bluuebunny/crossref_metadata_2025 huggingface dataset:
Determination of Selenium in Feeds and Premixes: Collaborative Study
Authors: Palmer Ivan S , Thiex Nancy ,   Collaborators:, Allen R , Alley E , Anderson N , Bell J , Carpenter N , Cunningham W , Deuschle L , Kane P , Marts R , Rottinghaus G , Rutta S , Torma L , Vindiola A , Wenger J , Whanger P , Williams A , Wo C
Published: February 2020

A total of 17 laboratories participated in a collaborative study for the determination of selenium in feeds and premixes using either a fluorometric or a continuous hydride generation atomic absorption (HGAA) method. Each collaborator analyzed 16 blind duplicate samples of feed and premixes from various feed manufacturers. The amount of Se in these materials ranged from 0.2 to 5500 μg/g. Six laboratories used only the fluorometric procedure, 8 laboratories used only the hydride generation atomic absorption procedure, and 3 laboratories used both procedures. One laboratory in the fluorometric study and 3 laboratories in the HGAA study were initially excluded because of invalid data. Poor agreement between the blind duplicates indicated probable sample interchange and/or dilution error. The data from 8 laboratories were submitted to statistical analysis, including data from 2 laboratories participating in both studies. The repeatability standard deviation (RSDr) for samples analyzed by the fluorometric procedure ranged from 5.9 to 33%, and the reproducibility standard deviation (RSDR) ranged from 12 to 33%. RSDf for samples analyzed by HGAA ranged from 2.8 to 18%, and RSDR ranged from 4.0 to 36%. Both fluorometric and continuous hydride generation atomic absorption methods for the determination of Se in feeds and premixes have been adopted first action by AOAC INTERNATIONAL.
Liquid Chromatographic Determination of the Glycoalkaloids α-Solanine and α-Chaconine in Potato Tubers: NMKL Interlaboratory Study
Authors: Hellenás Karl-Erik , Branzell Carina ,   Collaborators:, Poutanen H , Suortti T , Kaario R , Gjerstad K O , Brekke T , Jensen A M , Larsen K , Knuthsen P , Halén B , Olsson K , Ingólfsdóttir; I K , Pittet A
Published: February 2020

Twelve laboratories participated in a collaborative study to evaluate precision parameters of a liquid chromatographic method for analysis of the glycoalkaloids α-solanine and α-chaconine in potato tubers. Samples consisted of frozen potato tuber homogenates distributed as 3 blind duplicates and 3 split-level pairs. The analytical method included aqueous extraction, workup on disposable solidphase extraction cartridges, and reversed-phase chromatography with photometric detection at 202 nm. Results for α-solanine and α-chaconine were received from 10 and 9 laboratories, respectively. Relative standard deviations for reproducibilo ity for α-solanine and α-chaconine were similar, ranging from 8 to 13% in the applied concentration range of 12 to 260 mg/kg fresh weight.
Certification of Nutrients in Standard Reference Material 1846: Infant Formula
Authors: Sharpless Katherine E , Schiller Susannah B , Margolis Sam A , Thomas Jeanice Brown , Iyengar G Venkatesh , Colbert Jennifer C , Gills Thomas E , Wise Stephen A , Tanner James T , Wolf Wayne R
Published: February 2020

In 1996, the National Institute of Standards and Technology (NIST) released Standard Reference Material 1846 (Infant Formula), which can be used as a control material for assigning values to in-house control materials and for validating analytical methods for measurement of proximates, vitamins, and minerals in infant formula and similar matrixes. The SRM was manufactured by preparing a spray-dried formula base containing fat, protein, carbohydrates, and minerals and then combining that formula base with a dry-blend vitamin premix that supplied the vitamins. The Certificate of Analysis for SRM 1846 provides assigned values for concentrations of proximates (fat, protein, etc.), vitamins, and minerals for which product labeling is required by the Infant Formula Act of 1980 and by the Nutrition Labeling and Education Act of 1990. These assigned values were based on agreement of measurements by NIST and/or collaborating laboratories. Certified values are provided for vitamins A (trans), E, C, B2, and Be and niacin. Noncertified values are provided for solids, ash, fat, nitrogen, protein, carbohydrate, calories, vitamin D, δ-tocopherol, γ-tocopherol, vitamin Bi, vitamin B12, folic acid, pantothenic acid, biotin, choline, inositol, calcium, phosphorus, magnesium, iron, zinc, copper, sodium, potassium, and chloride. Information values are provided for iodine, manganese, selenium, and vitamin K.
Microwave Digestion for Determination of Aluminum, Boron, and 13 Other Elements in Plants by Inductively Coupled Plasma Atomic Emission Spectrometry
Authors: Sun Da-Hai , Waters James K , Mawhtnney Thomas P
Published: February 2020

A microwave digestion procedure was developed for determining aluminum and boron and 13 other elements in plant tissues by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample (0.5 g) was digested in a closed Teflon vessel with 10 mL concentrated nitric acid and 3 mL hydrofluoric acid, and further digested in an open Teflon vessel with 5 mL hydrogen peroxide. Excess hydrofluoric acid was eliminated by adding 0.2 g silicon (IV) oxide. Four National Institute of Standards and Technology standard reference materials (apple leaves, peach leaves, tomato leaves, and pine needles) were analyzed to test the reliability of the method. The excellent recoveries indicate that the proposed procedure is simple and effective for determination of Al, B, Ba, Ca, Cr, Cu, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn in plants.
Liquid Chromatographic Determination of Monensin in Premix and Animal Feeds: Collaborative Study
Authors: Coleman Mark R , Moran John W , Mowrey Daniel H ,   Collaborators:, Antalick J P , Bark D J , Bridges D A , Britton N L , Campbell H M , Cardenas J , Johannsen F H , Reeves V B , Siirila A , Smallidge R L , Wetzler L
Published: February 2020

