bluuebunny/crossref_metadata_2025_split huggingface dataset:
Interlaboratory Verified Liquid Chromatographic Method for Analysis of Vitamins A and E in Soy-Based Infant Formula Powder
Authors: Chase G William , Ye Lin , Stoakes Vicky C , Eitenmiller Ronald R , Long Austin R 
Published: February 2020

Abstract
An interlaboratory verified, liquid chromatographic (LC) method is presented for the analysis of all-rac-α-tocopheryl acetate and retinyl palmitate in soy-based infant formula. The extraction procedure uses sample dehydration with magnesium sulfate followed by extraction with isopropanol, hexane–ethyl acetate (85 + 15, v/v). After evaporation and filtration, the sample extract is injected directly onto a normal-phase LC system with fluorescence detection. All-rac-α-tocopheryl acetate and retinyl palmitate are quantitated isocratically with a mobile phase of hexane containing 0.50% (v/v) and 0.125% (v/v) isopropanol, respectively. A zero control reference material (ZRM) was spiked at 5 levels, with 5 replicate analyses of 1/2x, x, 2x, 4x, and 16x where “x” is the minimum level of 250 IU/100 kcal (vitamin A) and 0.7 IU/100 kcal (vitamin E) as specified in 21 Code of Federal Regulations 107.100. The following recoveries and RSD values represent an average (n = 25) of the 5 levels for each analyte: all-rac-α-tocopheryl acetate, 100% (RSD = 3.5%); retinyl palmitate, 97.2% (RSD = 2.1%). Two additional laboratories analyzed the fortified ZRM samples. Average recoveries (n = 24) of all-rac-α-tocopheryl acetate and retinyl palmitate at 4 levels were all-rac-α-tocopheryl acetate, 99.0% (RSD = 4.0%), and retinyl palmitate, 96.2% (RSD = 1.4%) at the second laboratory. Average recoveries (n = 24) of all-rac-α-tocopheryl acetate and retinyl palmitate at 4 levels were all-rac-α-tocopheryl acetate, 102% (RSD = 1.4%) and retinyl palmitate, 95.7% (RSD = 2.0%) at the third laboratory. In addition, 6 replicates of the same commercial soy-based infant formula powder were run by the 3 laboratories.
Determination of Processed Animal Proteins, Including Meat and Bone Meal, in Animal Feed
Authors: Gizzi Giséile , von Holst Christoph , Baeten Vincent , Berben Gilbert , van Raamsdonk Leo 
Published: February 2020

Abstract
An intercomparison study was conducted to determine the presence of processed animal proteins (PAPs), including meat and bone meal (MBM) from various species, in animal feed. The performances of different methods, such as microscopy, polymerase chain reaction (PCR), immunoassays, and a protocol based on iquid chromatography (LC), were compared. Laboratories were asked to analyze for PAPs from all terrestrial animals and fish (total PAPs); mammalian PAPs; ruminant PAPs; and porcine PAPs. They were free to use their method of choice. In addition, laboratories using microscopy were asked to determine the presence of PAPs from terrestrial animals, which is applicable only to microscopy. For total PAPs microscopy, LC and some immunoassays showed sufficient results at a concentration as low as 0.1% MBM in the feed. In contrast, PCR was not fit for purpose. In differentiating between MBM from terrestrial animals and fishmeal, microscopy detected 0.5% of terrestrial MBM in feed in the presence of 5% fishmeal, but was less successful when the concentration of MBM from terrestrial animals was 0.1%. The animal-specific determination of MBM from mammals or, more specifically from either ruminants or pigs, by PCR showed poor results, as indicated by a high number of false-positive and false-negative results. The only PCR method that scored quite well was applied by a member of the organizer team of the study. Immunoassays scored much better than PCR, showing sufficient sensitivity but some deficiency in terms of specificity. The results also demonstrated that the reliable determination of MBM from ruminants has not been resolved, especially for low concentrations of MBM (0.1%) in feed. Comparison of the results for mammalian MBM from all methods indicated that, for control purposes, the immunoassay method, especially when applied as dipsticks, could be used as a rapid screening method combined with microscopy to confirm the positive samples. However, implementation of such a system would require that the immunoassays were previously validated to demonstrate that this approach is fit for purpose. The determination of ruminant or porcine PAPs by immunoassays was more difficult, partly because the MBM in this study contained about 50% bovine and porcine material, thereby reducing the target concentration level to 0.05%.
Real-Time Polymerase Chain Reaction-Based Approach for Quantification of the pat Gene in the T25 Zea mays Event
Authors: Weighardt Florian , Barbati Cristina , Paoletti Claudia , Querci Maddalena , Kay Simon , De Beuckeleer Marc , Van den Eede Guy 
Published: February 2020

