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Showing papers in "Journal of AOAC International in 2019"


Journal ArticleDOI
TL;DR: This paper aims to give a reliable overview of the chemical classification of natural polyphenols, which can be simply classified into flavonoids and non-flavonoids, or be subdivided in many sub-classes depending on the number of phenol units within their molecular structure, substituent groups, and/or the linkage type between Phenol units.
Abstract: Background: Polyphenols are natural compounds synthesized exclusively by plants with chemical features related to phenolic substances and eliciting strong antioxidants properties. Objective: The aim of this paper is to give a reliable overview of the chemical classification of natural polyphenols. Methods: Literature survey was done through google scholar, pubmed and scopus search engine. Results and Discussion: These molecules or classes of natural substances are characterized by two phenyl rings at least and one or more hydroxyl substituents. This description comprehends a large number of heterogeneous compounds with reference to their complexity. Therefore, polyphenols can be simply classified into flavonoids and non-flavonoids, or be subdivided in many sub-classes depending on the number of phenol units within their molecular structure, substituent groups, and/or the linkage type between phenol units. Polyphenols are widely distributed in plant tissues where they mainly exist in form of glycosides or aglycones. The structural diversity of flavonoid molecules arises from variations in hydroxylation pattern and oxidation state resulting in a wide range of compounds: flavanols, anthocyanidins, anthocyanins, isoflavones, flavones, flavonols, flavanones, and flavanonols.

201 citations


Journal ArticleDOI
TL;DR: This review highlights potential health benefits of commonly used spices and herbs such as chili pepper, cinnamon, ginger, black pepper, turmeric, fenugreek, rosemary, and garlic.
Abstract: Spices and herbs have been in use for centuries both for culinary and medicinal purposes. Spices not only enhance the flavor, aroma, and color of food and beverages, but they can also protect from acute and chronic diseases. More Americans are considering the use of spices and herbs for medicinal and therapeutic/remedy use, especially for various chronic conditions. There is now ample evidence that spices and herbs possess antioxidant, anti-inflammatory, antitumorigenic, anticarcinogenic, and glucose- and cholesterol-lowering activities as well as properties that affect cognition and mood. Research over the past decade has reported on the diverse range of health properties that they possess via their bioactive constituents, including sulfur-containing compounds, tannins, alkaloids, phenolic diterpenes, and vitamins, especially flavonoids and polyphenols. Spices and herbs such as clove, rosemary, sage, oregano, and cinnamon are excellent sources of antioxidants with their high content of phenolic compounds. It is evident that frequent consumption of spicy foods was also linked to a lower risk of death from cancer and ischemic heart and respiratory system diseases. However, the actual role of spices and herbs in the maintenance of health, specifically with regards to protecting against the development of chronic, noncommunicable diseases, is currently unclear. This review highlights potential health benefits of commonly used spices and herbs such as chili pepper, cinnamon, ginger, black pepper, turmeric, fenugreek, rosemary, and garlic.

130 citations


Journal ArticleDOI
TL;DR: The history of cannabis, its pharmacology, and its medical uses are provided and there is evidence of efficacy in the symptomatic treatment of nausea and vomiting, pain, insomnia, post-traumatic stress disorder, anxiety, loss of appetite, Tourette's syndrome, and epilepsy.
Abstract: Cannabis has been used as a medicinal plant for thousands of years. As a result of centuries of breeding and selection, there are now over 700 varieties of cannabis that contain hundreds of compounds, including cannabinoids and terpenes. Cannabinoids are fatty compounds that are the main biological active constituents of cannabis. Terpenes are volatile compounds that occur in many plants and have distinct odors. Cannabinoids exert their effect on the body by binding to receptors, specifically cannabinoid receptors types 1 and 2. These receptors, together with endogenous cannabinoids and the systems for synthesis, transport, and degradation, are called the Endocannabinoid System. The two most prevalent and commonly known cannabinoids in the cannabis plant are delta-9-tetrahydrocannabinol (THC) and cannabidiol. The speed, strength, and type of effects of cannabis vary based on the route of administration. THC is rapidly distributed through the body to fatty tissues like the brain and is metabolized by the cytochrome P450 system to 11-hydroxy-THC, which is also psychoactive. Cannabis and cannabinoids have been indicated for several medical conditions. There is evidence of efficacy in the symptomatic treatment of nausea and vomiting, pain, insomnia, post-traumatic stress disorder, anxiety, loss of appetite, Tourette's syndrome, and epilepsy. Cannabis has also been associated with treatment for glaucoma, Huntington's Disease, Parkinson's Disease, and dystonia, but there is not good evidence to support its efficacy. Side effects of cannabis include psychosis and anxiety, which can be severe. Here, we provided a summary of the history of cannabis, its pharmacology, and its medical uses.

