bluuebunny/crossref_metadata_2025_split huggingface dataset:
Ergot Alkaloids in Grain Foods Sold in Canada
Authors: Scott Peter M , Lombaert Gary A , Pellaers Peter , Bacler Stanley , Lappi Judy 
Published: February 2020

Abstract
Six pharmacologically active ergot alkaloids (ergonovine [ergometrine], ergosine, ergotamine, ergocornine, α-ergokryptine, and ergocristine) were determined by liquid chromatography with fluorescence detection in over 400 samples of grain foods. The survey was conducted over a 6-year period for rye flour, wheat flour, and bran/bran cereal, and a 5-year period for rye bread/crispbread; triticale flour was analyzed over a total of 3 years. The predominant alkaloids found were ergocristine and ergotamine. Rye flour was the most contaminated food; the incidence of alkaloid-positive samples was 118/128, annual mean concentrations of total alkaloids in positive samples ranged from 70 to 414 ng/g, and 1 sample contained as high as 3972 ng total alkaloids/g. In wheat flour, total alkaloid concentrations were much lower than in rye flour, with annual means in positive samples (68/93) of 15-68 ng/g. Bran/bran cereal had alkaloid concentrations similar to those in wheat flour, with annual means of 12-69 ng total alkaloids/g positive samples (incidence 29/35). Triticale flour was also an important source of ergot alkaloids; incidence was 24/26, and annual mean total alkaloid concentrations in positive samples were 46-283 ng/g. Ergot alkaloids were found in rye bread (46/100) and other heat-processed rye flour products (6/14). Annual mean total alkaloids in positive rye bread/crispbread samples ranged from 4.8 to 100 ng/g; the latter included a sample with 1248 ng total alkaloids/g.
Liquid Chromatographic Determination of Fumonisins B1 and B2 in Corn and Corn Products
Authors: Stack Michael E , Eppley Robert M 
Published: February 2020

Abstract
A liquid chromatographic (LC) method is described for determining fumonisin B1 (FB1) and fumonisin B2 (FB2), metabolites of Fusarium moniliforme, in corn and corn products. The metabolites are extracted with methanol-water (3 + 1), and the extract is added to a disposable strong anion exchange column. After the FB1 and FB2 are eluted from the column with methanol-acetic acid (199-1-1) and the eluate is evaporated to dryness, the metabolites are derivatized with o-phthaldialdehyde and 2- mercaptoethanol to make highly fluorescent derivatives. Reversed-phase LC with fluorescence detection is used for the final separation and determination. The estimated limit of quantitation is 10 ng/g for each metabolite. The average recoveries from corn were 67% for FB1 and 71% for FB2, with relative standard deviations of 5% for FB1 and 3% for FB2. The identities of the fumonisins were confirmed by mass spectrometry. Applications of the method include the analyses of corn meal and breakfast cereals.
Co-occurrence of Cyclopiazonic Acid and Aflatoxins in Corn and Peanuts
Authors: Urano Takashi , Trucksess Mary W , Beaver Rodney W , Wilson David M , Dorner Joe W , Dowell Floyd E 
Published: February 2020

Abstract
Fifty samples of peanuts and 45 samples of com, collected in Georgia during 1990, were examined for the co-occurrence of cyclopiazonic acid (CPA) and aflatoxins (AF). The corn was collected from fields in Georgia, before harvest, under the mycotoxin- monitoring program of the U.S. Department of Agriculture's Agricultural Research Service. The peanuts were designated for oil production or animal feed because of visible damage to the nutmeats. CPA was determined by reversed-phase liquid chromatography (RPLC) using a linear gradient. Solvent A was methanol-water (85 +15), and solvent B was 4 mM ZnS04 in methanol-water (85 +15). The gradient started at 0% B and reached 100% B at 10 min. AF were determined by RPLC with postcolumn iodination. Of the 45 corn samples analyzed, 51 % were contaminated with CPA (&lt;25-2800 ng/g, av. 467 ng/g), and 87% were contaminated with AF (1-2300 ng/g, av. 252 ng/g). Of the 50 peanut samples, 90% contained CPA (&lt;50- 2900 ng/g, av. 460 ng/g), and 100% contained AF (3- 22 000 ng/g, av. 1685 ng/g). The identity of CPA was confirmed in selected samples of corn and peanuts by mass spectrometry.
Determination of Polynuclear Aromatic Hydrocarbons in Seafood by Liquid Chromatography with Fluorescence Detection
Authors: Perfetti Gracia A , Nyman Patricia J , Fisher Sheryl , Joe Frank L , Diachenko Gregory W 
Published: February 2020