An interlaboratory study of a liquid chromatographic (LC) method for determining monensin in premix (60–80 g/lb or 132–5176 mg/g) and animal feeds (5–200 g/ton or 0.0055–0.22 mg/g) was conducted in laboratoriesin the United States, Canada, France, and Germany. The LC system used a reversed- phase column, postcolumn derivatization with vanillin, and UV detection. The method separates monensin from other ionophores such as narasin and salinomycin. Each laboratory analyzed a total of 20 samples of premix, liquid feed supplements, poultry, and cattle feeds. Concentrations of monensin in all samples ranged from 0 to 176 mg/g (80 g/lb). Reproducibility relative standard deviation (RSDR) for premix ranged from 2.8 to 3.4%. For feed samples containing monensin, repeatability standard deviation (Sr) ranged from 0.9 to 7.0. Reproducibility standard deviation (SR) ranged from 1.2 to 11. Repeatability relative standard deviation (RSDr) ranged from 6.1 to 21% and RSDR valuesranged from 8.6 to 25%. Sample preparation for the LC method is less labor intensive than that for the microbiological assays. The LC assay is more efficient than the microbiological assays. This LC method for determination of monensin in premix and animal feeds has been adopted first action by AOAC INTERNATIONAL.
Determination of Ethoxyquin in Feeds by Liquid Chromatography: Collaborative Study
Authors: Schreier Curtis J , Greene Robert J ,   Collaborators:, Bhandari S , Britton N , Greene B , Grimm D , Hannah K , Hwang Y , Jeffress D , Kegley M , Mawhinney T , McGill B , Oehrl L , Schulze C , Smallidge R , Vincent D , Wallace M , Willis D
Published: February 2020

Ethoxyquin is a chemical antioxidant used in feeds, ingredients, fats, and oils. A liquid chromatographic (LC) method for determination of ethoxyquin was developed. The method involves acetonitrile extraction of the sample and isocratic Cis reversed-phase chromatography with ammonium acetate buffer-acetonitrile as mobile phase and fluorescence detection. A collaborative study of the determination of ethoxyquin in various meals and extruded pet foods was conducted by The lams Company Research Laboratory. Eleven laboratories analyzed 16 samples (including 2 blind duplicates) consisting of 7 meat meals and 9 extruded pet foods. Sample means ranged from 0.25 to 289 ppm. Repeatability standard deviations ranged from 0.08 to 3.2 ppm, and repeatability relative standard deviations ranged from 4.5 to 32%. Reproducibility standard deviations ranged from 0.12 to 13 ppm, and reproducibility relative standard deviations ranged from 4.5 to 55%. The LC method for determination of ethoxyquin in feeds has been adopted first action by AOAC INTERNATIONAL.
Comparison of the Petrifilm Dry Rehydratable Film and Conventional Culture Methods for Enumeration of Yeasts and Molds in Foods: Collaborative Study
Authors: Knight Michael T , Newman Melissa C , Benzinger M Joseph , Neufang Karen L , Agin James R , McAllister J Sue , Ramos Mary ,   Collaborators:, Carter M , Duran B , Hagan K , Hansen R , Rudolph C , Quinley S , Updaw A , Neufang K , Brook L , Lucia L , Koeritzer B , Tomer J , Smith T , Brown D , Lobo C , Tobin P , O’Brien-Gammon L , Boleszcczuk P
Published: February 2020

A collaborative study was performed involving 18 laboratories and 6 food types to compare 3M Petrifilm yeast and mold count plates with the method described in the U.S. Food and Drug Administration’s Bacteriological Analytical Manual. Four species of mold and 2 species of yeast were used to inoculate the following foods: hot dogs, corn meal, ketchup, orange juice, yogurt, and cake mix. Each collaborator received 15 samples of each food type: 5 low-level inoculations, 5 high- level inoculations, and 5 uninoculated samples. There was no significant difference between the means of the 2 methods for any product or inoculation level. The Petrifilm yeast and mold count plate method for enumeration of yeasts and molds in foods has been adopted first action by AOAC INTERNATIONAL.
Development and Validation of a Quantitative Method for Determination of Carmine (E120) in Foodstuffs by Liquid Chromatography: NMKL Collaborative Study
Authors: Merino Leonardo , Edberg Ulla , Tidriks Hakan ,   Collaborators:, Berndtsson I , Blomberg K , Gustavsen S , Hestdal M , Jensen A , Knuthsen P , Larsen K , Moe K , Nordbotten A , Warne N , Olsen O , Sinervo T , Thim A M
Published: February 2020

ThimA liquid chromatographic method for quantitative determination of carmine (E120) in different foodstuffs is described. Qualitative and semiquantita- tive methods for analysis of carmine and other related dyes are well established. However, quantitative methods available are based mainly on enzymatic reactions that are time-consuming or specific for analysis of carminic acid in yoghurt. In the method developed and validated here, carminic acid is extracted by boiling the sample with HCI, purified on a solid-phase extraction cartridge, and injected on a Cis analytical column. The method was evaluated by an internal analytical quality control and a collaborative study in which 11 laboratories from the Nordic countries participated. The food samples analyzed were fruit jelly, liqueur, juice, yoghurt, and ice cream. Materials were distributed to participants as uniform level and split level. Validation showed that the proposed method is well suited for quantitative determination of carmine. The detection limit is 0.1 mg/L. The mean relative standard deviation for reproducibility varies from 7.9 to 11.7%. The proposed method is simple and relatively fast compared with previously published methods.
Liquid Chromatographic Determination of Tilmicosin in Swine Feed at 200–400 mg/kg Level: Interlaboratory Study
Authors: Readnour Robin S , Coleman Mark R , Leadbetter Mary G ,   Collaborators:, Armstrong F , Campbell H , Cleveland C , Dixon S , Massom L , Nandihalli U , Pritts K , Smallidge R , Steed M , Wallace M
Published: February 2020