67 citations


Journal ArticleDOI
TL;DR: Main classes of phenols from plant foods, their role as dietary components, and an overview on analytical methods for their extraction from food matrices, their separation, detection and quantification are presented.
Abstract: Background: In the last few decades, the media has been overwhelming the consumer with various dietary requirements that some of which lead to no avail. On the other hand, the Mediterranean diet, which stems from a very ancient lore, stands as one of the most effective diets whose conspicuous and positive results are still impacting the lives of many Mediterranean locals. The "Mediterranean Diet" is an umbrella term that is used to denote a plethora of natural ingredients used in the culinary tradition of the region, and which comprises but is not limited to olive oil, cereals, wine, fruits, dried fruits, and spices. MD components are known for being rich in antioxidant compounds. Polyphenols belong to the category of antioxidants that occur in the above-mentioned Mediterranean foods. Objective: The current review aims at presenting main classes of phenols from plant foods, their role as dietary components, and an overview on analytical methods for their extraction from food matrices, their separation, detection and quantification. Conclusions: The discrimination of phenols is not an easy matter, and several methods are described in the literature, mainly chromatographic methods, which are herein reviewed. In short, phenols are mainly found in vegetable foods in which the Mediterranean Diet is rich. The health effects of some phenols and analytical methods are herein revised. Highlights: Phenols or Phenolics is a designation corresponding to compounds that have one or more hydroxyl groups attached to a 6-carbon aromatic ring. Phenols in foods occur mainly as secondary metabolites of vegetables, often found in polymeric forms (polyphenols). Phenols from foods are mainly simple phenols (e.g., caffeic acid), flavonoids, the most varied and ubiquitous class (e.g., catechin, quercetin), stilbenes (resveratrol), lignans, and tannins. In addition to the wide range of polyphenols present in foods, the compounds are quantitatively and qualitatively distributed in a heterogenous way in the different compartments of the food matrix. This structural and compartmental diversity leads to an important variability of the physicochemical properties impacting otherwise the extraction of phenols. Total phenols are determined by the Folin Cioucalteau method, as described in European Pharmacopeaea.

59 citations


Journal ArticleDOI
TL;DR: The role of spices and herbs in human life, adulteration of the commonly consumed herbs and herbs, identification of their adulterants, as well as the most popular analytical techniques and methods used in their detection are covered, including spectroscopic, chromatographic, electronic sensing, and deoxyribonucleic acid-based methodologies.
Abstract: Background: Spices and aromatic herbs have long been used by people to impart sensory appetizing elements, including aroma, flavor, and color, to foods and beverages in an effort to enhance their palatability. Herbs and spices exhibit a plethora of medicinal properties including antimicrobial and antioxidant properties. Spices serve as natural preservatives to delay food spoilage and extend shelf life. As spice trading has exponentially increased globally, herbs and spices have become prone to adulteration, which can be deliberate or unintentional. Deliberate adulteration is usually economically motivated, aimed at maximizing profit margins, whereas unintentional adulteration is often attributed to improper harvesting or processing of the plant material or collecting/substituting closely related species. Adulteration of herbs or spices with toxic ingredients such as Sudan dyes or metal salts (e.g., lead chromate) may result in serious public health consequences. Objective: To provide a concise account of ongoing adulteration issues with spices and herbs in order to enhance general awareness of the short- and longer-term implications of such fraud. Method: Last twenty-years of literature on various aspects of spice adulteration including text books and online resources were gathered and compiled. In addition, a number of original reports have been published prior to year 2000 that are directly associated with adulteration of commonly traded herbs and spices were also included. Results: The current review covers the role of spices and herbs in human life, adulteration of the commonly consumed spices and herbs, identification of their adulterants, as well as the most popular analytical techniques and methods used in their detection, including spectroscopic, chromatographic, electronic sensing, and deoxyribonucleic acid-based methodologies. Conclusions: Spices and herbs, being high-priced commodities, have been often subjected to adulteration in many ways which reduces their quality and potentially has harmful health implications. Adulteration is attributed primarily to increased demand or supply shortage of the spices and aromatic herbs. The motivation for spice fraud is largely attributed to economical interest to gain greater profit margins and such adulteration of spices can have serious implications for public health. To combat the adulteration of spices and herbs effectively, a range of analytical techniques across many different technologies have been developed. These techniques are expected to aid in the detection of adulterants and establish quantifiable concentrations for the compounds in question in various matrices, including spices and aromatic herbs.

42 citations


Journal ArticleDOI
TL;DR: A method for measurement of total dietary fiber (TDF) has been validated and addresses each of the issues identified by analysts in using that method over the past 8 years.
Abstract: A method for measurement of total dietary fiber (TDF) has been validated. This method is applicable to plant materials, foods, and food ingredients as consumed, consistent with the 2009 CODEX definition (ALINORM 09/32/REP), and measures insoluble dietary fiber (IDF) and soluble dietary fiber (SDF), comprising SDF that precipitates in the presence of 78% ethanol (SDFP) and SDF that remains soluble in the presence of 78% ethanol (SDFS). The method is an update of AOAC Method 2009.01 and addresses each of the issues identified by analysts in using that method over the past 8 years. A total of 13 laboratories participated in the study, with all laboratories returning valid assay data for most of the 16 test portions (8 blind duplicates) consisting of samples with a range of content of traditional dietary fibers, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 6.90 to 60.37 g/100 g. TDF was calculated as the sum of IDF plus SDFP measured gravimetrically and SDFS measured by HPLC. The repeatability SD ranged from 0.27 to 0.76 g/100 g, and the reproducibility SD ranged from 0.54 to 3.99 g/100 g. The RSDr ranged from 1.22 to 6.52%, and the RSDR ranged from 2.14 to 10.62%.

