With continued global population expansion, food production will have to increase with crops prot... more With continued global population expansion, food production will have to increase with crops protected against the growing menace of pests, requiring the increased use of pesticides globally to ensure that agricultural production is optimised and remains economically viable. The aim of this systematic review was to perform an in-depth analysis of pesticide legislation, focusing on rice, to understand the gaps that exist in the harmonisation across different countries. Tricyclazole, carbendazim, thiamethoxam and acephate were considered as these received the highest numbers of RASFF notifications and alerts due to their presence in rice. Global differences in regulations cause trade issues, especially when developing countries use unauthorised pesticides or different MRLs. Discrepancies in the registration and regulation of sales were found to be a global problem. Sales of pesticides and resulting residues in developing countries that are banned in the EU or US is highly concerning. ...
During 2019 a series of food poisoning events and deaths occurred in Uganda due to an unknown cau... more During 2019 a series of food poisoning events and deaths occurred in Uganda due to an unknown causative agent. In response the World Food Programme (WFP) initiated investigations into the incidents which included contacting expert laboratories to analyse the main suspect product known as Super Cereal. The laboratories used a broad gamut of their testing capabilities to determine the cause of the incidents. This included targeted and non-targeted methodologies such as LC-MS/MS, QToF-MS and spectroscopic techniques coupled to chemometrics. The conclusion of the investigation was that the cause of the food poisoning was due to the presence of the Tropane alkaloids, atropine and scopolamine, in the Super Cereal. These alkaloids were found to be present due to the incorporation of Datura seeds during production of the Super Cereal. Furthermore, the data generated showed all outbreaks were caused by a single batch of the Super Cereal.
In the past decade, several major food safety crises originated from problems with feed. Conseque... more In the past decade, several major food safety crises originated from problems with feed. Consequently, there is an urgent need for early detection of fraudulent adulteration and contamination in the feed chain. Strategies are presented for two specific cases, viz. adulterations of (i) soybean meal with melamine and other types of adulterants/contaminants and (ii) vegetable oils with mineral oil, transformer oil or other oils. These strategies comprise screening at the feed mill or port of entry with non-destructive spectroscopic methods (NIRS and Raman), followed by post-screening and confirmation in the laboratory with MS-based methods. The spectroscopic techniques are suitable for on-site and on-line applications. Currently they are suited to detect fraudulent adulteration at relatively high levels but not to detect low level contamination. The potential use of the strategies for non-targeted analysis is demonstrated.
ABSTRACT Tetrodotoxin (tetrodotoxin) is a potent neurotoxin, which shuts down electrical signalin... more ABSTRACT Tetrodotoxin (tetrodotoxin) is a potent neurotoxin, which shuts down electrical signaling in nerves by blocking the voltage-gated sodium channel proteins in nerve cell membranes. It was originally discovered in puffer fish but is found in a range of animal species and thought to be produced by bacteria. The toxin can be lethal to humans being 10 000 times more potent than cyanide. Human fatalities have been attributed to the ingestion of this toxin through consumption of puffer fish, a delicacy in Japan and other regions, and other marine species. The effects of tetrodotoxin poisoning onset quickly and include shortness of breath, numbness, tingling, light-headedness, paralysis, and irregular heartbeat. Treatment usually consists of respiratory assistance as no antidote has been developed. The accepted method of analysis for tetrodotoxin is the mouse bioassay, although recently more ethical assays have been developed including high performance liquid chromatography, biosensor and enzyme-linked immunosorbant assay.
Refined vegetable oils are widely used in the food industry as ingredients or components in many ... more Refined vegetable oils are widely used in the food industry as ingredients or components in many processed food products in the form of oil blends. To date, the generic term 'vegetable oil' has been used in the labelling of food containing oil blends. With the introduction of new EU Regulation for Food Information (1169/2011) due to take effect in 2014, the oil species used must be clearly identified on the package and there is a need for development of fit for purpose methodology for industry and regulators alike to verify the oil species present in a product. The available methodologies that may be employed to authenticate the botanical origin of a vegetable oil admixture were reviewed and evaluated. The majority of the sources however, described techniques applied to crude vegetable oils such as olive oil due to the lack of refined vegetable oil focused studies. Nevertheless, DNA based typing methods and stable isotopes procedures were found not suitable for this particular purpose due to several issues. Only a small number of specific chromatographic and spectroscopic fingerprinting methods in either targeted or untargeted mode were found to be applicable in potentially providing a solution to this complex authenticity problem. Applied as a single method in isolation, these techniques would be able to give limited information on the oils identity as signals obtained for various oil types may well be overlapping. Therefore, more complex and combined approaches are likely to be needed to identify the oil species present in oil blends employing a stepwise approach in combination with advanced chemometrics. Options to provide such a methodology are outlined in the current study.
