobial drugs in bovine milk

Country/Organization

North Macedonia

Type

Peer review

Year

2019

Publication URL

https://www.mdpi.com/1420-3049/23/6/1264

Description

Determination of veterinary drug Residues, Antimicrobial Activity and Presence of Resistance Genes

Country/Organization

Chile

Type

Conference proceedings

Year

2019

Description

Dallos, J. A. G., Huérfano, I. M. "Screening methods for determination of pesticides residues in fruits and vegetables using LC-High Resolution Mass Spectrometry- Orbitrap”. 7th Latin American pesticide residue workshop, Foz do Iguazu

Country/Organization

Colombia

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