39 citations


Journal ArticleDOI
Mathieu Dubois1, Anna-Maria Empl1, Greg Jaudzems1, Quentin Baslé1, Erik J M Konings1 
TL;DR: A single-laboratory validation method for the direct determination of 2- and 3-MCPD and indirect determination of glycidyl esters in infant and adult/pediatric nutritional formulas by GC coupled to MS met the Standard Method Performance Requirements (SMPR) set by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals.
Abstract: Background: Monochloropropanediol (MCPD) and its fatty acid esters as well as glycidyl fatty acid esters are substances generated during oil refining or food processing. The free form released during digestion, 3-MCPD and glycidol, have shown adverse effects in animal studies. Objective: So far, the available analytical methods have not been validated in a collaborative study for infant and adult nutritional formulas. This manuscript describes a single-laboratory validation method in view of a future multilaboratory validation trial. Methods: The method described is for the direct determination of 2- and 3-MCPD and indirect determination of 2- and 3-MCPD esters and glycidyl esters in infant and adult/pediatric nutritional formulas by GC coupled to MS. Results: The analytical range was found to be 4-2000 μg/kg powder formula and 0.7-333 μg/kg liquid formula for fatty acid esters of MCPD and glycidol, and 2.5-750 μg/kg samples for free MCPD. The recovery rates were within 91-124% for all samples. Repeatability precision was <20% at levels close to the LOQ. Conclusions: The results met the Standard Method Performance Requirements® (SMPR) set by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals. Highlights: The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2018.03.

33 citations


Journal ArticleDOI
TL;DR: The presented UA-IL-DLLME method is simple, low in cost, environmentally friendly, rapid, and sensitive and requires minimal use of toxic organic solvents.
Abstract: Background: A rapid and new ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction method (UA-IL-DLLME) was presented for the determination of curcumin by spectrophotometry. Objective: To determine trace levels of curcumin in food samples by using green and low-cost method development. Methods: 1-Butyl-3-methylimidazolium hexafluorophosphate was used to extract curcumin from sample solutions with the aid of sonication. Optimum extraction efficiency was determined by examining extraction solvents, pH, centrifugation speed, time, sonication period, and temperature. The influences of diverse ions on the recovery of curcumin were examined. The concentration of curcumin in the final solution was measured by spectrophotometer at 425 nm. Results: The enrichment factor achieved was 167. The LOD and the RSD were 0.51 μg/L and 4.3%, respectively. The presented method was performed to detect curcumin in 20 food samples. Conclusions: The presented UA-IL-DLLME method is simple, low in cost, environmentally friendly, rapid, and sensitive and requires minimal use of toxic organic solvents. Highlights: A microextraction method was applied to increase sensitivity. Higher enrichment factors and lower detection limits were observed. The proposed technique is easy, cost-effective, accurate, and precise.

29 citations


Journal ArticleDOI
TL;DR: The popularity of dairy as the source for polyphenol fortified beverages in the diet will be dictated by optimization of the technology for maximizing the bioavailability of the antioxidants.
Abstract: Dairy-based functional beverages have been a growing segment as consumer demands for health foods have shifted focus from simply enhancing lifespan to protecting health. Green tea is often limited in use because of poor bioavailability and disagreeable taste. However, milk is considered an ideal platform for the delivery of active polyphenolic compounds in green tea. Furthermore, the antioxidant enzymatic activity and antioxidant index of polyphenols in green tea have been known to be protected through interaction with dairy proteins inside the unstable intestinal environment. In addition, consumption of green tea infused with milk has been found to have a significant impact on reducing skin wrinkles and roughness in elderly subjects, through a decrease in lipid peroxidation and a concomitant reduction in oxidative stress. A similar affinity has been observed between antioxidants in coffee and milk proteins. Dark chocolate has been known to contain significant phenolic content and antioxidant activity. The activation of protein complex NF-κB, which is responsible for cell survival, was found to be significantly reduced upon consumption of cocoa with water, whereas consuming cocoa with milk had no effect on the bioavailability of the phenolic compounds in cocoa. The popularity of dairy as the source for polyphenol fortified beverages in the diet will be dictated by optimization of the technology for maximizing the bioavailability of the antioxidants.

28 citations


Journal ArticleDOI
TL;DR: Phenolic compounds exert different biological functions, such as antioxidant activity, modulation of detoxifying enzymes, stimulation of the immune system, reduction of platelet aggregation, modulation and reduction of blood pressure, and anti-inflammatory, antibacterial, antiviral, and antifungal activities.
Abstract: Background: The interest in phenolic compounds present in foods of vegetable origin has shown a notable increase in recent decades. This interest is due to the growing number of scientific studies concerning their beneficial role in human health. The interest in polyphenols has been supported by the current and growing awareness, and attention of consumers to food from a food safety viewpoint and also because of the beneficial effects ascribed to polyphenols. Objective: The aim of this article is to highlight antibacterial, antifungal, and anti-inflammatory activities of various phenolic compounds normally found in certain foods. Conclusions: Phenolic compounds exert different biological functions, such as antioxidant activity, modulation of detoxifying enzymes, stimulation of the immune system, reduction of platelet aggregation, modulation of hormonal metabolism, reduction of blood pressure, and anti-inflammatory, antibacterial, antiviral, and antifungal activities.

25 citations


Journal ArticleDOI
TL;DR: The CF procedure should be abandoned as it fails to quantify fiber properly and detergent analyses quantify IDF, and TDF methods quantify both IDF and SDF.
Abstract: Background: Because of its chemical complexity, the estimation of dietary fiber content of feed and food materials is a difficult analytical challenge. Three major fiber analyses are conducted routinely in the United States including crude fiber (CF), detergent fiber, and total dietary fiber (TDF). Objective: Factors crucial to the successful measurement of dietary fibers are described and suggestions provided as to how to overcome potential analytical problems within assays. Methods: An accounting of methodological details that result in variation in fiber concentration values is presented along with suggestions as to how to decrease the variation. Results: CF analysis remains in use in the livestock feed and pet food industries for nutrition labeling purposes in spite of the fact that the analysis does not separate mammalian enzyme-digestible from indigestible carbohydrate components, and values obtained are usually 30-50% of the actual dietary fiber concentration. Detergent fiber methods quantify the insoluble dietary fibers (IDF) accurately, but not the soluble dietary fiber (SDF) components. TDF methods account for intrinsic and intact fibers, isolated and extracted fibers, and synthetic fibers found in feed and food ingredients and complete diet matrixes. Conclusions: The CF procedure should be abandoned as it fails to quantify fiber properly. Detergent analyses quantify IDF. TDF methods quantify both IDF and SDF. Highlights: Accurate dietary fiber quantification is essential given the role of fiber in health and well-being of animals and humans.