Chili powder is a globally traded commodity which has been found to be adulterated with Sudan dye... more Chili powder is a globally traded commodity which has been found to be adulterated with Sudan dyes from 2003 onwards. In this study, chili powders were adulterated with varying quantities of Sudan I dye (0.1e5%) and spectra were generated using near infrared reflectance spectroscopy (NIRS) and Raman spectroscopy (on a spectrometer with a sample compartment modified as part of the study). Chemometrics were applied to the spectral data to produce quantitative and qualitative calibration models and prediction statistics. For the quantitative models coefficients of determination (R 2) were found to be 0.891e0.994 depending on which spectral data (NIRS/Raman) was processed, the mathematical algorithm used and the data pre-processing applied. The corresponding values for the root mean square error of calibration (RMSEC) and root mean square error of prediction (RMSEP) were found to be 0.208e0.851% and 0.141e0.831% respectively, once again depending on the spectral data and the chemometric treatment applied to the data. Indications are that the NIR spectroscopy based models are superior to the models produced from Raman spectral data based on a comparison of the values of the chemometric parameters. The limit of detection (LOD) based on analysis of 20 blank chili powders against each calibration model gave 0.25% and 0.88% for the NIR and Raman data, respectively. In addition, adopting a qualitative approach with the spectral data and applying PCA or PLS-DA, it was possible to discriminate between adulterated chili powders from non-adulterated chili powders.
Pantothenic acid (PA), vitamin B 5 , is an essential B vitamin that may be fortified in food and ... more Pantothenic acid (PA), vitamin B 5 , is an essential B vitamin that may be fortified in food and as such requires robust and accurate methods of detection to meet compliance legislation. This study reports the production and characterisation of the first monoclonal antibody (MAb) specific for PA and the subsequent development of a surface plasmon resonance (SPR) biosensor assay for the quantification of PA. The developed assay was compared with an SPR based commercial kit which utilised a polyclonal antibody (PAb). Foodstuffs, including cereals (n = 43), infant formulas and baby food (n = 10) and fruit juices (n = 48) were analysed by both the MAb and PAb biosensor assays and comparison plots showed good correlation (R 2 0.77-0.99). The results indicate that the MAb based biosensor assay is suitable for the measurement of PA in foodstuffs and has the added advantage of facilitating a constant, long term supply of identical antibody. Preliminary matrix studies suggest the MAb based assay is an excellent candidate for further validation studies and routine quality assurance based analysis.
Basic vegetable blends (BVB's) and soya oils, used in the animal feed industry, are sometimes adu... more Basic vegetable blends (BVB's) and soya oils, used in the animal feed industry, are sometimes adulterated with transformer and mineral oil as a means of illegally increasing profit. A set of BVB's and soya oil samples adulterated with transformer oil and mineral oil were characterised using both NIRS and Raman spectroscopy. Applying chemometrics to the NIRS and Raman spectral data, very good calibration and prediction statistics were obtained for transformer and mineral oils. Using NIRS, R 2 values greater than 0.99 were obtained with corresponding values for root mean squared error of calibration and prediction (<0.57 and <0.55, respectively). Using Raman, R 2 values greater than 0.97 were obtained with the root mean squared error of calibration (<2.01) and prediction (<1.92) calculated. Furthermore, using a qualitative approach it was possible, using PCA, to discriminate between 100% soya and BVB. This study demonstrates that both NIRS and Raman technology can be successfully applied as rapid screening techniques for the detection of oil adulteration and fraud in the food and feed industry.