Abstract
In Europe, a growing interest for reliable techniques for the quantification of genetically modified component(s) of food matrixes is arising from the need to comply with the European legislative framework on novel food products. Real-time polymerase chain reaction (PCR) is currently the most powerful technique for the quantification of specific nucleic acid sequences. Several real-time PCR methodologies based on different molecular principles have been developed for this purpose. The most frequently used approach in the field of genetically modified organism (GMO) quantification in food or feed samples is based on the 5′-3′-exonuclease activity of Taq DNA polymerase on specific degradation probes (TaqMan® principle). A novel approach was developed for the establishment of a TaqMan quantification system assessing GMO contents around the 1% threshold stipulated under European Union (EU) legislation for the labeling of food products. The Zea mays T25eliteeventwas chosen as a model for the development of the novel GMO quantification approach. The most innovative aspect of the system is represented by the use of sequences cloned in plasmids as reference standards. In the field of GMO quantification, plasmids are an easy to use, cheap, and reliable alternative to Certified Reference Materials (CRMs), which are only available for a few of the GMOs authorized in Europe, have a relatively high production cost, and require further processing to be suitable for analysis. Strengths and weaknesses of the use of novel plasmid-based standards are addressed in detail. In addition, the quantification system was designed to avoid the use of a reference gene (e.g., a single copy, species-specific gene) as normalizer, i.e., to perform a GMO quantification based on an absolute instead of a relative measurement. In fact, experimental evidences show that the use of reference genes adds variability to the measurement system because a second independent real-time PCR-based measurement must be performed. Moreover, for some reference genes no sufficient information on copy number in and among genomes of different lines is available, making adequate quantification difficult. Once developed, the method was subsequently validated according to IUPAC and ISO 5725 guidelines. Thirteen laboratories from 8 EU countries participated in the trial. Eleven laboratories provided results complying with the predefined study requirements. Repeatability (RSDr)values ranged from 8.7 to 15.9%, with a mean value of 12%. Reproducibility (RSDR) values ranged from 16.3 to 25.5%, with a mean value of 21%. Following Codex Alimentarius Committee guidelines, both the limits of detection and quantitation were determined to be &lt;0.1%.
Regulatory and Compliance Activities to Protect Food-Allergic Consumers in Canada: Research in Support of Standard Setting and Consumer Protection
Authors: Ben Rejeb Samuel , Lauer Bruce , Salminen John , Roberts Irene , Wadhera Ashwani , Abbott Michael , Davies David , Cléroux Chantal , Weber Dorcas , Lau Benjamin , Bacler Stan , Langlois Daniel , Kurz Karl 
Published: February 2020