An analytical method for the determination of tilmicosin at 200–400 mg/kg, the intended use concentration range, was evaluated in an interlaboratory study involving 5 laboratories, including the sponsor. The interlaboratory study evaluated the intra- and interlaboratory precision and accuracy of a tilmicosin feed method. The method procedure involved extracting tilmicosin from feed by adding 200 mL extractant to 20 g feed and shaking for 1 h. The extract is filtered and analyzed by gradient liquid chromatography which separates tilmicosin from feed matrix in 30 min. Each laboratory assayed 5 replicates of fortified feed at concentrations of 0,100, 200, 400, and 600 mg/kg. The mean recovery among fortified samples ranged from 81.4 to 98.8%, with a percent coefficient of variation (%CV) ranging from 0.3 to 4.0%. For all blank control feed samples no significant interferences were observed. In addition, each laboratory assayed 5 replicates of medicated feed samples prepared at 2 levels (200 and 400 mg/kg) with either a horizontal or vertical mixer. Along with the medicated feed samples were included 5 replicates of a blank control feed. The identities of the medicated and blank control feed samples were blinded to the analysts. The results for the medicated feed samples ranged from 95.8 to 106% of label claim, with a %CV ranging from 2.1 to 6.7%.
Bacterial Inhibition Tests Used To Screen for Antimicrobial Veterinary Drug Residues in Slaughtered Animals
Authors: Korsrud Gary O , Boison Joe O , Nouws Jacques F M , Macneil James D
Published: February 2020

Bacterial inhibition tests used to screen milk, tissues, blood, and urine for antimicrobial veterinary drug residues must be high volume, quick, rugged, inexpensive, and sensitive. Bacterial inhibition tests—such as the Swab Test on Premises (STOP), the Calf Antibiotic and Sulfa Test (CAST), the Fast Antibiotic Screen Test (FAST), the Charm Farm Test (CFT), the Antimicrobial Inhibition Monitor 96 (AIM-96) assay, the German Three Plate Test, the European Union Four Plate Test and the New Dutch Kidney Test—have been used to screen tissues for antimicrobial activity. The CFT and the Brilliant Black Reduction Test (BBRT) also have been used to screen plasma. The Live Animal Swab Test (LAST) was developed to screen urine. This review examines the use and limitations of these screening tests for regulatory control and avoidance of veterinary drug residues in meat. The ideal bacterial inhibition test for screening antimicrobial residues in slaughtered animals does not exist. Each of the current and potential tests has limitations.
Evaluation of the European Four-Plate Test as a Tool for Screening Antibiotic Residues in Meat Samples from Retail Outlets
Authors: Okerman Lieve , Hoof Jan van , Debeuckelaere Wim
Published: February 2020

A modified 4-plate test was used to screen 4795 meat samples from retail outlets in the European Community (EC). This microbial inhibition test uses 3 media seeded with Bacillus subtilis at different pH values (6, 7.2, or 8) and a fourth medium seeded with Micrococcus luteus. Positive samples were confirmed by a receptor test for macrolides, a thin-layer chromatographic method for sulfonamides, or an enzyme-linked immunosorbent assay test for tetracyclines. Inhibition on M. luteus plates, often by beef and veal samples, could not be confirmed. Circumstantial evidence indicated these test results had to be considered presumptively false positives. Of the samples, 95 inhibited at least one plate seeded with B. subtilis. Usually, samples were positive on more than one plate: 70 samples were positive on all 3 plates, and only 6 samples did not inhibit the plate at pH 6. The majority of positive results on plates seeded with B. subtilis, 77 of 89 samples tested, contained tetracycline antibiotics. One sample also contained sulfadimidine. Two other samples contained high levels of enrofloxacine and ciprofloxacine. The 4-plate test is not sensitive enough to detect sulfonamides and quinolones at the EC maximum residue limits, but higher levels may cause inhibition. The 4-plate test can be used to detect meat samples containing tetracycline residues, but the method is too complicated when used only for that purpose.
LOCATE Enzyme-Linked Immunosorbent Assay for Detection of Salmonella in Food: Collaborative Study
Authors: Gangar Vidhya , Curiale Michael S , D'onorio Armando , Donnelly Carol , Dunnigan Paul ,   Collaborators:, Allen MaryLou , Theresa L Ammons , Baxter Patricia , Brock Gordon , Chenouda Michael , D'Onorio Armando , Dittman Carl , Donnelly Carol , Dunnigan Paul , Finot M , Gale Jason , Gangar Vidhya , Goodall Tracy , Grilli Tony , Guazelli Laura , Gudge Bob , Hagen Brad , Hannon Catherine , Herau M , Hoffman Carrie , Hourani Wendy , Hurlus Jean-Luc , Jaworski Maria , Jost Keating Kathy , Keller Mindy , Kohkur Nausheen , Loser Tony , McNally Steven , Moorman Mark , Naish Neil , Oda William J , Okereke Amechi , Parkin Geniese , Phan Phuong , Raghubeer Errol , Robinson Lorraine , Rogers Cathy , Schnitker Ronald , Schoenfeldt Maricarol , Shah Samir , Skillman Jay , Smythe Glen , Southerton Karen , Sumpter Rita , Walters Janet , Wang Xiao Ming , Wilkinson Carol , Woodruff Ted , Zablan Russell
Published: February 2020