Journal ArticleDOI
TL;DR: Different extraction and clean-up protocols, based on either the dispersive solid-phase extraction (d-SPE) and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach, were optimized and compared for the determination of selected bisphenols such as BPA and BPS in breast milk samples.
Abstract: Different extraction and clean-up protocols, based on either the dispersive solid-phase extraction (d-SPE) and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach, were optimized and compared for the determination of selected bisphenols such as bisphenol A (BPA) and bisphenol S (BPS) in breast milk samples. QuEChERS-based sample preparation procedure was optimized by evaluation of different clean-up sorbents including zirconium-based sorbents (Z-Sep and Z-Sep Plus) and primary secondary amine. Negligible matrix interference was observed for most of the analytes due to application of 45 mg Z-Sep or 45 mg Z-Sep + 5 mg Z-Sep Plus sorbents in d-SPE clean-up step. Acceptable analytical performance for the BPA and BPS was observed with recoveries percentage in the range of 70-92% and RSD less than 15%. The pilot study was performed by applying HPLC with diode-array detection, and optimized procedures were transferred to the LC triple-quadrupole MS system. LC with electrospray ionization and tandem MS operating in the multiple reaction monitoring mode provide high sensitivity and selectivity for trace analysis. The LODs were 0.10 and 0.54 ng/mL, and the LOQs were 0.20 and 1.35 ng/mL for BPS and BPA, respectively. The developed procedures were evaluated in terms for material collection obtained from women (inhabitants of Lublin, Poland). In 20 samples, bisphenol residues were detected at concentrations from 0.09 to 11.56 ng/mL.

Journal ArticleDOI
TL;DR: The ThRAll project aims to support the application of risk-based approaches to food-allergen management through the development of common protocols for collection and curation of data that will be applied to allergenic foods for which there are currently data gaps.
Abstract: Risk-based approaches to managing allergens in foods are being developed by the food industry and regulatory authorities to support food-allergic consumers to avoid ingestion of their problem food, especially in relation to the traces of unintended allergens. The application of such approaches requires access to good quality data from clinical studies to support identification of levels of allergens in foods that are generally safe for most food-allergic consumers as well as analytical tools that are able to quantify allergenic food protein. The ThRAll project aims to support the application of risk-based approaches to food-allergen management in two ways. First, a harmonized quantitative MS-based prototype reference method will be developed for the detection of multiple food allergens in standardized incurred food matrices. This will be undertaken for cow's milk, hen's egg, peanut, soybean, hazelnut, and almond incurred into two highly processed food matrices, chocolate and broth powder. This activity is complemented by a second objective to support the development and curation of data on oral food challenges, which are used to define thresholds and minimum eliciting doses. This will be achieved through the development of common protocols for collection and curation of data that will be applied to allergenic foods for which there are currently data gaps.


Journal ArticleDOI
TL;DR: The study showed that the FDA EAM method performed satisfactorily as a standard method for extractible elemental analysis of food.
Abstract: Background: An interlaboratory study was conducted to test U.S. Food and Drug Administration (FDA) Elemental Analysis Manual (EAM) Method 4.7, "Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave Assisted Digestion." Objective: The goal of the study was to demonstrate the performance of FDA EAM Method 4.7. Methods: Fourteen laboratories participated in the collaborative study, including nine Food Emergency Response Network state laboratories and five federal FDA laboratories. Laboratories tested 8 labeled standard reference materials and 12 blinded foods: mayonnaise, dark chocolate, sunflower seeds, hamburger with cheese, brown rice flour (blinded reference material included as a test food), infant formula, canned smoked oysters, sardines in tomato paste, swordfish, mineral water, cinnamon, and a multivitamin. The blinded test foods represented every sector of the AOAC food triangle. Participants measured the mass fraction of each element in each sample in triplicate. Results: Horwitz Ratio (HorRat) values were better than 1.5 for all As, Cd, Cu, Hg, Mo, Ni, Pb, and Se measurements when at least eight laboratories reported results greater than LOQ. The HorRat values were better than 1.5 for all Mn and Zn measurements except for the multivitamin and for all Cr measurements except for sunflower seeds, in which the nonhomogeneity was identified. The average HorRat value of the blinded test foods was 0.66 for results greater than LOQ (n = 4206). Conclusions: The study showed that the method performed satisfactorily as a standard method for extractible elemental analysis of food. Highlights: The method met or exceeded the performance expected.

Journal ArticleDOI
TL;DR: Setting these guidelines will facilitate and streamline the validation process for qualitative real-time PCR-based assays for probiotic identity authentication in support of quality assurance systems.
Abstract: Backgroud: Probiotics have been shown to benefit human health through several mechanisms, including their role in improving the health of our gastrointestinal tracts. The health benefits of probiotics are strain specific, and therefore it is critical to include the correct strains in probiotic products when claiming specific health benefits. Several studies have reported issues concerning the accuracy of labeling of commercial probiotic products, including inaccurate taxonomy, missing species, or undeclared species. Consequently, there is a growing need to develop and validate assays to reliably verify strain identity in commercial probiotic products. PCR-based methods are the most commonly used methods for food species ingredient diagnostics because they are simple, fast, sensitive, and can be validated. Objective: The aim of this paper is to set the guidelines for validating targeted qualitative real-time PCR assays to verify the presence of specific strains in a probiotic supplement. Methods and Results: Qualitative real-time PCR assays are validated to evaluate the assay performance in terms of specificity, sensitivity, repeatability, and reproducibility in detecting target strains. Conclusions and Highlights: Setting these guidelines will facilitate and streamline the validation process for qualitative real-time PCR-based assays for probiotic identity authentication in support of quality assurance systems.