The illegal adulteration of milk with melamine in 2008 in China led to adverse kidney and urinary... more The illegal adulteration of milk with melamine in 2008 in China led to adverse kidney and urinary tract effects in hundreds of thousands of children and the reported deaths of six. The milk had been deliberately adulterated to elevate the apparent protein content, and subsequently melamine was detected in many milk-related products which had been exported. This led to the banning of imports of milk and milk products from China intended for the nutritional use of children and to the implementation of analytical methods to test products containing milk products. An optical biosensor inhibition immunoassay has been developed as a rapid and robust method for the analysis of infant formula and infant liquid milk samples. A compound with a chemical structure similar to that of melamine was employed as a hapten to raise a polyclonal antibody and as the immobilized antigen on the surface of a biosensor chip. The sensitivity of the assay, given as an IC(50), was calculated to be 67.9 ng mL(-1) in buffer. The antibody did not cross-react with any of the byproducts of melamine manufacture; however, significant cross-reactivity was observed with the insecticide cyromazine of which melamine is a metabolite. When sample matrix was applied to the assay, a limit of detection of &amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;lt;0.5 μg mL(-1) was determined in both infant formula and infant liquid milk. The development of the immunoassay and validation data for the detection of melamine is presented together with the results obtained following the analysis of melamine-contaminated milk powder.
The performance of three near-infrared spectroscopy (NIRS) instruments was compared through the i... more The performance of three near-infrared spectroscopy (NIRS) instruments was compared through the investigation of coriander seed authenticity. The Thermo Fisher iS50 NIRS benchtop instrument, the portable Ocean Insights Flame-NIR and the Consumer Physics handheld SCiO device were assessed in conjunction with chemometric modelling in order to determine their predictive capabilities and use as quantitative tools through regression analysis. Two hundred authentic coriander seed samples and ninety adulterated samples were analysed on each device. Prediction models were developed and validated using SIMCA 15 chemometric software. All instruments correctly predicted 100% of the adulterated samples. The best models resulted in correct predictions of 100%, 98.5% and 95.6% for authentic coriander samples using spectra from the iS50, Flame-NIR and SCiO, respectively. The development of regression models highlighted the limitations of the Flame-NIR and SCiO for quantitative analysis, compared t...
With continued global population expansion, food production will have to increase with crops prot... more With continued global population expansion, food production will have to increase with crops protected against the growing menace of pests, requiring the increased use of pesticides globally to ensure that agricultural production is optimised and remains economically viable. The aim of this systematic review was to perform an in-depth analysis of pesticide legislation, focusing on rice, to understand the gaps that exist in the harmonisation across different countries. Tricyclazole, carbendazim, thiamethoxam and acephate were considered as these received the highest numbers of RASFF notifications and alerts due to their presence in rice. Global differences in regulations cause trade issues, especially when developing countries use unauthorised pesticides or different MRLs. Discrepancies in the registration and regulation of sales were found to be a global problem. Sales of pesticides and resulting residues in developing countries that are banned in the EU or US is highly concerning. ...
During 2019 a series of food poisoning events and deaths occurred in Uganda due to an unknown cau... more During 2019 a series of food poisoning events and deaths occurred in Uganda due to an unknown causative agent. In response the World Food Programme (WFP) initiated investigations into the incidents which included contacting expert laboratories to analyse the main suspect product known as Super Cereal. The laboratories used a broad gamut of their testing capabilities to determine the cause of the incidents. This included targeted and non-targeted methodologies such as LC-MS/MS, QToF-MS and spectroscopic techniques coupled to chemometrics. The conclusion of the investigation was that the cause of the food poisoning was due to the presence of the Tropane alkaloids, atropine and scopolamine, in the Super Cereal. These alkaloids were found to be present due to the incorporation of Datura seeds during production of the Super Cereal. Furthermore, the data generated showed all outbreaks were caused by a single batch of the Super Cereal.
In the past decade, several major food safety crises originated from problems with feed. Conseque... more In the past decade, several major food safety crises originated from problems with feed. Consequently, there is an urgent need for early detection of fraudulent adulteration and contamination in the feed chain. Strategies are presented for two specific cases, viz. adulterations of (i) soybean meal with melamine and other types of adulterants/contaminants and (ii) vegetable oils with mineral oil, transformer oil or other oils. These strategies comprise screening at the feed mill or port of entry with non-destructive spectroscopic methods (NIRS and Raman), followed by post-screening and confirmation in the laboratory with MS-based methods. The spectroscopic techniques are suitable for on-site and on-line applications. Currently they are suited to detect fraudulent adulteration at relatively high levels but not to detect low level contamination. The potential use of the strategies for non-targeted analysis is demonstrated.