abstract

A collaborative study was performed in 27 laboratories to validate the enzyme-linked immunosorbent procedure LOCATE for rapid detection of Salmonella in foods. Results were read visually and with a microtiter plate reader. The LOCATE method was compared with the Bacteriological Analytical Manual (BAM)/AOAC INTERNATIONAL culture method for detecting Salmonella in 6 foods: milk chocolate, nonfat dry milk, dried whole egg, soy flour, ground black pepper, and ground raw turkey. Two foods—dried whole egg and black pepper—required repeat rounds because insufficient data sets were produced initially (AOAC INTERNATIONAL stipulates a minimum of 15 sets per food type). Each laboratory tested one or more of the 6 foods. A total of 1 439 samples were analyzed, and no significant differences (P <0.05) were observed between LOCATE with either visual or reader detection and BAM/AOAC INTERNATIONAL results. The LOCATE screening method with visual or reader detection is recommended for Official First Action Approval
Measurement of 13C/12 C Ratios of Sugars, Malic Acid, and Citric Acid as Authenticity Probes of Citrus Juices and Concentrates
Authors: Jamin Eric , Gonzalez Javier , Bengoechea Ibon , Kerneur Ghislaine , Remaud Gérald , Naulet Norbert , Martin Gilles G
Published: February 2020

abstract

The carbon-13 content of sugars, malic acid, and citric acid has been determined in authentic orange, lemon, and tangerine juices. After a cleanup step, sugars and organic acids were separated from each other by an anion-exchange process, and pure malic and citric acids were isolated by preparative reversed-phase liquid chromatography. This method has been applied to the stable isotope analysis of citrus juice samples of different botanical and geographical origins and of different years. Correlations between the carbon isotope ratios of all metabolites have been found, and typical ranges for the differences in δ13C values between them have been defined for each fruit. These data provide new tools for detecting adulterations that cannot be detected by the conventional carbon-13 method with the whole juice.
A Simple Membrane Immunobead Assay for Detecting Ciguatoxin and Related Polyethers from Human Ciguatera Intoxication and Natural Reef Fishes
Authors: Hokama Yoshitsugi , Takenaka Warren E , Nishimura Kristi L , Ebesu Joanne S M , Bourke Robert , Sullivan Patrick K
Published: February 2020

A simple membrane immunobead assay (MIA) for detecting ciguatoxin (CTX) and related polyethers directly from fish tissue is presented. A membrane laminated onto a solid plastic support is immersed with a piece of fish tissue in methanol. The membrane is thoroughly dried and placed into an immunobead suspension containing polystyrene particles coated with monoclonal antibody to CTX (MAb-CTX). Two beads of different diameter and color are used. The color intensity of the membrane is related to the concentration of the toxin bound to the membrane. Twelve of 13 fish implicated in human ciguatera fish poisoning showed borderline or positive responses in the assay. A Sphyraena barracuda sample that tested negative with the MIA and was highly toxic with the mouse toxicity bioassay showed only weak CTX-like toxin activity in the guinea pig atrial assay, indicating that the major toxin in the sample was not CTX-like. Examination of 154 routinely caught reef fish from Hawaii, Kosrae, and Kwajalein by MIA found 132 (86℅) negative and 8 (5℅) positive for CTX, with 14 (9℅) giving a borderline response. Fish from Hawaii showed a higher frequency of borderline or positive responses than those from Kosrae and Kwajalein, probably because several species of fish from several islands of Hawaii were tested, whereas only one species from a single area was examined from each of the islands of Kosrae and Kwajalein.
Data Processing and Software Requirement for Analytical Method Validation
Authors: Feinberg Max H
Published: February 2020

Method documentation and validation reports are necessary steps in developing quality assurance programs in laboratories. Consequently, large amounts of data must be stored, archived, and processed in a standardized way. This paper presents these new requirements and proposes a programming approach based on Object Linking and Embedding (OLE) automation technology. Major advantages of this technique include a very flexible and modular programming technique and the possible integration of classically well known software, such as spreadsheets, into the new application. Both advantages reduce development and personnel training costs. Several examples are presented to explain some computing aspects and implementation problems
Determination of Magnesium and Calcium in Foods by Atomic Absorption Spectrometry after Microwave Digestion: NMKL Collaborative Study
Authors: Julshamn Kaare , Maage Amund , Wallin Harriet C ,   Collaborators:, Lierhagen S , Nielsen J , Åsbø E , Engman J , Berg H , Johansson M-L , Liukkonen-Lilja H , Hirvonen A , Højgaard A , Meyland I , Niemi E
Published: February 2020

On the basis of results of the performed collaborative study, the 49th Annual General Meeting of the Nordic Committee on Food Analysis (NMKL) in The Faroe Islands, August 1995, approved this method to be printed and included in NMKL's collection of methods of analysis of foods. Eleven laboratories participated in an interlaboratory methods-performance (collaborative) study of a method for determining magnesium and calcium in foodstuffs by atomic absorption spectrometry (AAS) after wet microwave digestion. The study was preceded by a practice round of familiarization samples. The method was tested on 7 materials: 5 foods (apple, milk powder, minced fish, wheat bran, and chocolate cake) and 2 composite diets ranging in Mg content from 240 to 3900 mg/kg and in Ca content from 290 to 9300 mg/kg. The materials were presented to study participants as blind duplicates, and participants were asked to perform single determinations on each sample. Repeatability relative standard deviations (RSDr) ranged from 1.9 to 4.9% for Mg and from 2.2 to 8.1 % for Ca. Reproducibility relative standard deviations (RSDR) ranged from 4.0 to 13% for Mg and from 5.9 to 23% for Ca. For Ca, lowest RSDR values were found for samples with high concentrations of Ca (>3800 mg/kg sample) and with nitrate ion residues of <1.3% (w/v).
Determination of Small Amounts of Niacin in Vinegar: Comparison of Liquid Chromatographic Method with Microbiological Methods
Authors: Hirayama Shuji
Published: February 2020

