bluuebunny/crossref_metadata_2025_split huggingface dataset:
Single Laboratory Validation of a Method for Determination of Glucosamine in RawMaterials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization
Authors: Zhou Joseph ZiQi , Waszkuc Ted , Mohammed Felicia 
Published: February 2020

Abstract
Single laboratory validation of a method for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by with high-performance liquid chromatography FMOC-Su derivatization. Tests with 2 blank matrixes containing SAMe, vitamin C, citric acid, chondroitin sulfates, methylsulfonylmethane, lemon juice concentrate, and other potential interferents showed the method to be selective and specific. Eight calibration curves prepared over 7 working days indicated excellent reproducibility with the linear range at least over 2.0–150 μg/mL, and determination coefficients &gt;0.9999. Average spike recovery from the blank matrix (n = 8 over 2 days) was 93.5, 99.4, and 100.4% at respective spike levels of 15, 100, and 150%, and from the sample matrix containing glucosamine (n = 3) was 99.9 and 102.8% at respective levels of 10 and 40%, with relative standard deviations &lt;0.9%. The method was also applied to 12 various glucosamine finished products and raw materials. The stability tests confirmed that glucosamine–FMOC-Su derivative once formed is stable at room temperature for at least 5 days. Limit of quantitation was 1 μg/mL and limit of detection was 0.3 μg/mL. The method is ready to proceed for the collaborative study.
Evaluation of the Swab Test On Premises for Detection of Antimicrobial Residues in Bovine and Porcine Kidneys
Authors: Salisbury Craig D C 
Published: February 2020

Abstract
The effect of sample matrix on the sensitivity of the Swab Test On Premises (STOP) was evaluated for selected antimicrobials. Fluid was extracted from bovine and porcine kidneys, and fortified with known levels of drugs. Aqueous standards were also prepared at the same levels. An aliquot of the fortified fluid or water was pipeted onto a dry swab which was placed onto the surface of a STOP plate, and the plate was incubated as outlined in the test kit manual. Zones of bacterial growth inhibition were measured and recorded, and additional testing was performed with decreasing levels of drug until a minimum detectable level was determined. The effect of temperature on the sensitivity of the test was also evaluated by running samples in duplicate, one set at a nominal temperature of 28°C, and the second set at a nominal temperature of 32°C. Fortified bovine kidney fluid produced significantly larger zones than did porcine kidney fluid at both temperatures, but the mean zone sizes for fortified water were not significantly different from those of bovine or porcine kidney fluid at either temperature. For all 3 matrixes, than 32zones of inhibition were significantly larger at 28°C than 32°C.
A Multicommutated Flow System for Determination of Bismuth in Milk Shakes by Hydride Generation Atomic Fluorescence Spectrometry Incorporating On-Line Neutralization of Waste Effluent
Authors: Ventura-Gayete Josep F , Ródenas-Torralba Eva , Morales-Rubio Ángel , Garrigues Salvador , Guardia Miguel De La 
Published: February 2020

Abstract
A highly sensitive method was developed for determination of bismuth in milk shakes by multicommutation hydride generation atomic fluorescence spectrometry (HG-AFS) based on off-line sonication for 10 min with aqua regia 8% (v/v) and on-line waste treatment. The instrumentation and chemistry variables were studied in order to provide the best performance. The limit of detection in the original samples, established for a probability level of 99.6% (k = 3), was 1.67 ng/g Bi. The method provides a fast alternative in control analysis with a sampling throughput of 72 h as compared with 31 h obtained by the classical continuous measurement. Additionally, multicommutation reduces waste generation by a factor of 2.6. The consumption of sample, reductant, and blank, as compared with continuous mode HG-AFS, was reduced 9.6, 4.5, and 13.3 times, respectively. To confirm the accuracy of the method, recovery studies were performed, and excellent agreement between multicommutation and continuous measurement-based values was obtained. Application of the developed methodology for bismuth determination in milk shake samples from the Spanish market provided concentrations ranging from 4.2 to 15.0 ng/mL, and good comparability with data obtained by continuous measurements after microwave-assisted total digestion of samples for a 95% probability level and 12 degrees of freedom was found.
Determination of Attapulgite and Nifuroxazide in Pharmaceutical Formulations by Sequential Digital Derivative Spectrophotometry
Authors: Toral M Inés , Paine Maximiliano , Leyton Patricio , Richter Pablo 
Published: February 2020