ABSTRACT Tetrodotoxin (tetrodotoxin) is a potent neurotoxin, which shuts down electrical signalin... more ABSTRACT Tetrodotoxin (tetrodotoxin) is a potent neurotoxin, which shuts down electrical signaling in nerves by blocking the voltage-gated sodium channel proteins in nerve cell membranes. It was originally discovered in puffer fish but is found in a range of animal species and thought to be produced by bacteria. The toxin can be lethal to humans being 10 000 times more potent than cyanide. Human fatalities have been attributed to the ingestion of this toxin through consumption of puffer fish, a delicacy in Japan and other regions, and other marine species. The effects of tetrodotoxin poisoning onset quickly and include shortness of breath, numbness, tingling, light-headedness, paralysis, and irregular heartbeat. Treatment usually consists of respiratory assistance as no antidote has been developed. The accepted method of analysis for tetrodotoxin is the mouse bioassay, although recently more ethical assays have been developed including high performance liquid chromatography, biosensor and enzyme-linked immunosorbant assay.
Refined vegetable oils are widely used in the food industry as ingredients or components in many ... more Refined vegetable oils are widely used in the food industry as ingredients or components in many processed food products in the form of oil blends. To date, the generic term 'vegetable oil' has been used in the labelling of food containing oil blends. With the introduction of new EU Regulation for Food Information (1169/2011) due to take effect in 2014, the oil species used must be clearly identified on the package and there is a need for development of fit for purpose methodology for industry and regulators alike to verify the oil species present in a product. The available methodologies that may be employed to authenticate the botanical origin of a vegetable oil admixture were reviewed and evaluated. The majority of the sources however, described techniques applied to crude vegetable oils such as olive oil due to the lack of refined vegetable oil focused studies. Nevertheless, DNA based typing methods and stable isotopes procedures were found not suitable for this particular purpose due to several issues. Only a small number of specific chromatographic and spectroscopic fingerprinting methods in either targeted or untargeted mode were found to be applicable in potentially providing a solution to this complex authenticity problem. Applied as a single method in isolation, these techniques would be able to give limited information on the oils identity as signals obtained for various oil types may well be overlapping. Therefore, more complex and combined approaches are likely to be needed to identify the oil species present in oil blends employing a stepwise approach in combination with advanced chemometrics. Options to provide such a methodology are outlined in the current study.
Chili powder is a globally traded commodity which has been found to be adulterated with Sudan dye... more Chili powder is a globally traded commodity which has been found to be adulterated with Sudan dyes from 2003 onwards. In this study, chili powders were adulterated with varying quantities of Sudan I dye (0.1e5%) and spectra were generated using near infrared reflectance spectroscopy (NIRS) and Raman spectroscopy (on a spectrometer with a sample compartment modified as part of the study). Chemometrics were applied to the spectral data to produce quantitative and qualitative calibration models and prediction statistics. For the quantitative models coefficients of determination (R 2) were found to be 0.891e0.994 depending on which spectral data (NIRS/Raman) was processed, the mathematical algorithm used and the data pre-processing applied. The corresponding values for the root mean square error of calibration (RMSEC) and root mean square error of prediction (RMSEP) were found to be 0.208e0.851% and 0.141e0.831% respectively, once again depending on the spectral data and the chemometric treatment applied to the data. Indications are that the NIR spectroscopy based models are superior to the models produced from Raman spectral data based on a comparison of the values of the chemometric parameters. The limit of detection (LOD) based on analysis of 20 blank chili powders against each calibration model gave 0.25% and 0.88% for the NIR and Raman data, respectively. In addition, adopting a qualitative approach with the spectral data and applying PCA or PLS-DA, it was possible to discriminate between adulterated chili powders from non-adulterated chili powders.
