bluuebunny/crossref_metadata_2025_split huggingface dataset:
Analytical Methods for Foods in the Next Decade
Authors: Tanner James T 
Published: February 2020

Abstract
With each passing decade new problems arise for the regulatory analytical chemist. The push for low detection limits from percent to parts per million to parts per billion brought the need for new and improved analytical instrumentation followed by questions of reliability at such low values. Each question has been met by new instruments or techniques and critical studies. The question for the 1980s is not how to achieve low detection limits but how to reliably and rapidly perform analyses at low values. During the 1960s the emphasis was on the single component/element techniques. We seem now to be entering the computer-controlled era. In each analytical specialty, computer-controlled instruments are offered which greatly aid the analyst in producing an accurate, reliable analysis in a shorter time. The advantage of larger numbers of analyses per unit of time with, in some cases, reduced personnel are not to be overlooked in this age of economy. To the AOAC collaborative study this means a reduction in the number of laboratories who can participate. It also means greater standardization of methodology, and the chemist’s laboratory ability becomes less of a factor in producing reliable analyses. Specific analytical examples are discussed to illustrate the trend for the 1980s.
Malt Beverages and Brewing Materials: Screening and Confirmatory Methods for Nitrosamines in Beer
Authors: Cutaia Anthony J 
Published: February 2020

Abstract
Screening methods for nitrosamines in beer were studied by 15 collaborators. Collaborators studied 4 extraction techniques and 2 calculation procedures. All methods showed acceptable recoveries and no significant differences between methods. Based on accuracy, simplicity and speed, the Celite extraction with internal standard calculation is recommended. Fifteen collaborators also studied a distillation confirmatory method compared with a direct extraction with dichloromethane. Because the former gives an extract more suitable for mass spectrometric confirmation of nitrosamines, it is the recommended reference method. The screening and confirmatory methods have been adopted official first action.
Mass Spectrometric 13C/12C Determinations to Detect High Fructose Corn Syrup in Orange Juice: Collaborative Study
Authors: Doner Landis W , Bills Donald D ,   Collaborators:, Carro O , Drimmie R , Fritz P , Gearing J N , Marcel C Hillaire , Parker P L , Reeseman R M , Smith B N , Ziegler H 
Published: February 2020

Abstract
The 13C/12C ratios in orange juice are sufficiently uniform and different from those in high fructose corn syrup (HFCS) so that the addition of HFCS to orange juice can be detected. HFCS averages –9.7‰ (parts per thousand) δ13C, orange juice averages —24.5‰, and mixtures of HFCS and orange juice possess intermediate values. One pure orange juice and 4 orange juice-HFCS mixtures containing from 25 to 70% orange juice were properly classified by 7 collaborators. Samples with δ13C values less negative than — 22.1‰, 4 standard deviations from the mean of pure juices, can, with a high degree of confidence, be classified as adulterated. Samples with values more negative than —22.1‰ must be considered unadulterated with HFCS, because pure orange juices possess a range of δ13C values. The 13C/12C mass spectrometric method was adopted official first action for detecting HFCS in orange juice.
Graphite Furnace Atomic Absorption Spectrophotometric Determination of 4-Hydroxy-3-Nitrobenzenearsonic Acid, Other Organic Arsenicals, and Inorganic Arsenic in Finished Animal Feed
Authors: George Glenn M , Frahm Larry J , McDonnell J Patrick 
Published: February 2020

Abstract
4-Hydroxy-3-nitrobenzenearsonic acid (roxarsone) is administered in animal feed as a growth stimulant over a concentration range of 25-50 ppm. The drug is extracted from 5 g feed with 200 mL aqueous 1.0% ammonium carbonate solution and 5 min of mechanical shaking. Undissolved feed particles are allowed to settle and 1.0 mL aliquot of extract is diluted with 9.0 mL 15% methanol solution. This solution is subjected to sample atomization by a graphite furnace and arsenic detection by atomic absorption spectrophotometry (AAS). Roxarsone recovery from nonmedicated commercial feed fortified at 25 ppm was 103.6% with a relative standard deviation (RSD) of 4.0%. Recovery for 50 ppm fortification was 104.5% (RSD 4.3%). Roxarsone assay results by furnace AAS were compared with results by the current AOAC spectrophotometric method and the AOAC total arsenic method. Results by the 3 methods compare well. The procedure was also used to determine other organic arsenicals and inorganic arsenic in laboratory-fortified feed samples; these recoveries were essentially theoretical.
Liquid Chromatographic Identification of cis- and trans- Cinnamoylcocaine in Illicit Cocaine
Authors: Noggle F Taylor , Clark C Randall 
Published: February 2020