An LC method using a new cleanup technique was compared with 2 microbiological methods for determining small amounts of niacin in vinegar. Coefficients of variation for grain vinegar and rice vinegar were 8.33 and 5.3%, respectively, with the LC method, 5.26 and 2.0% with the titrimetric method, and 5.55 and 7.11 % with the turbidimetric method. Among the 3 methods, titrimetry was the most precise. The turbidimetric method tended to yield greater positive error than the titrimetric method. On the other hand, the titrimetric method requires a longer incubation period (72 h) than the turbidimetric method. The LC method using the new cleanup procedure may be useful for routine analysis of small amounts of niacin in vinegars.
Solid-Phase Extraction and Spectrophotometric Determination of Iodate in Table Salt after Azo Dye Formation
Authors: Gosain Shefali , Pandey Madhurima , Verma Krishna K
Published: February 2020

A new reaction for determining iodate in table salt is proposed. It is based on oxidation of phenylhy-drazine-4-sulfonic acid by iodate in acidic medium to the 4-diazobenzenesulfonic acid cation and its electrophilic coupling with N-(1-naphthyl)ethylene- diamine dihydrochloride to give an azo dye, which is measured spectrophotometrically at 545 nm. Maximum molar absorptivity was 8.41 ×104 L/mol cm. A rectilinear calibration graph was obtained for iodate in the range 0.25–5 mg/L. The azo dye could be preconcentrated at least 40-fold by solid-phase extraction on C18 sorbent. The limit of detection was 0.6 μg iodate/L. The method was used to determine iodate in laboratory-prepared and commercially available table salt samples. Up to 5 mg bromate/kg and 10 mg iron(lll)/kg in table salt did not interfere.
Colorimetric Determination of Silver in Synthetically Prepared Ores with Preliminary Separation from Associated Metal Ions by Thin-Layer Chromatography
Authors: Mohammad Ali , Chahar Jay Pal Singh
Published: February 2020

Thin-layer chromatography (TLC) of metal ions on layers of microcrystalline cellulose, alumina G, and their binary mixtures was performed with aqueous solutions of ammonia (NH3), acetic acid (HOAc), sodium acetate (NaOAc), ammonium acetate (NH4OAc), and sodium nitrate (NaNO3) as mobile phases. Ag+ was separated from other metal ions by using a mixed layer with 1.0M aqueous NH3 as mobile phase. Some important binary, ternary, and quaternary separations were achieved. The effect of acid-base equilibria on the retention behavior of Ag+ was examined. After TLC separation, Ag+ was determined quantitatively by spectrophotometry using dithizone solution (in acetone) as chromogenic reagent. The TLC–colorimetric method was applied to recovery of Ag+ from horn silver (AgCI) and argentite (Ag2S).
Performance of Sampling Plans To Determine Aflatoxin in Farmers’ Stock Peanut Lots by Measuring Aflatoxin in High-Risk-Grade Components
Authors: Whitaker Thomas B , Hagler Winston M , Giesbrecht Francis G
Published: February 2020

Five 2 kg test samples were taken from each of 120 farmers’ stock peanut lots contaminated with aflatoxin. Kernels from each 2 kg sample were divided into the following U.S. Department of Agriculture grade components: sound mature kernels plus sound splits (SMKSS), other kernels (OK), loose shelled kernels (LSK), and damaged kernels (DAM). The kernel mass (g), aflatoxin mass (ng), and afla- toxin concentration (ng of aflatoxin/g of peanuts) were measured for each of the 2400 component samples. The variabilities associated with measuring aflatoxin mass (ng) in OK + LSK + DAM, or A(OLD)ng, and in LSK + DAM, or A(LD)ng, and afla-toxin concentration (ng/g) in OK + LSK + DAM, or A(OLD)ng/g, and in LSK + DAM, or A(LD)ng/g, were determined. The variance associated with measuring aflatoxin in each of the 4 combinations of components increased with aflatoxin, and functional relationships were developed from regression analysis. The variability associated with estimating the lot concentration from each of the 4 combinations of components was also determined. The coefficients of variation (CV) associated with estimating the aflatoxin for a lot with aflatoxin at 100 ng/g were 90,86,94, and 96% for aflatoxin masses A(OLD)ng and A(LD)ng and aflatoxin concentrations A(OLD)ng/g and A(LD)ng/g, respectively. The performance of aflatoxin sampling plans using the combination of aflatoxin masses in OK + LD + DAM and LD + DAM components was evaluated with a 2 kg test sample and a 50 ng/g accept/reject limit.
Value Assignment of Retinol, Retinyl Palmitate, Tocopherol, and Carotenoid Concentrations in Standard Reference Material 2383 (Baby Food Composite)
Authors: Sharpless Katherine E , Arce-Osuna Mariana , Thomas Jeanice Brown , Gill Lisa M
Published: February 2020