Pantothenic acid (PA), vitamin B 5 , is an essential B vitamin that may be fortified in food and ... more Pantothenic acid (PA), vitamin B 5 , is an essential B vitamin that may be fortified in food and as such requires robust and accurate methods of detection to meet compliance legislation. This study reports the production and characterisation of the first monoclonal antibody (MAb) specific for PA and the subsequent development of a surface plasmon resonance (SPR) biosensor assay for the quantification of PA. The developed assay was compared with an SPR based commercial kit which utilised a polyclonal antibody (PAb). Foodstuffs, including cereals (n = 43), infant formulas and baby food (n = 10) and fruit juices (n = 48) were analysed by both the MAb and PAb biosensor assays and comparison plots showed good correlation (R 2 0.77-0.99). The results indicate that the MAb based biosensor assay is suitable for the measurement of PA in foodstuffs and has the added advantage of facilitating a constant, long term supply of identical antibody. Preliminary matrix studies suggest the MAb based assay is an excellent candidate for further validation studies and routine quality assurance based analysis.
Basic vegetable blends (BVB's) and soya oils, used in the animal feed industry, are sometimes adu... more Basic vegetable blends (BVB's) and soya oils, used in the animal feed industry, are sometimes adulterated with transformer and mineral oil as a means of illegally increasing profit. A set of BVB's and soya oil samples adulterated with transformer oil and mineral oil were characterised using both NIRS and Raman spectroscopy. Applying chemometrics to the NIRS and Raman spectral data, very good calibration and prediction statistics were obtained for transformer and mineral oils. Using NIRS, R 2 values greater than 0.99 were obtained with corresponding values for root mean squared error of calibration and prediction (<0.57 and <0.55, respectively). Using Raman, R 2 values greater than 0.97 were obtained with the root mean squared error of calibration (<2.01) and prediction (<1.92) calculated. Furthermore, using a qualitative approach it was possible, using PCA, to discriminate between 100% soya and BVB. This study demonstrates that both NIRS and Raman technology can be successfully applied as rapid screening techniques for the detection of oil adulteration and fraud in the food and feed industry.
The illegal adulteration of milk with melamine in 2008 in China led to adverse kidney and urinary... more The illegal adulteration of milk with melamine in 2008 in China led to adverse kidney and urinary tract effects in hundreds of thousands of children and the reported deaths of six. The milk had been deliberately adulterated to elevate the apparent protein content, and subsequently melamine was detected in many milk-related products which had been exported. This led to the banning of imports of milk and milk products from China intended for the nutritional use of children and to the implementation of analytical methods to test products containing milk products. An optical biosensor inhibition immunoassay has been developed as a rapid and robust method for the analysis of infant formula and infant liquid milk samples. A compound with a chemical structure similar to that of melamine was employed as a hapten to raise a polyclonal antibody and as the immobilized antigen on the surface of a biosensor chip. The sensitivity of the assay, given as an IC(50), was calculated to be 67.9 ng mL(-1) in buffer. The antibody did not cross-react with any of the byproducts of melamine manufacture; however, significant cross-reactivity was observed with the insecticide cyromazine of which melamine is a metabolite. When sample matrix was applied to the assay, a limit of detection of &amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;lt;0.5 μg mL(-1) was determined in both infant formula and infant liquid milk. The development of the immunoassay and validation data for the detection of melamine is presented together with the results obtained following the analysis of melamine-contaminated milk powder.
The performance of three near-infrared spectroscopy (NIRS) instruments was compared through the i... more The performance of three near-infrared spectroscopy (NIRS) instruments was compared through the investigation of coriander seed authenticity. The Thermo Fisher iS50 NIRS benchtop instrument, the portable Ocean Insights Flame-NIR and the Consumer Physics handheld SCiO device were assessed in conjunction with chemometric modelling in order to determine their predictive capabilities and use as quantitative tools through regression analysis. Two hundred authentic coriander seed samples and ninety adulterated samples were analysed on each device. Prediction models were developed and validated using SIMCA 15 chemometric software. All instruments correctly predicted 100% of the adulterated samples. The best models resulted in correct predictions of 100%, 98.5% and 95.6% for authentic coriander samples using spectra from the iS50, Flame-NIR and SCiO, respectively. The development of regression models highlighted the limitations of the Flame-NIR and SCiO for quantitative analysis, compared t...
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