Abstract
An overview is presented of the activities of Health Canada and the Canadian Food InspectionAgency (CFIA) in the area of food allergens. Since the 1990s, changes were made in the Food and Drug Regulations in order to better protect allergic consumers by imposing labeling requirements to clearly identify sources of priority food allergens in prepackaged foods. Policies of application as well as risk management strategies are discussed with some statistics on allergen-related food recalls in Canada for the years 1997–2001. Health Canada's allergen method development program is a pioneering research initiative that was developed in the early 1990s in support of the changing Canadian regulatory environment. The objectives and some of the accomplishments of this program are presented. The development of the CanadianCompendium of Allergen Methodologies under aWeb-based application to compile data on evaluated allergen detection methods will provide further support to compliance activities nationally, as well as to the international analytical community in both government and the food industry. Some emerging techniques for the confirmation of results generated by enzyme-linked immunosorbent assays are also discussed.
Immunochemical Analytical Methods for the Determination of Peanut Proteins in Foods
Authors: Whitaker Thomas B , Williams Kristina M , Trucksess Mary W , Slate Andrew B 
Published: February 2020

Abstract
Peanut proteins can cause allergenic reactions that can result in respiratory and circulatory effects in the body sometimes leading to shock and death. The determination of peanut proteins in foods by analytical methods can reduce the risk of serious reactions in the highly sensitized individual by allowing for the detection of these proteins in a food at various stages of the manufacturing process. The method performance of 4 commercially available enzyme-linked immunosorbent assay (ELISA) kits was evaluated for the detection of peanut proteins in milk chocolate, ice cream, cookies, and breakfast cereals: ELISA-TEK Peanut Protein Assay, now known as “Bio-Kit” for peanut proteins, from ELISA Technologies Inc.; Veratox for Peanut Allergens from Neogen Corp.; RIDASCREEN Peanut Kit from R-Biopharm GmbH; and ProLisa from Canadian Food Technology Ltd. The 4 test kits were evaluated for accuracy (recovery) and precision using known concentrations of peanut or peanut proteins in the 4 food matrixes. Two different techniques, incurred and spiked, were used to prepare samples with 4 known concentrations of peanut protein. Defatted peanut flour was added in the incurred samples, and water-soluble peanut proteins were added in the spiked samples. The incurred levels were 0.0, 10, 20, and 100 μg whole peanut per g peanut protein per g food; the spiked levels were 0.0, 5, 10, and 20 μg peanut protein per g food. Performance varied by test kit, protein concentration, and food matrix. The Veratox kit had the best accuracy or lowest percent difference between measured and incurred levels of 15.7% when averaged across all incurred levels and food matrixes. Recoveries associated with the Veratox kit varied from 93 to 115% for all food matrixes except cookies. Recoveries for all kits were about 50% for cookies. The analytical precision, as measured by the variance, increased with an increase in protein concentration. However, the coefficient of variation (CV) was stable across the 4 incurred protein levels and was 7.0% when averaged across the 4 food matrixes and analytical kits. The R-Biopharm test kit had the best precision or a CV of 4.2% when averaged across all incurred levels and food matrixes. Because measured protein values varied by test kit and food matrix, a method was developed to normalize or transform measured protein concentrations to an adjusted protein value that was equal to the known protein concentration. The normalization method adjusts measured protein values to equal the true protein value regardless of the type test kit or type food matrix.
Results from Two Interlaboratory Comparison Tests Organized in Germany and at the EU Level for Analysis of Acrylamide in Food
Authors: Klaffke Horst , Fauhl Carsten , Mathar Wolfgang , Palavinskas Richard , Wittkowski Reiner , Wenzl Thomas , Anklam Elke 
Published: February 2020

Abstract
After the publication of high levels of acrylamide (AA) in food, many research activities started all over the world in order to determine the occurrence and the concentration of this substance in various types of food. As no validated methods were available at that time, interlaboratory studies on the determination of AA in food were of the highest priority. Under the boundary conditions of applying well-established evaluation schemes, the results of 2 studies conducted by the Federal Institute for Risk Assessment (BfR) in Germany and by the European Commission's Directorate General Joint Research Center (JRC) exhibited an overall acceptable performance of the participants in these studies. Nevertheless, many laboratories showed problems in determining AA in food with a complex matrix such as cocoa. The results of analysis also showed a broader variation of AA for samples with low AA concentrations and indicated a bias of the results obtained by gas chromatography–mass spectrometry without derivatization. Improvements of the performance of some laboratories appeared to be necessary.
Validation of a Method for the Determination of Narasin in the Edible Tissues of Chickens by Liquid Chromatography
Authors: Ward Tracey L Cash , Moran John W , Turner James M , Coleman Mark R 
Published: February 2020