In 1997, the National Institute of Standards and Technology (NIST) released Standard Reference Material (SRM) 2383 Baby Food Composite. This SRM can be used as a control material when assigning values to in-house control materials and when validating analytical methods for the measurement of proximates, vitamins, minerals, and trace elements in baby foods and similar matrixes. The Certificate of Analysis for SRM 2383 provides certified and reference values for concentrations of lutein, zeaxanthin, β-cryptoxanthin, lycopene, αcarotene, β-carotene, δ-tocopherol, γ-tocopherol, α-tocopherol, retinol, and retinyl palmitate for 2 types of sample preparation—extraction and saponification. The assigned values were based on the agreement of measurements made by NIST and collaborating laboratories. The Certificate of Analysis also provides reference and information values for concentrations of proximates, minerals, and additional vitamins; assignment of these values is discussed in a companion paper (this issue, page 276).
Relevance of Matrix Effect in Determination of Biogenic Amines in Plaice (Pleuronectes platessa) and Whiting (Merlangus merlangus)
Authors: Duflos Guillaume , Dervin Catherine , Malle Pierre , Bouquelet Stephane
Published: February 2020

Spoilage can be evaluated by separating and determining biogenic amines by various techniques, notably high-performance liquid chromatography. Previous studies have not taken into account how the muscle tissue matrix affects the assay. We demonstrate a matrix effect in plaice and whiting and show that it changes during spoilage. This effect should be taken into account when plotting regression lines relating the quantity of amine to the biogenic amine/internal standard ratio.
Determination of Lipids in Infant Formula Powder by Direct Extraction Methylation of Lipids and Fatty Acid Methyl Esters (FAME) Analysis by Gas Chromatography
Authors: Cantellops Dennis , Reid Anne P , Eitenmiller Ronald R , Long Austin R
Published: February 2020

Fatty acid methyl esters (FAMEs) of pure triglyceride standards, oils, and fat from dry matrixes were formed by transesterification using sodium methoxide in methanol–hexane. FAMEs were produced by direct addition of sodium methoxide¯hexane to samples and heating to simultaneously extract and transesterify acyl lipids. FAMEs were quantitated by capillary gas chromatography (GC) over a fatty acid concentration range of 0 to 1.7 mg/mL (r ≥ 0.9997). Total fat was calculated as the sum of individual fatty acids expressed as triglyceride equivalents, in accordance with nutrition labeling guidelines. Saturated, polyunsaturated, and monounsaturated fats were calculated as sums of individual free fatty acids. Absolute recoveries determined from individual fatty acids in test samples ranged from 69.7 to 106%. Recoveries (relative to the C13:0 internal standard) for individual fatty acids in test samples ranged from 95 to 106%. Reproducibility was constant at each fatty acid level in the reaction mixture (n = 5, coefficient of variation [CV] <2%). Absolute recovery determined from the sum of total fatty acids in standard reference material (SRM) 1846 (powdered infant formula) was 96.4%. Analysis of SRM 1846 gave results that agreed closely with the certified fat and fatty acid values. Analysis of commercial infant formula gave results that were comparable to those obtained with AOAC Method 996.01. The direct extraction methylation procedure is rapid, and the transesterification of acyl lipids to form FAMEs is complete within 15 min. Classical saponification and refluxing are not required. This method provides FAMEs free of interferences and easily quantitated by GC or confirmed by GC/mass spectrometry (MS). Unambiguous MS identification of individual FAMEs derived from pure standards, SRM 1846, and powdered infant formula product was obtained.
Liquid Chromatographic Determination of Sulfentrazone in Soil
Authors: Ohmes G Anthony , C Mueller Thomas
Published: February 2020

A rapid method for the determination of sulfentrazone in soils is described. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components through a C18 column, and ultraviolet detection at 220 nm. Recoveries from fortified surface soils were >85% for sulfentrazone. Average relative standard deviations over the soils examined was 7.7%. A conservative lower limit of quantitation for sulfentrazone was 40 ng/g soil.
Determination of Inorganic Arsenic in Marine Food Samples by Hydrochloric Acid Distillation and Flow-Injection Hydride-Generation Atomic Absorption Spectrometry
Authors: Øygard Joar Karsten , Lundebye Anne-Katrine , Julshamn Kåre
Published: February 2020

A simple, rapid, and reliable method was developed for determination of inorganic As in biological samples such as fish fillet. Inorganic AS was distilled from the sample as AsCl3 with HCI. The separated inorganic AS was determined by flow-injection hydride-generation atomic absorption spectrometry after prereduction with Kl and HCI. The influences of various concentrations of Kl, ascorbic acid, and HCI in the prereduction stage; NaBH4 as the reductant; and HCI as the carrier solution on analytical results were studied. Digestion was performed in a Kjeldahl digestion system for 75 min with 4 mL nitric acid and 1 mL sulfuric acid at 380°C. The concentrations of inorganic As in samples were less than 0.1 mg/kg dry weight for fish fillet and somewhat higher for crustaceans and bivalve molluscs. The total and inorganic As contents of various marine biological samples and certified reference materials were determined.
Analysis of Fumigant Residues—A Critical Review
Authors: Desmarchelier James M , Ren Yong-Lin
Published: February 2020

This review concentrates on the main fumigants currently applied to commodities: phosphine (PH3) and methyl bromide (CH3Br). It discusses possible new fumigants, such as carbonyl sulfide (COS) and ethyl formate (EtF), that may be able to be applied in such a way that “residues” after fumigation do not exceed the range of natural levels. The review aims to raise some general issues and to suggest some general conclusions from a synthesis of studies on analytical chemistry and on fumigant behavior.
Use of Biogenic Amines to Evaluate Spoilage in Plaice (Pleuronectes platessa) and Whiting (Merlangus merlang)
Authors: Duflos Guillaume , Dervin Catherine , Malle Pierre , Bouquelet Stephane
Published: February 2020