Abstract
Modification of a previously published method for determination of polynuclear aromatic hydrocarbons (PAHs) produces very clean seafood extracts in less than half the time. After alkaline digestion of the seafood, PAHs were partitioned into 1,1,2- trichlorotrifluoroethane. The resulting extract was cleaned up by solid-phase extraction on alumina, silica, and C18 adsorbents and then analyzed by gradient reversed-phase liquid chromatography with programmable fluorescence detection. Average recoveries of 12 PAHs [acenaphthene, anthracene, fluoranthene, pyrene, benz(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)- fluoranthene, benzo(a)pyrene, dibenz(a,h)anthracene, benzo(ghi)perylene, and indeno(1,2,3-cd)pyrene] from 5 different matrixes (mussels, oysters, clams, crabmeat, and salmon) spiked at low partsper- billion levels ranged from 76 to 94%. Estimated limits of quantitation ranged from 0.01 to 0.6 ppb PAHs in extracts that were free of matrix interferences. Results of analyses of a mussels standard reference material obtained from the National Institute of Standards and Technology were in good agreement with the certified values.
Determination and Confirmation of cis-9-Tricosene in Technical Materials by Capillary Gas Chromatography and Gas Chromatography/Mass Spectrometry
Authors: Ko Jinren , Nguyen Jack , Burleson Jim 
Published: February 2020

Abstract
A capillary gas chromatographic (GC) method was developed for the quantitation of cis-9-tricosene in technical material. This method is capable of resolving cis-9-tricosene from the trans-9-tricosene isomer and other impurities in technical 9-tricosene. Samples are dissolved in methylene chloride and analyzed by splitless GC using docosane as an internal standard. The integrity and purity of the peak of interest were confirmed by GC/mass spectrometry. The overall recovery of this method was 101.3 ± 0.82%. The correlation coefficient of the standard calibration curve was 0.9999. The system and method precision for cis-9-tricosene were 0.18 and 0.20%, respectively. The reproducibility of the method by different analysts was within 0.5%.
Determination of Total Vitamin C in Various Food Matrixes by Liquid Chromatography and Fluorescence Detection
Authors: Dodson Karen Y , Young Edna R , Soliman Abdel-Gawad M 
Published: February 2020

Abstract
A liquid chromatographic method was developed for quantitation of total vitamin C content in various food matrixes. The method includes extraction with 3% mete-phosphoric acid-acetic acid and oxidation of ascorbic acid to dehydroascorbic acid with Norit, followed by reaction with ophenylenediamine to form a fluorescent derivative. The fluorescent derivative is separated on a µBondapak C18 (10 µm) column with methanol-water (55 + 45) and detected fluorometrically. This method is demonstrated to be suitable for several sample matrixes, including complex matrixes of canned corn, potatoes, green beans, potato chips, and cereals. Other products analyzed include infant formula, medical foods, fruit juice, and multivitamin tablets. Recoveries are in the range of 90-108%. Comparison of results with those by the AOAC fluorometric method shows excellent agreement.
Liquid Chromatographic Assay for Naphazoline and Antazoline in Ophthalmic Preparations
Authors: Bocic Ronny , Vallejos Cristobal , Alvarez-Lueje Alejandro , LÓpez Fernando 
Published: February 2020

Abstract
A liquid chromatographic (LC) analysis has been developed for determining naphazoline and antazoline in ophthalmic preparations. The LC system is designed so that a variety of ophthalmic solutions containing naphazoline and antazoline can be analyzed with precision.
Determination Of Total Fat In Meat And Meat Products By Solvent Extraction After Hydrochloric Acid Hydrolysis: NmkL Interlaboratory Study
Authors: Croon Lars-Börje , Wallin Harriet C 
Published: February 2020