Abstract
A new method for the sequential determination of attapulgite and nifuroxazide in pharmaceutical formulations by first-and second-derivative spectrophotometry, respectively, has been developed. In order to obtain the optimal conditions for nifuroxazide stability, studies of solvent, light, and temperature effects were performed. The results show that a previous hydrolysis of 2 h in 1.0 × 10–1M NaOH solution is necessary in order to obtain stable compounds for analytical purposes. Subsequently, the first-and second-derivative spectra were evaluated directly in the same samples. The sequential determination of the drugs can be performed using the zero-crossing method; the attapulgite determination was carried out using the first derivative at 278.0 nm and the nifuroxazide determination, using the second derivative at 282.0 nm. The determination ranges were 5.7 × 10–6–1.0 × 10–4 and 3.7 × 10–8 –1.2 × 10–4M for attapulgite and nifuroxazide, respectively. Repeatability (relative standard deviation) values of 1.2 and 3.0% were observed for attapulgite and nifuroxazide, respectively. The ingredients commonly found in commercial pharmaceutical formulations do not interfere. The proposed method was applied to the determination of these drugs in tablets. Further, infrared spectroscopy and cyclic voltammetry studies were carried out in order to obtain knowledge of the decomposition products of nifuroxazide.
Food Allergen Detection Methods: A Coordinated Approach
Authors: Goodwin Philip R 
Published: February 2020

Abstract
The levels (1–2%) and increasing severity of allergic responses to food in the adult population are well documented, as is the phenomenon of even higher (3–8%) and apparently increasing incidence in children, albeit that susceptibility decreases with age. Problematic foods include peanut, milk, eggs, tree nuts, and sesame, but the list is growing as awareness continues to rise. The amounts of such foods that can cause allergic reactions is difficult to gauge; however, the general consensus is that ingestion of low parts per million is sufficient to cause severe reactions in badly affected individuals. Symptoms can rapidly—within minutes—progress from minor discomfort to severe, even life-threatening anaphylactic shock in those worst affected. Given the combination of high incidence of atopy, potential severity of response, and apparently widespread instances of “hidden” allergens in the food supply, it is not surprising that this issue is increasingly subject to legislative and regulatory scrutiny. In order to assist in the control of allergen levels in foods to acceptable levels, analysts require a combination of test methods, each designed to produce accurate, timely, and cost-effective analytical information. Such information contributes significantly to Hazard Analysis Critical Control Point programs to determine food manufacturers’ risk and improves the accuracy of monitoring and surveillance by food industry, commercial, and enforcement laboratories. Analysis thereby facilitates improvements in compliance with labeling laws with concomitant reductions in risks to atopic consumers. This article describes a combination of analytical approaches to fulfill the various needs of these 3 analytical communities.
Bioinformatics and Food Allergens
Authors: Gendel Steven M 
Published: February 2020

Abstract
Bioinformatics can play an important role in developing improved technology for the detection and characterization of food allergens. However, the full realization of this potential will depend on the development of allergen-specific databases as well as improved methods for data mining within these databases. Examples of existing allergen databases and analysis tools are described, as are the most important issues that need to be addressed in the next stage of database development.
Analytical Methods Used in the United Kingdom Wildlife Incident Investigation Scheme for the Detection of Animal Poisoning by Pesticides
Authors: Brown Peter M , Turnbull Gordon , Charman Sheonaidh , Charlton Andrew J A , Jones Ainsley 
Published: February 2020