Fish muscle decarboxylases generate biogenic amines during spoilage. We monitored spoilage in plaice and whiting by assaying biogenic amines represented by the amine index (Al), and by using expert assessors to determine a freshness index (Fl) for each fish. First we characterized the assessor- and fish species-related effects on Fl, and then we sought to correlate changes in Al and Fl by statistical data analysis. We propose rejection limits on the basis of our findings.
Rapid Immunoaffinity-Based Method for Determination of Zearalenone in Corn by Fluorometry and Liquid Chromatography
Authors: Kruger Scott C , Kohn Barb , Ramsey Catherine S , Prioli Reginaldo
Published: February 2020

An immunoaffinity-based method was developed to determine zearalenone in corn. Corn samples were extracted in acetonitrile-water (90 + 10, v/v), applied to an immunoaffinity column, and eluted with methanol. The isolated toxin was quantitated either by reaction with aluminum chloride hexahydrate (AlCl33.6H2O) prior to measurement with a fluorometer or injection into a liquid chromatographic (LC) system with a fluorescence detector. Performance was evaluated in terms of antibody specificity, limit of detection, percentage recovery, precision, column capacity, assay linearity, and comparison with AOAC Official Method 985.18. With the immunoaffinity column cleanup procedure, only zearalenone and its metabolites were recognized by the antibody (≥75% recovery). Limits of detection were 0.10 μg/g for the fluorometer and 0.10 or 0.0025 μg/g (sensitive method) for the LC method. Percentage recovery averaged 105% (fluorometer) and 93% (LC method), with average relative standard deviations (RSDs) of 15.7 and 9 .3%. Naturally contaminated samples gave comparable RSDs of 8.3 and 9.9% for the fluorometer and LC methods, respectively. Column capacity was 4.0 μg with 89% recovery. Assay linearity was comparable for both methods (r2 = 0.998). Optimum assay ranges were 0.10-5.0 μg/g for the fluorometer and 0.10-50 or 0.0025-5.0 μg/g (sensitive method) for the LC method. Comparative analysis of 17 naturally contaminated corn samples using ZearalaTest LC and the official AOAC LC method for detection of zearalenone showed that ZearalaTest is statistically comparable to the AOAC Official Method 985.18 (r2 = 0.747).
Evaluation of the Novel Soxflo Technique for Rapid Extraction of Crude Fat in Foods and Animal Feeds
Authors: Brown Ron H , Mueller-harvey Irene
Published: February 2020

The new Soxflo instrument was evaluated for the determination of crude fat in foods and animal feeds. Samples are packed into small columns and extracted with petroleum ether at room temperature. The Soxflo yielded accurate data from foods, ranging from 0.4 to 73.2% crude fat, compared with Soxhlet extractions and Certified Reference Materials, for which recoveries averaged 99.7 and 100.7%, respectively. Relative standard deviations (1.81 %) were approximately half those of Soxhlet extractions (3.68%). Regression analysis of the data suggested that there was no proportional bias. A small but acceptable constant bias was measured. Soxflo extractions are easy to perform and take approximately 1 h to complete. The main difference between the Soxflo and Soxhlet techniques lies in the extraction procedure. Estimated savings during extractions are in time (85% reduction), energy (95%), cooling water (100%), and solvents (50%). Soxflo extractions are, therefore, more environmentally friendly than Soxhlet extractions.
Beware of Bar Charts for Plotting Calibration Curves for Analytical Method Development
Authors: Shayanfar Ali
Published: February 2020

Some researchers, in their published articles in authentic scientific journals, plot calibration curves using bar charts instead of scatter plots using common software such as Excel. Bar charts can significantly affect the apparent linear range and sensitivity of the developed method, and using bar charts as calibration curves gives the wrong results. Therefore, this issue should be considered by researchers in developing analytical methods.
Long-term health-related quality of life in pediatric brain tumor survivors receiving proton radiotherapy at <4 years of age
Authors: Eaton Bree R , Goldberg Saveli , Tarbell Nancy J , Lawell Miranda P , Gallotto Sara L , Weyman Elizabeth A , Kuhlthau Karen A , Ebb David H , MacDonald Shannon M , Yock Torunn I
Published: February 2020

Background

The purpose of this analysis is to report long-term health-related quality of life (HRQoL) among brain tumor survivors treated with proton therapy (PRT) at a very young age.

Methods

Fifty-nine children <4 years old received PRT between 2000 and 2011. Forty families participated. HRQoL was assessed by child self-report (CSR; age ≥5) and parent proxy report (PPR; age 2+) using the PedsQL Core.

Results

The median age was 2.5 years (range, 0.3–3.8) at PRT and 9.1 years (5.5–18) at last follow-up. The most common diagnoses were ependymoma (n = 22) and medulloblastoma (n = 7). Median follow-up is 6.7 years (3–15.4). Follow-up mean CSR and PPR scores were: total core (78.4 and 72.9), physical (82.9 and 75.2), psychosocial (76.0 and 71.6), emotional (74.4 and 70.7), social (81.2 and 75.1), and school (72.4 and 69.9). Parent-reported HRQoL fell within a previously defined range for healthy children in 37.5% of patients, and for children with severe health conditions in 45% of patients. PPR HRQoL was stable from baseline to last follow-up among all domains except for social functioning. History of gastrostomy tube was significantly associated with poorer CSR and PPR HRQoL on multivariable analysis. Ninety percent of children functioned in a regular classroom, 14 (36%) used a classroom aid, 9 (23%) used an outside tutor, and 18 (46%) had an individualized education plan.

Conclusion

Long-term HRQoL among brain tumor survivors treated with PRT at a very young age is variable, with over a third achieving HRQoL levels commensurate with healthy children.