Abstract
A gravimetric method including acid hydrolysis and solvent extraction according to SBR (Schmid, Bondzynski, and Ratzlaff) for the determination of total fat in meat and meat products was collaboratively studied in 12 laboratories. The study aimed at investigating whether an older SBR method for the determination of fat in meat and meat products, published by the Nordic Committee on Food Analysis in 1974, could be simplified without significant losses in precision. The study samples consisted of 12 materials in the form of 6 matched pairs of meat types: ham, beef trimmings, pork loin, black pudding, sausage, and liver pate. The fat contents of the samples varied between 2.6 and 44.4 g fat per 100 g. The participating laboratories were asked to analyze the samples by both the old and the new methods. The results indicated that there was no significant difference between the results obtained by the 2 methods. The precision of the revised method in most respects meets the U.S. Department of Agriculture, Food Safety and Inspection Service requirements on methods for the analysis of meat and meat products. The relative standard deviation for repeatability of the method varied from 0.93% for the 44.5 g/100 g level of fat to 4.5% for the 2.5 g/100 g level. The relative standard deviation for reproducibility varied correspondingly between 1.2 and 6.1%. For samples with a fat content &lt;5 g/100 g, the revised method gave somewhat lower fat concentrations than the older method. However, the mean differences were small and did not exceed the precision (repeatability and reproducibility) of the method. Ten of the 12 participating laboratories found the revised method easier to work with than the original method
Optimization, Automation, and Validation of the Solid-Phase Extraction Cleanup and On-Line Liquid Chromatographic Determination of N-Methylcarbamate Pesticides in Fruits and Vegetables
Authors: De Kok André , Hiemstra Maurice 
Published: February 2020

Abstract
A fully automated liquid chromatographic (LC) method was developed for the determination of 21 N-methylcarbamates and 12 of their metabolites. Our previously developed solid-phase extraction (SPE) cleanup method can now be performed using an automated SPE cleanup apparatus. The cleaned-up extract is injected on-line into the LC carbamate analysis system, which is based on a reversed- phase LC separation, postcolumn hydrolysis of the carbamates on a solid-phase catalyst, reaction of the methylamine formed with ophthalaldehyde reagent, and fluorescence detection of the derivatives. The optimized method was evaluated. Recovery and repeatability data were collected for 13 representative carbamates and 12 metabolites on 12 different food product types. The reliability of the method in routine analysis of fruit and vegetable samples is demonstrated. Registration of the analytical results of control samples in Shewhart charts during a year of routine analysis has demonstrated the excellent performance of this complete method. The limits of determination are in the 5-50 μg/kg (ppb) range. Sample throughput is about 20 per 24 h. Data are presented on real residues of N-methylcarbamates found in fruits and vegetables during 4 years of routinely applying this multiresidue method
Liquid Chromatographic Determination of Methazole in Technical and Formulated Products: Collaborative Study
Authors: Belkind Benjamin A 
Published: February 2020

Abstract
An isocratic normal-phase liquid chromatographic (LC) method for measuring methazole in technical and formulated products was collaboratively studied by 12 laboratories. Samples of technical or formulated products are dissolved in 1,4-dioxane-hexane containing 2-chloro-5-nitrobenzophenone as internal standard. Following centrifugation and further dilution, the sample is analyzed by LC on a 25 cm x 4.6 mm stainless steel column packed with 5 μm silica, with ultraviolet detection at 254 nm. Premixed 1% 2-propanol in hexane is used as the mobile phase. Peak areas are obtained at the retention times corresponding to the internal standard and methazole. The quantity of active ingredient is determined by comparing the area ratio of active ingredient to internal standard in the sample with the same ratio in a single calibration solution. Collaborators were provided with 1 Youden matched pair for each of the technical, 75% wettable granular, and 4 lb/gal flowable products studied. The reproducibility relative standard deviations (RSDR) for the product types studied were 1.05% for technical, 1.80% for granular, and 4.76% for flowable. The method has been adopted first action by AOAC International.
δ18 Measurements in Water for Detection of Sugar
Beet-Derived Syrups in Frozen Concentrated Orange Juice:
Collaborative Study
Authors: Doner, Landis W , Brause Allan R , Petrus Donald R 
Published: February 2020

Abstract
Stable isotope ratio mass spectrometry has shown that pure frozen concentrated orange juices (FCOJ) of 63-67° brix possess a mean δ18 value of +14.28%o, with a standard deviation of 1.80. Beet invert syrups, which are produced using ground water, possess negative values. As a result, δ18 values decrease on addition of such syrups to FCOJ. Samples with values less than +8.9%o (3 standard deviations from the mean for pure FCOJs) can confidently be considered as adulterated. A collaborative study was conducted in which a pure FCOJ and 4 samples adulterated to various levels with medium beet invert syrup were sent to each of 6 collaborators. In all but 2 instances, juices containing more than 10% beet syrup would have been classified as adulterated by the collaborators; none would have classified pure juice as adulterated. The plot of mean δ18 values for all collaborators at each adulteration level has a correlation coefficient &gt;0.999. The method has been adopted first action by AOAC International.
Rapid Isolation Of The Sterol Fraction In Edible Oils
Using A Silica Cartridge
Authors: Bello Ada C 
Published: February 2020