Abstract
A liquid chromatographic procedure is described for the analysis of illicit cocaine samples. The isomeric cis- and trans-cinnamoylcocaines are separated from cocaine, benzoylecgonine, and benzoic acid in a reverse phase isocratic system with dual wavelength detection at 254 and 280 nm. Specific identification of cocaine and the cinnamoylcocaines is accomplished by ultraviolet spectrophotometry and mass spectrometry of the chromatographic effluent.
Analytical Methods Used by Industry for Lead in Infant Formula
Authors: Miles J Preston 
Published: February 2020

Abstract
The lead content of liquid infant products has been a prime focus of regulatory, industrial, and private analysts for some time. The principal source of Pb in these products is the solder used in 3-piece can manufacture. Voluntary surveys by the Infant Formula Council member companies from 1978 to present show that even low 1978 levels have been significantly reduced. Two procedures, anodic stripping voltammetry and electrothermal atomization (graphite furnace and carbon rod) atomic absorption spectrophotometry, are currently used by industry analysts. The results of 2 comparison studies provide a means of estimating the reliability of the procedures. Results of thousands of trace Pb determinations have demonstrated that steps to ensure the validity of results must be integrated into the entire analytical scheme. Quality control practices are described. Control of the laboratory environment is essential for ultimate sensitivity, and the design and performance of a trace metals analysis facility are discussed.
Induction of Aryl Hydrocarbon Hydroxylase Activity in Cell Cultures by Aroclors, Residues from Yusho Oil Samples, and Polychlorinated Biphenyl Residues from Fish Samples
Authors: Trotter William J , Young Susan J V , Casterline James L , Bradlaw June A , Kamps Laverne R 
Published: February 2020

Abstract
Four Aroclor reference materials, cleaned-up extracts of 2 Yusho rice oil samples, and cleaned-up extracts of 3 fish samples containing polychlorinated biphenyl (PCB) residues were tested for their ability to induce aryl hydrocarbon hydroxylase (AHH) activity in a rat hepatoma cell line. Before the AHH bioassay, the samples were fractionated by a Florisil column chromatographic method. All samples contained about 1000 fig PCBs before Florisil column chromatography. The first Florisil eluate contains about 95% of the PCBs in a typical Aroclor, and the second contains the more polar or adsorbent PCB congeners. In this study, the first eluate for all samples produced no quantifiable AHH activity. The second Florisil eluates of both Aroclors 1242 and 1248 induced AHH activity, whereas these eluates of both Aroclors 1254 and 1260 did not. This difference may be due to the presence in Aroclors 1242 and 1248 of 3,3',4,4'-tetrachlorobiphenyl, which has not been detected in Aroclors 1254 and 1260. The second Florisil eluates of the fish samples induced somewhat less AHH activity than did Aroclor 1242 or 1248. The second Florisil eluates of the PCB residues from Yusho rice oil samples induced significantly greater AHH activity than these eluates of either Aroclor 1242 or 1248, perhaps because Yusho rice oil contains a greater amount of polychlorinated dibenzofurans than PCB commercial mixtures on a PCB equivalent basis.
Spectrophotometric Determination of Ephedrine Hydrochloride and Phenylephrine Hydrochloride
Authors: Amer Mohamed M , Taha Aly M , El-Shabouri Salwa R , Khashaba Pakinaz Y 
Published: February 2020

Abstract
A method is described for quantitative determination of the sympathomimetic amines ephedrine HCl and phenylephrine HCl. The method is based on the interaction of N-alkylvinylamine formed from the condensation of the free secondary amine group and acetaldehyde with chloranil to give a vinylaminosubstituted quinone. The colored product for ephedrine HCl and phenylephrine HCl exhibits 2 maximas at about 320 and 680 nm. All variables were studied to optimize reaction conditions. The relationship between absorbance and concentration was linear within 1-25 μg/mL under the conditions studied for both drugs at both wavelengths. The method has been applied to the analysis of some pharmaceutical formulations including tablets and eye drops with good recoveries (98.75-100.4%).
Stability of Individual Natural Pyrethrins in Solution after Separation by Preparative High Performance Liquid Chromatography
Authors: Dickinson Charlotte M 
Published: February 2020