Abstract
The United Kingdom Wildlife Incident Investigation Scheme (WIIS) investigates cases of suspected poisoning of wildlife, honey bees, and companion animals by pesticides. Together with field inquiries and veterinary post-mortem examinations, the analytical procedures presented here provide a comprehensive approach to the investigation of these cases. The paper covers selection of animal tissues for analysis and methods suitable for the analysis of honey bees and for various types of bait. Seven multiresidue methods cover around 130 pesticides, and methods are also described for a further 8 compounds. These methods are currently used on samples submitted to the Scheme in England and Wales.
Densitometric High Performance Thin-Layer Chromatography Identification and Quantitative Analysis of Psychotropic Drugs
Authors: Maślanka Anna , Krzek Jan 
Published: February 2020

Abstract
A thin-layer chromatography (TLC)-densitometry method has been developed to identify and quantify haloperidol, amitriptyline, sulpiride, promazine, fluphenazine, doxepin, diazepam, trifluoperazine, clonazepam, and chlorpromazine in selected psychotropic drugs. Separation was performed on precoated silica gel 60 F254 TLC plates. Chromatograms were developed in various mobile phases, and 8 of 30 tested phases were selected based on spot location and developing time. The identification and quantification were carried out based on ultraviolet densitometric measurements at chosen wavelengths. In addition to retention coefficients, the absorption spectra recorded directly from chromatograms were also used in qualitative analysis. Under established experimental conditions, high sensitivity of the method was achieved. The limit of detection ranged from 0.009 to 0.260 μg, depending on the wavelength selected for measuring. A satisfactory recovery, ranging from 92.99 to 104.70%, was achieved for individual constituents.
Determination of Metal Concentration in Fat Supplements for Swine Nutrition by Atomic Absorption Spectroscopy
Authors: Cocchi Marina , Faeti Valerio , Manfredini Matteo , Manzini Daniela , Marchetti Andrea , Sighinolfi Simona 
Published: February 2020

Abstract
The presence of some essential and toxic metals in fat supplements for swine diet was investigated. Collected samples represented a relevant production of the Italian industry. In particular, some samples were enriched with antioxidants or waste cooking oils. The method for the determination of Ca, Cu, Cd, Fe, Mg, Mn, Ni, Pb, and Zn in fat samples was developed by means of a certified reference material (CRM 186) and a representative fatty sample (RFS). All samples were digested in closed vessels in a microwave oven and then analyzed by flame atomic absorption or graphite furnace atomic absorption spectrometry. The entire analytical method provided a satisfactory repeatability and reproducibility confirmed by agreement between the experimental recovery data obtained for the CRM 186 sample and, with the method of standard additions, for the RFS material. The samples generally showed a small amount of metals compared with the recommended daily intake for the essential elements. On the other hand, some samples contained a significant concentration, from an analytical point of view, of Cd, Ni, and Pb. Principal component analysis (PCA) was applied to inspect the experimental data obtained from samples analysis. Basically no differences were detected in terms of metal concentration among the fat supplements analyzed.
Simultaneous Determination of Three Opiates in Serum by Micellar Liquid Chromatography Using Direct Injection
Authors: Capella-Peiró Maria-Elisa , Bose Devasish , Durgbanshi Abhilasha , Martinavarro-Domínguez Adriá , Gil-Agustí Mayte , Esteve-Romero Josep , Carda-Broch Samuel 
Published: February 2020