Abstract
A commercial silica cartridge was used successfully to separate the fraction of the unsaponifiable components of edible oils containing the sterols and some related compounds. Analysis by gas chromatography indicates that there is good agreement between the results from samples obtained by the new rapid method and those isolated using the time-consuming thin-layer chromatographic technique. This paper presents comparison data for 7 vegetable oils (peanut, soy, corn, rapeseed, olive, sesame, and coconut), a 2-component blend (olive and soy), and a commercial milk product erroneously labeled cholesterol-free.
Comparison of Analytical Methods Used to Determine
Metal Concentrations in Environmental Water Samples
Authors: Davis Andy , Olsen Roger 
Published: February 2020

Abstract
Al, Cd, Cu, Fe, Pb, Mn, and Zn were determined in water samples collected from Clear Creek and North Clear Creek, CO, that had been impacted by acid mine drainage. These samples contained a wide range of total suspended solid concentrations. The samples were prepared and digested by dissolved, acid-soluble, total recoverable, U.S. Environmental Protection Agency (EPA total), and Contract Laboratory Program (CLP) total procedures. The CLP method resulted in the highest reported metal concentrations for 67% of the analyses (primarily Al, Cd, Cu, and Fe), the EPA total method for 11 % of the analyses (mainly Mn and Zn), and the acid-soluble method for 9% of the analyses. For the remainder (13%), 2 or more methods resulted in similar metal concentrations. The same analyses using the Three Kids Mine standard reference material demonstrated that the EPA total and total recoverable methods underestimate the maximum metal concentrations in sediment-bearing water samples. In addition, use of acid-soluble or total methods is inappropriate to determine compliance with aquatic water quality standards that were originally promulgated on the basis of dissolved concentrations
Extraction of Light Filth from Oriental Sauces Containing Soy Sauce, Thickeners, and Spices: Collaborative Study
Authors: Nakashima Marvin J ,   Collaborators:, Gallman J A , Haynos R R , Highfield C E , Kelly G P , Loechelt H K , Millward P A , Ocus W , Rodriguez A , Wirth M D 
Published: February 2020

Abstract
Results are reported for a collaborative study of a method for the extraction of light filth from oriental sauces containing soy sauce, thickeners, and spices. A100 g test portion is pretreated in a 2% solution of Tergitol Anionic 4 over a steam bath, and oils are removed by wet-sieving on No. 230 sieve. Filth is isolated from 40% isopropanol by using Na4EDTA and mineral oil. Average recoveries by 9 collaborators for 3 spike levels of rat hairs (5,10, and 15) were 84, 78, and 79%, respectively; for insect fragments (5,15, and 30), recoveries were 92, 95, and 96%, respectively. The method was adopted first action by AOAC International.
Enzymatic Determination of Sulfite in Foods: NMKL Interlaboratory Study
Authors: Edberg Ulla ,   Collaborators:, Anttonen Maija-Liisa , Berg-Nilsen Karen , Blomberg Karin , Gjerstad Karl Olav , Gustavsson Tomas , Joner Per , Loimaranta Jukka , Mustranta Antti , Oksanen Mikko , Pero Leena , Sönsterud Björn 
Published: February 2020