Abstract
The 6 components of natural pyrethrum (jasmolins I and II, cinerins I and II, and pyrethrins I and II) were separated by preparative high performance liquid chromatography (HPLC) from a standard pyrethrum extract. Each component was then isolated and weighed, and its identity was established by mass spectrometry. Dilute solutions of each compound were prepared incorporating an internal standard and stored under the test conditions: Solutions were placed in clear-glass vials covered with aluminum foil to protect the contents from light, and one vial of each compound was stored at —18, —5,23, and 37°C. One set of vials not covered with foil was stored at room temperature under a fluorescent desk lamp burning continuously for the 2 month test. The solutions were analyzed periodically by gas chromatography, and all 6 compounds were stable during the test period if protected from light. Temperatures up to 37°C had no effect on stability. It was concluded that standard solutions of individual pyrethrum compounds could be prepared and stored for use in the quantitative analysis of pyrethrum formulations. During studies of the effect of light on the solutions, photoproducts of all 6 compounds were formed. The photoproducts of pyrethrins I and II were isolated and identified, in each case, as the (E)-isomer of the parent compound. Nuclear magnetic resonance spectra (300 MHz) of these new compounds are presented.
Determination of Lead and Cadmium in Foods by Anodic Stripping Voltammetry: II. Collaborative Study
Authors: Capar Stephen G , Gajan Raymond J , Madzsar Elizabeth , Albert Richard H , Sanders Marion , Zyren John ,   Collaborators:, Baetz R , Beavin P , Davis P H , Faul K , Gardner W T , Hansen C , Hopefl R , Hostetter J O , Klopp T , Loges M D , Moffitt R , Newton C B , Newton R T , Paillard G , Panaro K , Satzger R D , Schwartz D , Snider P , Suddendorf R F , Tepedino N , Williams J 
Published: February 2020

Abstract
A dry ash anodic stripping voltammetric method for determining lead and cadmium in foods was collaboratively studied by 20 laboratories. The food commodities studied were strained green beans, beef (baby food), fish (mackerel), infant formula (milk base), apple juice, and cereal (wheat farina). Each collaborator analyzed 3 commodities, each consisting of 2 duplicate lead and cadmium fortification levels, for a total of 4 samples for each commodity. The low fortification levels ranged from 0.03 to 0.08 ppm for cadmium and from 0.05 to 0.15 ppm for lead. The high fortification levels ranged from 0.12 to 0.28 ppm for cadmium and from 0.24 to 0.45 ppm for lead. Each commodity was analyzed by 10 collaborators. The average overall reproducibilities of the low level fortifications were 247c for lead and 21% for cadmium; for the high level fortifications, average overall reproducibilities were 18% for lead and 16% for cadmium. The average accuracies of the collaborative results as measured by comparison to reference values were 96 and 97% for cadmium and lead, respectively. This method has been adopted official first action.
Precautions in Ashing Techniques for Lead Determination in Food
Authors: Thornburg Wayne 
Published: February 2020

Abstract
In determining lead in food, the matrix must be destroyed before quantitation by atomic absorption spectrophotometry. Wet or dry ashing techniques are generally used. Dry ashing assisted by ultrapure H2SO4 or K2SO4 has the advantages of safety, low reagent blanks, rapidity, and good recoveries of added lead. These techniques are also less laborintensive than wet ashing.
High Performance Liquid Chromatographic Determination of Subsidiary Colors in FD&C Red No. 3
Authors: Calvey Robert J , Goldberg Allen L 
Published: February 2020

Abstract
Two rapid, sensitive, reproducible methods that use a Zorbax C-8 reverse phase column and high performance liquid chromatography are described for the determination of the subsidiary colors in FD&C Red No. 3. With the first method, 8 subsidiary colors (fluorescein, 2'-iodofluorescein, 4'-iodofluorescein, 2',5'-diiodofluorescein, 2',7'-diiodofluorescein, 4',- 5'-diiodofluorescein, 2',4',7'-triiodofluorescein, and 2',4',5'-triiodofluorescein) are eluted in a reproducible pattern by increasing the organic nature of a buffered mobile phase. Method 1 is capable of quantitating all the subsidiary colors except 4'-iodofluorescein and 4',5'-diiodofluorescein. If these 2 subsidiary colors are seen, the sample must be run again by method 2, which uses a different program and solvent system to quantitate them. The average recoveries for the 6 subsidiary colors quantitatively determined in FD&C Red No. 3 by method 1 ranged from 96 to 98%. The average recoveries for 4'-iodofluorescein and 4',5'-diiodofluorescein, quantitatively determined in FD&C Red No. 3 by method 2, were 101 and 103%, respectively. The amounts of the 6 subsidiary colors recovered by method 1 were 0.04-7.4% by weight of the total sample. The amounts of the 2 subsidiary colors recovered by method 2 were 0.13-2.6% by weight of the total sample.
Extraction of Light Filth from Rice Flours, Extruded Rice Products, and Rice Paper: Collaborative Study
Authors: Dent Russell G ,   Collaborators:, Bryce J R , Cox B C , Hughes D D , Karpus J T , Nagy J , Vail D J 
Published: February 2020