Abstract
Maxiban® and Monteban® are 2 products marketed by Elanco Animal Health. They contain narasin and are used for the prevention of coccidiosis in chickens. Products used in the European market must be regularly re-registered with new data to support label claims. This study was undertaken as part of such a re-registration effort. A method for the determination of narasin in poultry tissue was previously registered with the authorities; however, a method with more environmentally friendly solvents was desired. The Canadian Food Inspection Agency accomplished this goal and published an improved method. In order to register the method with European authorities as the official Elanco method for determination of narasin, Elanco scientists were required to provide validation data for all edible poultry tissues. This paper shows the validation of the method to detect residues of narasin using solid-phase extraction followed by liquid chromatographic analysis utilizing post-column derivatization.
Precolumn Derivatization Liquid Chromatography Method for Analysis of Dietary Supplements for Glucosamine: Single Laboratory Validation Study
Authors: Ji David , Zhang Lingjun , Chen Jianhai , Peng Emily 
Published: February 2020

Abstract
A precolumn derivatization liquid chromatography (LC) method was developed for the analysis of various dietary supplement formulations and raw materials for glucosamine. A 1 mL sample or standard water solution (containing about 0.05 mg glucosamine) was mixed with 1 mL pH 8.3 buffer, 1 mL 5% phenylisothiocyanate methanolic solution, and derivatized at 80°C in a water bath for 30 min. After derivatization, the solution was cooled in a cold water bath and centrifuged at 3000–5000 rpm. The clear upper layer was ready for injection. The LC system was equipped with a C18 reversed-phase column and an ultraviolet detector set at 240 nm. The column was developed with a linear gradient composed of 0.1% phosphoric acid in deionized water and 0.1% phosphoric acid in methanol. The method was subjected to Single Laboratory Validation. The method precision was 0.50% relative standard deviation, accuracy was less than ±1.5%, method linearity in the range 0–2 mg glucosamine/mL was 1.00, the detection limit was 0.0705 μg/mL, and the quantitation limit was 0.235 μg/mL. Chondroitin sulfate, amino acids, and excipients did not interfere with glucosamine testing. After derivatization, both standard and sample preparations were stable for at least 48 h. Due to its high sensitivity, this method can be used to assay glucosamine in functional foods and pet foods. The validation data will be published separately.
Validation of a Fast and Easy Method for the Determination of Residues from 229 Pesticides in Fruits and Vegetables Using Gas and Liquid Chromatography and Mass Spectrometric Detection
Authors: Lehotay Steven J , Kok André de , Hiemstra Maurice , Bodegraven Peter van 
Published: February 2020

Abstract
Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10–100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid–liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70–120% (90–110% for 206 pesticides), and repeatabilities typically &lt;10% were achieved for a wide range of fortified pesticides, including methamidophos, spinosad, imidacloprid, and imazalil. Dispersive SPE with PSA retained carboxylic acids (e.g., daminozide), and &lt;50% recoveries were obtained for asulam, pyridate, dicofol, thiram, and chlorothalonil. Many actual samples and proficiency test samples were analyzed by the method, and the results compared favorably with those from traditional methods.
Determination of Chloramphenicol Residues in Milk, Eggs, and Tissues by Liquid Chromatography/Mass Spectrometry
Authors: Penney Lisa , Smith Anderson , Coates Brent , Wijewickreme Arosha 
Published: February 2020