Journal ArticleDOI
TL;DR: This is the first report that allows for the characterization and quantification of vitamins A, E, and K and five carotenoids in <1 mL human milk.
Abstract: Background: Human milk is the optimal nutrition for all newborns in the first 6 months of life. In order to assess the nutritional needs of the breastfed infant, human milk is often characterized for multiple nutrients. Objective: To ensure that we minimize the volume of milk dedicated for research and optimize the number of nutrients characterized, we developed analytical methodologies for the determination of vitamins A (retinol), E (alpha and gamma tocopherol), K (phylloquinone and menaquinone-4), and five carotenoids (β-carotene, lycopene, β-cryptoxanthin, lutein, and zeaxanthin) using <1 mL human milk. Method: Vitamins E and K and carotenoids are simultaneously isolated from 750 μL milk by liquid-liquid extraction (LLE). Tocopherols and carotenoids are determined by normal-phase LC with fluorescence and ultraviolet detection respectively. Vitamin K is analyzed on the same extracts after resuspension and clean-up by reversed phase liquid chromatography coupled to tandem MS. The analysis of vitamin A involves saponification of 200 μL milk followed by LLE and determination by normal-phase LC with UV detection. Results: Full single-laboratory validation at four different concentration levels is presented. Recovery rates were within 90-105% in all except one case (retinol at 1.9 μg/mL, 88% recovery), with RSDs of repeatability and intermediate reproducibility below 10 and 15%, respectively for all the compounds. Conclusions and Highlights: To the best of best knowledge, this is the first report that allows for the characterization and quantification of vitamins A, E, and K and five carotenoids in <1 mL human milk.

Journal ArticleDOI
TL;DR: This paper describes a single-laboratory validation of a liquid chromatography-diode array detection (LC-DAD) method for quantification of 12 major cannabinoids in Cannabis dried plant materials, concentrates, and oils, and demonstrates applicability of the method to quantitative analysis of important cannabinoids.
Abstract: This paper describes a single-laboratory validation of a liquid chromatography-diode array detection (LC-DAD) method for quantification of 12 major cannabinoids in Cannabis dried plant materials, concentrates, and oils. The method met Standard Method Performance Requirements for quantitative analysis of cannabinoids in Cannabis concentrates and Cannabis dried plant materials. The LOQs were in the range 0.003-0.10% (w/w), depending on the analyte and matrix. Spike recoveries were between 96.7 and 101.3% with relative SDs (RSDs) ≤2.3%. Precision expressed as repeatability and intermediate precision was within 0.3-4.8 and 1.1-5.1%, respectively. The chromatographic separation conditions used in this versatile method are compatible with both DAD-UV and MS detection. During method validation, high-resolution quadrupole time-of-flight MS was employed as a secondary detector (connected in series to the LC-DAD instrument) to provide high confidence identification of target analytes and as a tool for monitoring other cannabinoids for which reference standards were not available. The obtained results demonstrate applicability of the method to quantitative analysis of important cannabinoids in dried plants, concentrates, and oils. Limited data were generated for a food matrix (Cannabis-containing cookies) using this method with LC coupled to a compact single quadrupole mass spectrometer.

Journal ArticleDOI
TL;DR: The method met the SMPR criteria except where the trace minerals were present at very low levels, and the AOAC Stakeholder Panel for Infant Formula and Adult Nutritionals recommended Final Action status of the expanded applicability of the method.
Abstract: Official MethodSM 2011.14/ISO 15151:2018/IDF 229:2018 uses microwave digestion of samples and inductively coupled plasma-atomic emission spectrometry for determination of nine elements, including Ca, Cu, Fe, K, Mg, Mn, Na, P, and Zn. The method was evaluated in a collaborative study of 25 products, including 13 fortified nutritional products (powders, ready-to-feed liquids, and liquid concentrates), five product placebos, six dairy products (liquids, powders, butter, and processed cheese), and the National Institute for Standards and Technology (NIST) Standard Reference Material (SRM) 1849a, in compliance with AOAC INTERNATIONAL Standard Method Performance Requirement (SMPR®) 2014.004. This study significantly expanded the applicability of Official Method 2011.14 beyond the original scope of chocolate milk powder, dietetic milk powder, infant cereal, peanut butter, and wheat gluten. The study included 14 collaborators from 11 countries, and results were compared to SMPR 2014.004. Accuracy of the method was demonstrated using NIST SRM 1849a, yielding recoveries across all laboratories of 98-101% for the nine elements. Precision for the 13 fortified nutritional product samples was 2.2-3.9% for repeatability (relative SD of repeatability) and 6.0-12.2% for reproducibility (RSDR). Excluding Mn, which was present at a wide range of concentrations, the reproducibility was 6.0-9.5%, meeting the performance requirements of SMPR 2014.004. Placebo samples (not fortified with Cu, Fe, Mn, or Zn) yielded acceptable repeatability of 1.8-2.9% for Ca, K, Mg, Na, and P (minerals) but 5.4-29.4% for the low levels of Cu, Fe, Mn, and Zn (trace elements). Reproducibility for the placebos showed the same pattern, with acceptable reproducibility (5.4-10.3%) for minerals but not for the low levels of the trace elements (13.2-82.8%). In the six dairy product samples, repeatability ranged from 1.6 to 3.6% for the minerals, Zn, and the low range of Mn but from 9.4 to 24.6% for Cu, Fe, and the high range of Mn, where concentrations were low as for the nutritional placebos. Reproducibility in the dairy samples was 5.3-8.8% for the minerals but 11.4-55.0% for the trace elements. The mean concentrations of Cu, Fe, and Zn in the dairy products were similar with those in the placebo products, while Zn was present at levels more similar with the fortified nutritional products. Thus, the method met the SMPR criteria except where the trace minerals were present at very low levels. Based on these results, the AOAC Stakeholder Panel for Infant Formula and Adult Nutritionals recommended Final Action status of the expanded applicability of the method. The method was adopted as Final Action by the AOAC Official Methods Board.