Abstract
A simple and reliable micellar liquid chromatographic method was developed for the simultaneous determination of 3 opiates (codeine, morphine, and thebaine) in serum, using direct injection and ultraviolet detection. The separation of the drugs was optimized on a C18 column, thermostatically controlled at 25°C, by evaluating mobile phases containing sodium dodecyl sulfate (SDS) and various modifiers (propanol, butanol, or pentanol). Adequate resolution of the opiates was obtained with a chemometrics approach, in which retention was modeled as a first step by using the retention factors for several mobile phases. Next, an optimization criterion that takes into account the position and shape of the chromatographic peaks was applied. The 3 opiates were totally resolved and determined in 12 min with the mobile phase 0.15M SDS–7% (v/v) butanol buffered at pH 7. The limits of detection for codeine and morphine were greatly improved by using fluorimetric detection. Repeatability and intermediate precision were tested for 3 different concentrations of the drugs, and the relative standard deviations were &lt;0.8% for most of the assays. Finally, the method was successfully applied to the determination of morphine and codeine in serum samples.
Calf Antibiotic and Sulfonamide Test (CAST) for Screening Antibiotic and Sulfonamide Residues in Calf Carcasses
Authors: Dey Bhabani P , Reamer Richard P , Thaker Nitin H , Thaler Alice M 
Published: February 2020

Abstract
The Calf Antibiotic and Sulfonamide Test (CAST), a microbial inhibition screening test, was developed for detecting antibiotics and sulfonamides in bob veal calf carcasses. The test uses Bacillus megaterium ATCC 9885 as the indicator organism and Mueller Hinton agar as the growth medium. Compared to Swab Test on Premises (STOP), developed in 1970, this screening test has higher sensitivity and the ability to detect a wider range of veterinary antimicrobial residual drugs, particularly sulfonamides, at lower concentrations. Carcasses that are tested with CAST and suspected of containing chemical residue above tolerance level are retained for confirmation. Disposition of these carcasses are determined upon laboratory result. Routine testing of bob veal calves with CAST allowed the Food Safety and Inspection Service to release most calf carcasses within 24 h post-slaughter, thus conserving shipping and handling resources. However, changes in the regulation in 1990 dictate that disposition of carcasses found to contain violative levels of sulfonamide residues should be based on laboratory findings. The analysis of the data for the years 1990–1994 and 1998 indicate that the use of CAST over the years was significant, and had a direct impact on reduction of residue violations in veal carcasses. With the use of CAST, potentially harmful antimicrobial chemicals entering the human food chain through veal meat have been minimized.
Comparison Study of Two Procedures for the Determination of Emamectin Benzoate in Medicated Fish Feed
Authors: Farer Leslie J , Hayes John M 
Published: February 2020

Abstract
A new method has been developed for the determination of emamectin benzoate in fish feed. The method uses a wet extraction, cleanup by solid-phase extraction, and quantitation and separation by liquid chromatography (LC). In this paper, we compare the performance of this method with that of a previously reported LC assay for the determination of emamectin benzoate in fish feed. Although similar to the previous method, the new procedure uses a different sample pretreatment, wet extraction, and quantitation method. The performance of the new method was compared with that of the previously reported method by analyses of 22 medicated feed samples from various commercial sources. A comparison of the results presented here reveals slightly lower assay values obtained with the new method. Although a paired sample t-test indicates the difference in results is significant, this difference is within the method precision of either procedure.
Study of the Liquid Chromatography Retention of Some Fibrate-Type Antihyperlipidemic Drugs on C18 and CN Columns: Application for Quantitation in Pharmaceutical Formulations
Authors: Misztal Genowefa , Komsta Łukasz 
Published: February 2020