Abstract
Two new methods were developed for the extraction of rodent hairs and insect fragments from rice products: one for rice flour and one for extruded rice products and rice paper. A 100 g sample of rice flour was extracted with mineral oil-40% isopropanol, followed by a water phase as needed for additional cycles. For extruded rice products and rice paper, a 225 g sample of each was initially extracted as above, followed by a single extraction with mineral oil-20% isopropanol. Both methods used an acid hydrolysis pretreatment followed by wet sieving and a percolator extraction. Average rodent hair recoveries were 77.8% for rice flour and 82.2% for extruded rice products and rice paper. Average insect fragment recoveries were 89.6% for rice flour and 91.9% for extruded rice products and rice paper. Both methods were adopted official first action.
Howard Mold Count of Fruit Nectars, Purees, and Pastes: Collaborative Study
Authors: Cichowicz Stanley M , Bandler Ruth ,   Collaborators:, Bandler R , Dzidowski G , Floyd D , Galacci R , Kaminski J , McNerney F 
Published: February 2020

Abstract
The various mold count methods for nectars, purees, and pastes make no adjustment for concentration of the pulped liquid. Thus, mold counts of different forms of the same product (e.g., guava nectar, puree, or paste) or of the same product from different manufacturers cannot be compared. A method was developed in which the product is centrifuged under standardized conditions, then diluted to a standard pellet-to-final-volume ratio. Because variations in the concentration of fruit or vegetable tissue are corrected, comparisons of mold counts are possible. The method was adopted official first action.
Modified Gas-Liquid Chromatographic Method for Determination of Compound 1080 (Sodium Fluoroacetate)
Authors: Okuno Iwao , Meeker Dennis L , Felton Robert R 
Published: February 2020

Abstract
A method capable of determining 0.1 ppm 1080 (sodium fluoroacetate) in 1 g animal tissue was developed. It involves extraction of 1080 from the sample with acetone-water, and then evaporation of the acetone followed by extraction of 1080 as fluoroacetic acid from water with ethyl acetate. Ethyl acetate is removed by volatilization from fluoroacetic acid which is retained as the triethanolammonium fluoroacetate salt. Fluoroacetic acid is subsequently derivatized with α-bromo-2,3,4,5,6-pentafluorotoluene and quantitated by gas-liquid chromatography with an electron capture detector. The method is rapid and requires no special apparatus or equipment and no more than 12 ml of any one solvent. Recoveries of 1080 from tissue samples fortified with 0.1-100 ppm averaged about 85%.
Cylinder Plate Assay for Determining Bacitracin in Premix Feeds and Finished Feeds: Collaborative Study
Authors: Gallagher John B , Knotts Linda L ,   Collaborators:, Brennecke D , Bryant H H , Carter G G , Harpster C , Hasselberger M L , Jones K D , Knotts L L , Martin J , Olsen J I , Ragheb H S , Stouffer N , Winely C 
Published: February 2020

Abstract
A cylinder plate assay procedure was studied by 10 laboratories. For premix feeds, 3 samples of bacitracin methylene disalicylic acid and 3 samples of bacitracin zinc premixes covering the range of 10 to 50 g/lb were used. The repeatability standard deviation was 2.11, and the reproducibility standard deviation was 2.13. The average recovery of bacitracin was 101.5%. The method has been adopted official first action. For finished feeds, 6 samples of bacitracin methylene disalicylic acid and 6 samples of bacitracin zinc covering the range of 10 to 800 g/ton were used in the study. The procedure included a sample cleanup step using disposable reverse phase columns. This step appears to be the cause of the poor results reported by most collaborators. Continued study is needed to develop an acceptable method for finished feeds.
High Pressure Liquid Chromatographic Determination of Bacitracin in Premix Feeds and Finished Feeds: Collaborative Study
Authors: Gallagher John B , Love Paul W , Knotts Linda L ,   Collaborators:, Allred M , Hasselberger M L , Johnson A , Louie D , Love P W , Quick F , Sharley D , Smallidge R L , Thorpe V A , Williams W H 
Published: February 2020