Journal ArticleDOI
TL;DR: A double PCR method is established that can clearly identify fox, mink, or raccoon components in beef meat and mutton meat at the 1% (w/w) level.
Abstract: Background: The fraudulent substitution of cheap and low-quality meat for expensive and good-quality meats to gain profit is a common practice in industries worldwide. Adulteration of fox, raccoon, or mink in commercial beef and mutton meat in the supermarket has become a serious problem. Objective: To ensure the meat quality and safety, we have developed a multiplex PCR method to identify the fox, mink, and raccoon components adulterated in beef or mutton with very low detection limits. Methods: PCR primers were designed and tested by examining the size of PCR product, the nuclease digestion products, and DNA sequencing. Results: After primer interference tests, we have established a double PCR method that can clearly identify fox, mink, or raccoon components in beef meat and mutton meat at the 1% (w/w) level. Triplex PCR and quadruple PCR have been also developed, which are able to identify any two types of components or three mixed components in beef meat unambiguously. Conclusions: We have developed multiplex PCR systems. The duplex PCR systems can identify one component (fox, raccoon, or mink) adulterated in beef meat or mutton meat without question, and triplex PCR and quadruple PCR can discriminate two components and three components adulterated in beef meat. Highlights: These methods are convenient, low-cost, highly specific and reliable, and of a great value for meat quality control and food safety quarantine.

Journal ArticleDOI
TL;DR: Validation results showed that method linearity for all analytes in powdered and liquid infant formula ranged from 0.9981 to 0.9999, and in terms of consumer protection, the presented method is a novel approach for the sensitive and accurate determination of glycidol, 2- and 3-MCPD in infant formula and related foodstuffs.
Abstract: Background: Fatty acid esters of glycidol, 2-Monochloropropanediol (MCPD), and 3-MCPD are heat-induced foodborne processing contaminants with possible adverse health effects. These compounds occur frequently in refined edible oils. Consequently, glycidyl esters and 2- and 3-MCPD esters might also be present in foods that contain refined edible oils. Objective: This manuscript describes the single-laboratory validation of an analytical method for the quantitative determination of glycidol, 2-MCPD, and 3-MCPD present as fatty acid esters or as free 2- or 3-MCPD in infant and adult/pediatric nutritional formula. Methods: Technically, the presented method is based on the combination of a Heat-Ultrasound Pressure-supported Solvent Extraction and a GC-MS determination of glycidol, 2-MCPD, and 3-MCPD. From a chemical perspective, the method includes an alkaline catalyzed transesterification, conversion of the unstable glycidol into monobromopropanediol, and the parallel derivatization of all analytes with phenylboronic acid. Results: Validation results showed that method linearity for all analytes in powdered and liquid infant formula ranged from 0.9981 to 0.9999 (n = 18). Repeatability relative standard deviation values for concentration levels between 1.3 μg/kg and 331 μg/kg were in the range of 1 to 12%. Relative recoveries were found to be between 93 and 107%. The analytes were quantifiable down to 5-10 μg/kg in powdered samples and 1-2 μg/kg in liquid samples. Conclusions: The reported results met actual AOAC Standard Method Performance Requirements. Highlights: In terms of consumer protection, the presented method is a novel approach for the sensitive and accurate determination of glycidol, 2-MCPD, and 3-MCPD in infant formula and related foodstuffs.

Journal ArticleDOI
TL;DR: The rapid extraction and UHPLC-DAD methods could enhance throughput for some applications compared with standard protocols and Random effects modeling indicated that extraction and chromatographic methods explained a small proportion of variance compared with genetic and environmental sources.
Abstract: Background: Tomatoes (Solanum lycopersicum) are an economically and nutritionally important crop colored by carotenoids such as lycopene and β-carotene. Market diversification and interest in the health benefits of carotenoids has created the desire in plant, food, and nutritional scientists for improved extraction and quantification protocols that avoid the analytical bottlenecks caused by current methods. Objective: Our objective was to compare standard and rapid extraction as well as chromatographic separation methods for tomato carotenoids. Method: Comparison was based on accuracy and the ability to discriminate between alleles and genetic backgrounds. Estimates of the contribution to variance in the presence of genetic and environmental effects were further used for comparison. Selections of cherry and processing tomatoes with varying carotenoid profiles were assessed using both established extraction and HPLC-diode array detector (HPLC-DAD) methods and rapid extraction and ultra-HPLC-DAD (UHPLC-DAD) protocols. Results: Discrimination of alleles in samples extracted rapidly (<5 min/sample) was similar to samples extracted using a standard method (10 min/sample), although carotenoid concentrations were lower due to reduced extraction efficiency. Quantification by HPLC-DAD (21.5 min/sample) and UHPLC-DAD (4.2 min/sample) were comparable, but the UHPLC-DAD method could not separate all carotenoids and isomers of tangerine tomatoes. Random effects modeling indicated that extraction and chromatographic methods explained a small proportion of variance compared with genetic and environmental sources. Conclusions: The rapid extraction and UHPLC-DAD methods could enhance throughput for some applications compared with standard protocols.