Abstract
An enzymatic method for the determination of sulfite in foods was collaboratively studied in Nordic industry and government laboratories. The sulfite in liquid foods or extracts of solid foods is analyzed according to the following principle: Sulfite ions are oxidized to sulfate ions by oxygen in the presence of sulfite oxidase, thereby forming hydrogen peroxide. Hydrogen peroxide is transformed to water by reduced nicotinamide adenine dinucleotide (NADH) in the presence of NADH peroxidase. In this reaction, NAD+ is formed (and NADH is consumed) in amounts proportional to the sulfite concentration. Consumption of NADH can be measured spectro photo metrically at 340 nm. The method was collaboratively tested in 2 separate studies with high and low levels of sulfite tested. Results of both studies are reported here. The study samples consisted of potato flakes, wine, juice, and dried apples containing between 0 and about 960 mg SCVkg. Eleven laboratories participated in the full study and analyzed 12 samples. Six laboratories analyzed 8 samples in the complementary study. Before statistical evaluation of the collaborative study data, results were adjusted for the time-dependent decrease of sulfite in the case of materials with high sulfite content (dried apples and wine). For 2 blind duplicate samples of wine containing 75 mg S02/kg, the relative standard deviation for repeatability (RSDR, within-laboratory variation) was 3.9%. Relative standard deviation for reproducibility (RSDR, between-laboratory variation) was 7.6%. For 2 samples of dried apples containing 800 and 960 mg S02/kg, an RSDr value of 13.3% and an RSDR value of 13.9% were calculated. The corresponding parameters for 2 juice samples containing about 270 mg S02/kg were 4.8 and 10.4% for repeatability and reproducibility, respectively.
Matrix Solid-Phase Dispersion Extraction and Gas Chromatographic Screening of 14 Chlorinated Pesticides in Oysters (Crassostrea virginica)
Authors: Lott Heidi M , Barker Steven 
Published: February 2020

Abstract
A multiresidue isolation technique known as matrix solid-phase dispersion (MSPD) is presented for the extraction and subsequent gas chromatographic/electron capture detection (GC/ECD) determination of 14 chlorinated pesticides (α-BHC, (β-BHC, lindane, heptachlor, aldrin, heptachlor epoxide, p,p’-DDE, dieldrin, endrin, 4,4’-DDD, endrin aldehyde, p,p’-DDT, endosulfan sulfate, and methoxychlor) from oysters (Crassostrea virginica). Pureed whole oysters (0.5 g aliquots) are fortified with the 14 pesticides and δ-BHC, as an internal standard, and blended with 2 g C18 (octadecylsilyl)-derivatized silica. Pesticides are eluted from an extraction column composed of C18/oyster matrix blend and 2 g activated Florisil by addition of 8 mL acetonitrile-methanol (90 + 10). Then, 2 μL of the eluate is analyzed by GC/ECD. Unfortified blank controls are treated similarly. The eluate contained all the pesticide analytes and was free of interfering coextractants. Correlation coefficients for the standard curves of the 14 extracted pesticides (linear regression analysis) ranged from 0.9849 to 0.9980. Average relative percent recoveries over the range of concentrations examined (66 ± 12.7% to 84 ± 25.3%, n = 25 for each pesticide), interassay variability (13.6 ± 8.8% to 30.2 ± 9.1 %, n = 25 for each pesticide), and intra-assay variability (5.8-11.8%, n = 5 for each pesticide) indicated that the MSPD methodology successfully extracted and determined the 14 chlorinated pesticides in oyster at levels of 31.3-500 ng/g.
Determination of Oxyfluorfen in Pesticide Formulations by Liquid Chromatography
Authors: Bushway Rodney J , Perkins Lewis B 
Published: February 2020

Abstract
A normal-phase liquid chromatographic method was developed to determine oxyfluorfen, a herbicide, in pesticide formulations. Technical and liquid formulations were dissolved in 10% water and 90% tetrahydrofuran. A 5 μL aliquot was injected into a Phenomenex Spherex amino column and monitored at 240 nm. The mobile phase was tetrahydrofuran-hexane (5 + 95). Total analysis time was 80 min. Six different liquid formulations and 1 solid formulation were analyzed. Within-day percent coefficients of variation (%CVs) ranged from 0.5 to 3.5, and between-day %CVs ranged from 1.4 to 3.9. Purity of each oxyfluorfen chromatographic peak was checked by using a photodiode array detector in the spectrum mode. No interferences were observed.
Determination of Cymiazole Residues in Honey by Liquid Chromatography
Authors: Cabras Paolo , Melis Marinella , Spanedda Lorenzo 
Published: February 2020

Abstract
A liquid chromatographic method is described for the determination of cymiazole residues in honey. This acaricide is determined on a reversed-phase (C18) column, with a CH3CN-O.OOIN HCI-NaCI mixture (950 mL + 50 mL + 0.3 g/L) as the mobile phase, and UV detection at 265 nm. Cymiazole is extracted with n-hexane from aqueous alkalinized (pH 9) honey solutions. No further cleanup of the honey extract was required before chromatographic analysis. Recoveries on control samples fortified with 0.01,0.10, and 1.00 ppm cymiazole ranged from 92 to 102%. The limit of determination was 0.01 ppm.