Abstract
A new liquid chromatography/mass spectrometry (LC/MS) method is presented for the determination of chloramphenicol (CAP) residues in milk, eggs, chicken muscle and liver, and beef muscle and kidney. CAP is extracted from the samples with acetonitrile and defatted with hexane. The acetonitrile extracts are then evaporated, and residues are reconstituted in 10mM ammonium acetate–acetonitrile mobile phase and injected into the LC system. CAP is determined by reversed-phase chromatography using an Inertsil ODS-2 column and MS detection with negative ion electrospray ionization. Calibration curves were linear between 0.5–5.0 ng/g for all matrixes studied. The relative standard deviations for measurements by this method were generally &lt;12%, and average recoveries ranged from 80 to 120%, depending on the matrix involved. The method detection limits of CAP ranged from 0.2 to 0.6 ng/g, which are comparable to previously reported results. The proposed method is rapid, simple, and specific, allowing a single analyst to easily prepare over 40 samples in a regular working day.
Isoelectric Focusing Identification of Four Freshwater Fish Commercially Labeled “Perch”
Authors: Berrini Anna , Tepedino Valentina , Borromeo Vitaliano , Secchi Camillo 
Published: February 2020

Abstract
Isoelectric focusing (IEF) was used to distinguish 4 freshwater fish species that are sold in the European Union under the generic label of “perch”: Perca fluviatilis (European perch), Lates niloticus (Nile perch), Stizostedion lucioperca (European pikeperch), and Morone chrysops x saxatilis (Sunshine bass). These species have different commercial values but are easily interchangeable because they are sold already filleted, in view of the numerous bones of the whole fish. IEF of the water-soluble proteins extracted from fish muscle resulted in species-specific patterns. None of the bands was common to all 4 species. Intraspecies polymorphism was low and did not concern the bands identified as characteristic of the species.
Determination of Ochratoxin A in Green Coffee by Immunoaffinity Column Cleanup and Liquid Chomatography: Collaborative Study
Authors: Vargas Eugênia Azevedo , dos Santos Eliene Alves , Pittet Alain ,   Collaborators:, Corrêa T B S , da Rocha A P P , Diaz G J , Gorni R , Koch P , Lombaert G A , MacDonald S , Mallmann C A , Meier P , Nakajima M , Neil R J , Patel S , Petracco M , Prado G , Sabino M , Steiner W , Stroka J , Taniwaki M H , Wee S M 
Published: February 2020

Abstract
A collaborative study was conducted to evaluate a method using immunoaffinity column cleanup with liquid chromatography (LC) for the determination of ochratoxin A (OTA) in green coffee at levels that could be included in possible future regulations of the European Union. The test portion was extracted with methanol–3% aqueous sodium hydrogen carbonate solution (50 + 50, v/v). The extract was filtered, and the filtrate was diluted with phosphate-buffered saline and applied to an immunoaffinity column containing antibodies specific for OTA. After washing, the toxin was eluted from the column with methanol and quantified by LC with fluorescence detection. Pairs of 4 homogeneous noncontaminated and naturally contaminated materials (mean levels of &lt;0.12, 2.44, 5.15, and 13.46 ng/g) and blank samples (&lt;0.12 ng/g) for spiking were sent to 20 participant laboratories from 8 countries. The materials were analyzed according to the method description and all difficulties encountered in the analysis were reported. Statistical analysis was carried out according to the Harmonized Protocol of the International Union of Pure and Applied Chemistry. The relative standard deviation for repeatability (RSDr) ranged from 7.42 to 20.94%, and the relative standard deviation for reproducibility (RSDR) ranged from 16.34 to 29.17%. The method showed acceptable within-laboratory and between-laboratories precision for green coffee materials, as evidenced by HorRat values of ≤0.85, at the studied range, for spiked and naturally contaminated materials. The mean recovery was 92.8% for green coffee material spiked with OTA at a level of 4.82 ng/g.