Key Points

1. One third of survivors reported long-term HRQoL scores comparable to those of healthy children.

2. Treatment for hydrocephalus or a feeding tube was associated with significantly lower HRQoL.

3. Total core HRQoL scores remained stable from baseline to last follow-up.
Predicting Long-Term Outcomes After Poor-Grade Aneurysmal Subarachnoid Hemorrhage Using Decision Tree Modeling
Authors: Liu Jinjin , Xiong Ye , Zhong Ming , Yang Yunjun , Guo Xianzhong , Tan Xianxi , Zhao Bing
Published: February 2020

BACKGROUND

Despite advances in the treatment of poor-grade aneurysmal subarachnoid hemorrhage (aSAH), predicting the long-term outcome of aSAH remains challenging, although essential.

OBJECTIVE

To predict long-term outcomes after poor-grade aSAH using decision tree modeling.

METHODS

This was a retrospective analysis of a prospective multicenter observational registry of patients with poor-grade aSAH with a World Federation of Neurosurgical Societies (WFNS) grade IV or V. Outcome was assessed by the modified Rankin Scale (mRS) at 12 mo, and an unfavorable outcome was defined as an mRS of 4 or 5 or death. Long-term prognostic models were developed using multivariate logistic regression and decision tree algorithms. An additional independent testing dataset was collected for external validation. Overall accuracy, sensitivity, specificity, and area under receiver operating characteristic curves (AUC) were used to assess model performance.

RESULTS

Of the 266 patients, 139 (52.3%) had an unfavorable outcome. Older age, absence of pupillary reactivity, lower Glasgow coma score (GCS), and higher modified Fisher grade were independent predictors of unfavorable outcome. Modified Fisher grade, pupillary reactivity, GCS, and age were used in the decision tree model, which achieved an overall accuracy of 0.833, sensitivity of 0.821, specificity of 0.846, and AUC of 0.88 in the internal test. There was similar predictive performance between the logistic regression and decision tree models. Both models achieved a high overall accuracy of 0.895 in the external test.

CONCLUSION

Decision tree model is a simple tool for predicting long-term outcomes after poor-grade aSAH and may be considered for treatment decision-making.
Detection of H3N8 influenza A virus with multiple mammalian-adaptive mutations in a rescued Grey seal (Halichoerus grypus) pup
Authors: Venkatesh Divya , Bianco Carlo , Núñez Alejandro , Collins Rachael , Thorpe Darryl , Reid Scott M , Brookes Sharon M , Essen Steve , McGinn Natalie , Seekings James , Cooper Jayne , Brown Ian H , Lewis Nicola S
Published: February 2020

Avian influenza A viruses (IAVs) in different species of seals display a spectrum of pathogenicity, from sub-clinical infection to mass mortality events. Here we present an investigation of avian IAV infection in a 3- to 4-month-old Grey seal (Halichoerus grypus) pup, rescued from St Michael’s Mount, Cornwall in 2017. The pup underwent medical treatment but died after two weeks; post-mortem examination and histology indicated sepsis as the cause of death. IAV NP antigen was detected by immunohistochemistry in the nasal mucosa, and sensitive real-time reverse transcription polymerase chain reaction assays detected trace amounts of viral RNA within the lower respiratory tract, suggesting that the infection may have been cleared naturally. IAV prevalence among Grey seals may therefore be underestimated. Moreover, contact with humans during the rescue raised concerns about potential zoonotic risk. Nucleotide sequencing revealed the virus to be of subtype H3N8. Combining a GISAID database BLAST search and time-scaled phylogenetic analyses, we inferred that the seal virus originated from an unsampled, locally circulating (in Northern Europe) viruses, likely from wild Anseriformes. From examining the protein alignments, we found several residue changes in the seal virus that did not occur in the bird viruses, including D701N in the PB2 segment, a rare mutation, and a hallmark of mammalian adaptation of bird viruses. IAVs of H3N8 subtype have been noted for their particular ability to cross the species barrier and cause productive infections, including historical records suggesting that they may have caused the 1889 pandemic. Therefore, infections such as the one we report here may be of interest to pandemic surveillance and risk and help us better understand the determinants and drivers of mammalian adaptation in influenza.
Terminal Ulcers, SCALE, Skin Failure, and Unavoidable Pressure Injuries: Results of the 2019 Terminology Survey
Authors: Sibbald R. Gary , Ayello Elizabeth A.
Published: February 2020

This article reports the results of a global wound care community survey on Kennedy terminal ulcers, Skin Changes At Life’s End, Trombley-Brennan terminal tissue injuries, skin failure, and unavoidable pressure injury terminology. The survey consisted of 10 respondent-ranked statements to determine their level of agreement. There were 505 respondents documented. Each statement required 80% of respondents to agree (either “strongly agree” or “somewhat agree”) for the statement to reach consensus. Nine of the 10 statements reached consensus. Comments from two additional open-ended questions were grouped by theme. Conclusions and suggested recommendations for next steps are discussed. This summary is designed to improve clinical care and foster research into current criteria for unavoidable skin changes at the end of life.

GENERAL PURPOSE

To present the results of the 2019 study of healthcare professionals’ consensus and opinions regarding terminology for terminal ulcers, Skin Changes At Life’s End, skin failure, and unavoidable pressure injuries to improve clinical care and to foster research into current criteria for unavoidable skin changes at the end of life.

TARGET AUDIENCE

This continuing education activity is intended for physicians, physician assistants, NPs, and nurses with an interest in skin and wound care.

LEARNING OBJECTIVES/OUTCOMES

After completing this continuing education activity, the participant should be better able to:

1. Explain the survey methodology and identify the consensus statements.

2. Synthesize the open-ended questions and respondent comments and their implications for clinical care and research.