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TL;DR: A literature search on processing and quality control of CR was performed using several literature resources including the Flora of China official website; various scientific databases such as PubMed, Google Scholar, the Web of Science, Science Direct, and China Knowledge Resource Integrated; and other web sources.
Abstract: Coptidis rhizoma (CR), also known as "Huanglian" in Chinese, is a traditional Chinese medicine commonly used in China, and it is an important species used in medicinal and food applications. It has been processed using a variety of methods, and the processed products have been widely used in clinical practice for thousands of years. However, few reports have focused on the systematic review of its processed products and quality control. In this study, a literature search on processing and quality control of CR was performed by using several literature resources including the Flora of China official website; various scientific databases such as PubMed, Google Scholar, the Web of Science, Science Direct, and China Knowledge Resource Integrated; and other web sources such as books and PhD and MS dissertations. Results showed that quality control for different processed products of CR received little or no attention. Its processing still followed ancient methods, and the quality of artifacts in different regions varied. Further attention should be paid to the study of processing technology and quality control with biomarkers. We suggest to establish a quality control mode based on traditional efficacy and with bioactive markers as detection indicators.

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TL;DR: This review presents the nutritional composition, factors influencing the bioavailability, and health outcomes of dark chocolate intake, and extracts pro- and counter-arguments to illustrate these effects from both experimental and clinical studies in an attempt to solve the dilemma.
Abstract: Dark chocolate is not the most popular chocolate; the higher concentration in antioxidants pays tribute to the increment in bitterness. The caloric density of dark chocolate is potentially lower but has a large variability according to recipes and ingredients. Nevertheless, in the last decade, the interest in dark chocolate as a potential functional food has constantly increased. In this review, we present the nutritional composition, factors influencing the bioavailability, and health outcomes of dark chocolate intake. We have extracted pro- and counter-arguments to illustrate these effects from both experimental and clinical studies in an attempt to solve the dilemma. The antioxidative and anti-inflammatory abilities, the cardiovascular and metabolic effects, and influences on central neural functions were selected to substantiate the main positive consequences. Beside the caloric density, we have included reports placing responsibility on chocolate as a migraine trigger or as an inducer of the gastroesophagial reflux in the negative effects section. Despite an extensive literature review, there are not large enough studies specifically dedicated to dark chocolate that took into consideration possible confounders on the health-related effects. Therefore, a definite answer on our initial question is, currently, not available.

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TL;DR: Recommendations for qualitative real-time PCR methods for validating identity tests for botanical ingredients are provided, according to which the practicability of the test method is evaluated by transferring the method to a second laboratory and by comparison with alternative methods.
Abstract: Background: PCR methods are the most commonly used DNA-based identity tool in the commercial food, beverage, and natural health product markets. These methods are routinely used to identify foodborne pathogens and allergens in food. Proper validation methods for some sectors have been established, while there are none in other markets, such as botanicals. Results: A survey of the literature indicates that some validation criteria are not addressed when developing PCR tests for botanicals. Objective: We provide recommendations for qualitative real-time PCR methods for validating identity tests for botanical ingredients. Methods: These include common criteria that underpin the development and validation of rigorous tests, including (1) the aim of the validation test, (2) the applicability of different matrix variants, (3) specificity in identifying the target species ingredient, (4) sensitivity in detecting the smallest amount of the target material, (5) repeatability of methods, (6) reproducibility in detecting the target species in both raw and processed materials, (7) practicability of the test in a commercial laboratory, and (8) comparison with alternative methods. In addition, we recommend additional criteria, according to which the practicability of the test method is evaluated by transferring the method to a second laboratory and by comparison with alternative methods. Conclusions and Highlights: We hope that these recommendations encourage further publication on the validation of PCR methods for many botanical ingredients. These properly validated PCR methods can be developed on small, real-time biotechnology that can be placed directly into the supply chain ledger in support of highly transparent data systems that support QC from the farm to the fork of the consumer.

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TL;DR: Currently, processed meats appear increasingly as a nonhealthy food because of their content of fat, salt, nitrite, and particularly in red meat, for the heme-iron concerning oxidant effect and radicals formation in human gut.
Abstract: Currently, processed meats appear increasingly as a nonhealthy food because of their content of fat, salt, nitrite, and particularly in red meat, for the heme-iron concerning oxidant effect and radicals formation in human gut. Polygonum cuspidatum and rosemary extract has been tested to counteract these effects and experiments were carried out to add polyphenols into whole meat cuts with the aims to improve their healthiness. The addition of these extracts can reduce the oxidation-reduction potential of products, increasing the antioxidant power. Nevertheless, a low percentage of polyphenols were found in the products because of the process effects and an interaction with the ascorbate residue was observed. In addition, some drawbacks were a decrease in of yield and a worsening of some sensorial properties when large amount of extract was added. The balance between the improvement of the wholesomeness content and the acceptability of products is the challenge the current research have to overcome.