Abstract
A liquid chromatographic technique for the determination of bacitracin in finished feeds and premix feeds consists of an isocratic reverse phase, ion-suppressed technique. The chromatography can be completed in less than 25 min. In a collaborative study involving 9 laboratories and 3 samples of bacitracin methylene disalicylic acid and 3 samples of bacitracin zinc premixes covering the range of 10-50 g/lb, the repeatability standard deviation was 0.55, and the reproducibility standard deviation was 1.35. The average recovery of the bacitracin was 102.0%. The method has been adopted official first action for bacitracin in premix feeds.
Rapid Screening Assay for Beta-Lactam Antibiotics in Milk: Collaborative Study
Authors: Charm Stanley E , Chi Ruey K ,   Collaborators:, Bryant H , Carson M , Chu W S , Fraser A , Gruetmacher C F , Hostetler O , Jones K , Kenell L , McQuattie R , O’Neill C , Richwine D , Salimbene J , Smith S , Wallace C , Yokote R 
Published: February 2020

Abstract
A 15 min assay for beta-lactam antibiotics has been used by dairies for several years as a screening procedure for testing milk tankers before they unload. The test is based on a competition between 14C-penicillin and beta-lactam antibiotics in the milk samples for sites on a microbial cell wall that specifically binds beta-lactam. In a collaborative study, 11 laboratories correctly distinguished 10 coded zero penicillin G samples and 10 coded 0.01 IU/mL samples. The proposed test is qualitative, positive or negative, and can detect the presence of beta-lactam antibiotics at the 0.01 IU/mL level. The control point for determining positive or negative samples is more than 3 standard deviations from the mean of 0.01 IU/mL. The method has been adopted official first action.
Qualitative Ampule and Multitest for Beta-Lactam Residues in Fluid Milk Products: Collaborative Study
Authors: Kelley Wesley N ,   Collaborators:, Andrews J , Appelt A W , Barber R , Barnett J , Barta L , Bass B , Bone E , Breske L , Bryant H H , Case R A , Coleman K , Cyr R , Dewald S K , Dombroski P , Dubs E L , Feldstein F F , Gay B E , Ginn R E , Gottomoller C , Grant H , Heady J , Hills D G , Jerrod L , Jones K , Kaus C , Lane A L , Leslie J E , Marchette D , Misup M , Morris L , Mullen R N , Payton C , Schmidt J , Schneider D , Share R , Sierck M , Wehr H M , Williams R 
Published: February 2020

Abstract
A collaborative study was performed on a rapid Bacillus stearothermophilus agar diffusion ampule method to detect low levels of penicillin G in 7 types of fluid milk products. A multitest technique for processing a large number of samples simultaneously was also studied. Slight modifications were made in the original method to establish more uniformity and to eliminate doubtful responses by specifying a confirmation procedure. Twenty samples spiked with penicillin G (0.000 to 0.008 IU/mL) and tetracycline hydrochloride were frozen and sent to 20 laboratories in the ampule test, and 16 laboratories in the multitest. Each analyst was asked to do a screening run and a confirmation run. Results were reported by color reaction and also as positive or negative for β-lactam inhibitors. The concentrations (penicillin G) where percent positive results equal 100 or not significantly less than 100 (α = 0.05) ranged from 0.005 to 0.007 IU/mi in the ampule test and from 0.004 to 0.007 IU/mL in the multitest. Both techniques have been adopted official first action.
Analysis of Fat-Soluble Vitamins. XXVII. High Performance Liquid Chromatographic arid Gas-Liquid Chromatographic Determination of Vitamin D in Fortified Milk and Milkpowder: Collaborative Study
Authors: De Vries Ellen J , Borsje Ben ,   Collaborators:, Ameika L , Baillies N T , Delano N , de Vries E J , Egtberts W , Fischer G A , George E , Gillingham P J , Hancock W , Knapstein H , Monard A , Muniz J F , Nedelkovitch G , Nicolaux G , Oelrich E , Phillips G F , Pollman R , Richter E F , Scholz H , Schwarze P , Steuerle H , Thiele U , Thorpe V A , Weaver C , Wehr H M 
Published: February 2020

Abstract
A collaborative study of the high performance liquid chromatographic (HPLC) method for vitamin D in fortified milkpowder (skimmed and whole milk) and a milkpowder preparation was carried out on 182 samples distributed to 26 laboratories. Thirteen laboratories submitted results. The level of vitamin D was 2-7IU vitamin D3/g milkpowder. All samples also contained vitamin A. Three laboratories were excluded from the statistical evaluation because of incomplete results or deviation from the analytical procedure. Other laboratories reported acceptable results. At the same time, 63 samples were distributed to 9 laboratories which used a gas-liquid chromatographic method for determining vitamin D in milkpowder. Only one laboratory reported results. The HPLC method has been adopted official first action.