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TL;DR: Although all tested methods showed as satisfactory regarding most analytical parameters, QuEChERS method showed much better results in terms of confidence, indicating that traditional SLE and Soxhlet extraction still need improvements for determination of multiclass pesticides in soil samples.
Abstract: Background: The increased use of pesticides leads to permanent pollution of soil, and there is a need for continuous monitoring of these agrochemicals in soil. Objective: Three methods for the simultaneous determination of 12 pesticides belonging to eight chemical groups in soil samples were tested and compared based on analytical parameters. Methods: The quick, easy, cheap, effective, rugged, and safe (QuEChERS); traditional solid-liquid extraction (SLE); and Soxhlet extraction were used for soil sample preparation, while detection and quantification of pesticides were performed using gas chromatography-mass spectrometry (GC-MS). Results: The tested methods featured good sensitivity, and with the exception for carbofuran (Soxhlet method, LOD = 29 μg/kg), for the rest of the pesticides, the studied LODs were less than 12 μg/kg. Except for simazine and carbofuran, LODs obtained by Soxhlet extraction were lower than values obtained by other two methods, whereas QuEChERS gave lower LODs than the traditional SLE method for all compounds except atrazine and acetochlor. The recoveries obtained applying QuEChERS, traditional SLE, and Soxhlet methods for multiple analyses of soil samples fortified at 10, 75, and 200 μg/kg of each pesticide were in the ranges 54-103, 40-91, and 12-92%, respectively. Except for chlorothalonil, the highest recoveries were obtained by the QuEChERS method. Soxhlet was better than traditional SLE method for chlorothalonil, heptachlor, and aldrin; organophosphorus pesticides (fenitrothion and diazinon) and trifluralin, gave similar recoveries for both methods. All three methods were proven to be repeatable, with RSDs lower than 19%. Conclusions: Although all tested methods showed as satisfactory regarding most analytical parameters, QuEChERS method showed much better results in terms of confidence, indicating that traditional SLE and Soxhlet extraction still need improvements for determination of multiclass pesticides in soil samples.

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TL;DR: An overview is given on the principles and applications of the new mass spectrometric methods and requirements and the present work of other institutions regarding method validation are described.
Abstract: The detection of food fraud and undeclared food allergens is one of the major challenges for competent authorities. Because adulterations are continuously adapted to the methods used to uncover them, the accomplishment of this task has become increasingly difficult over time. In recent years, various new promising methods for the detection of multiple food adulterants and multiple food allergens have been developed. Some of them utilize LC-MS to identify specific marker peptides. However, these methods have yet to be validated and standardized. For this reason, the German officials have established a working group with the objective of validating methods through multilaboratory validation studies. The experts of the working group also aim for the first time to standardize validated methods and to develop general validation criteria. This manuscript will highlight the current work of the group. For this purpose, an overview is given on the principles and applications of the new mass spectrometric methods. Moreover, requirements and the present work of other institutions regarding method validation are described.

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TL;DR: The developed SPE and preconcentration method exhibited simplicity and reliable, simultaneous determination of AR and BB in foodstuffs and will be more useful for future food quality and control applications.
Abstract: Background: Allura Red (AR) and Brilliant Blue FCF (BB) are highly water-soluble synthetic food dyes used to color baked goods, beverages, candies, jellies, sausages, etc. Although AR and BB are not entirely toxic, they can lead to health problems in humans. Objective: The aim of the study was to develop a column solid-phase extraction (SPE) and preconcentration method based on the adsorption on a Diaion HP-20 polymeric resin for simultaneous spectrophotometric determination of AR and BB. Methods: The column SPE method was used, and the analytical parameters of the SPE method, such as pH, sample flow rate, sample volume, etc., were systematically investigated and optimized. Results: The detection limits of AR and BB ranged between 0.90 and 0.19 μg/L and quantification limits between 2.59 and 0.53 μg/L, respectively. Preconcentration factors were obtained at 80 and 100 for AR and BB, respectively. The RSDs of the method were lower than 4% for both dyes. The method was successfully applied to foodstuffs. AR and BB contents in foodstuffs were determined between 9.48-407.34 and 2.96-137.12 μg/g, respectively, for solid samples; 52.28 and 5.91 μg/mL of dye contents of liquid samples were determined for AR and BB, respectively. Conclusions: Satisfactory recoveries show that the method will be more useful for future food quality and control applications. Highlights: The developed method exhibited simplicity and reliable, simultaneous determination of AR and BB in foodstuffs.

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TL;DR: A new culture method based on the most probable number approach, Legiolert®, with the formal culture method used at EnvironeX for regulatory compliance testing to quantify L. pneumophila from cooling tower waters in Québec showed several advantages over the agar plate method, including increased sensitivity, reduced interference, a simplified test procedure, and an easy-to-read positive signal.
Abstract: Background: Legionnaires' disease is a potentially lethal pneumonia contracted through inhalation of aerosolized water contaminated with Legionella bacteria. Detection and control of L. pneumophila, the primary species responsible for the disease, is critical to public health. In Quebec, cooling towers and evaporative condensers are required to follow a maintenance and testing program to ensure L. pneumophila concentrations remain at acceptable levels. Objective: This study compared a new culture method based on the most probable number approach, Legiolert®, with the formal culture method used at EnvironeX for regulatory compliance testing to quantify L. pneumophila from cooling tower waters in Quebec. Methods: A split-sample analysis was performed in which 401 samples from cooling towers in Quebec were tested with both methods. Results: Results with 74 positive samples showed that Legiolert provided a significant increase in sensitivity for L. pneumophila compared with the agar plate method. Cooling tower samples often contain non-Legionella flora that necessitate multiple treatment and plating conditions to prevent interference with the test. Legiolert showed little to no impact from non-Legionella organisms in this study. Conclusions: Overall, Legiolert showed several advantages over the agar plate method, including increased sensitivity, reduced interference, a simplified test procedure, and an easy-to-read positive signal.