Abstract
The 6 antihyperlipidemic agents—bezafibrate, ciprofibrate, clofibrate, clofibric acid, fenofibrate, and gemfibrozil—were separated on octadecyl (C18) and cyano (CN) chemically bonded columns using mobile phases containing phosphate buffer and different amounts of acetonitrile, dioxane, propan-2-ol, methanol, and tetrahydrofuran. Relationships between log k values and mobile phase composition have been examined for these systems. Analysis was performed on a Waters LC system with Merck LichroCART C18 and CN 125 mm columns using a flow rate of 1 mL/min and 227 nm detection. More than one-half of the results fitted Snyder-Soczewinski equations with r &gt; 0.995. Separation of all drugs was achieved on the C18 column with a mobile phase containing 45% propan-2-ol in phosphate buffer (pH = 2.145) and on a CN column with 20% acetonitrile in the same buffer. The best mobile phase, containing 45% propan-2-ol, was used to quantitate bezafibrate, ciprofibrate, fenofibrate, and gemfibrozil in pharmaceutical formulations. The active substances were extracted with methanol. The calibration curve was constructed in the 0.1–0.8 mg/mL range for all drugs and provided satisfactory linearity (Lack-of-Fit test and Mandel's test). The recovery function was sufficiently linear in all cases, with an insignificant intercept and slope very close to 1. Accuracy was tested by quantitating 3 fortified samples (50, 100, and 150%), which gave results without significant differences. None of the excipients interfered in the analysis. The recovery was 99.85% for bezafibrate, 99.02% for ciprofibrate, 99.53% for fenofibrate, and 99.92% for gemfibrozil, with relative standard deviation values of 0.63, 1.61, 1.84, and 0.88%, respectively.
Comparison of Various Dilutions and Solid-Phase Extraction Cleanup on the Determination of Ephedrine-Type Alkaloids and Internal Standard Recovery in Ephedra Botanical Raw Material and Powdered Extract
Authors: Trujillo William A , Sorenson Wendy R , Laluzerne Paul S , Scheuerell Chad R 
Published: February 2020

Abstract
A study was conducted to determine the effect of 3 dilution levels on the precision of the ephedra alkaloid method when used in conjunction with a solid-phase extraction (SPE) column. For the dilutions studied, SPE column cleanup is necessary because it promotes a greater recovery of the internal standard. However, overall, target precision values were not obtained on the test materials. It was determined that the SPE column is not the cause of the lower recovery in the more concentrated solutions. Significant signal suppression of the internal standard occurs in more concentrated solutions within the mass spectrometer. It is hypothesized that this lack of performance on the part of the SPE column may be linked to its inability to fully clean contaminants from the higher concentration solutions and/or a mass spectrometer overload, which resulted in the internal standard not fully correcting for signal suppression in more concentrated solutions. An internal standard is necessary, especially for accuracy, for the determination of all alkaloids, and only dilute solutions can be accurately analyzed. Due to the sensitivity of the mass spectrometer, it is recommended that the determination of ephedrine alkaloids in dietary supplements and botanicals should be studied using a standard graph at a level 10× less than the current method. It is also recommended that the SPE column used should be evaluated on its need for the sample dilutions made to fit the newly recommended standard graph.
Simultaneous Determination of Some Active Ingredients in Cough and Cold Preparations by Gas Chromatography, and Method Validation
Authors: Harsono Thresiana , Yuwono Mochammad , Indrayanto Gunawan 
Published: February 2020

Abstract
A simple and rapid gas chromatographic (GC) method has been developed for the simultaneous determination of combinations of acetaminophen, phenylpropanolamine hydrochloride, guaifenesin, pseudoephedrine hydrochloride, caffeine, chlorpheniramine maleate, and dextromethorphan hydrobromide in cough and cold tablets and syrups. After extraction of the analyte with alkaline ethyl acetate, 2 μL extract was injected (splitting ratio of 50:1) into a gas chromatograph equipped with a CBP1-M25-025 fused silica capillary column (25 m × 0.22 mm; film thickness, 0.25 μm). The column temperature was held at 150°C for 5 min, increased to 175°C at 3°C/min, and increased to 270°C at 10°C/min. The temperatures of the flame ionization detector and injector were maintained at 300°C. The GC method is inexpensive, rapid, accurate, and precise, and thus it can be used for routine analysis of tablet and syrup preparations in quality control laboratories of pharmaceutical companies.
Determination of 11 Aminoglycosides in Meat and Liver by Liquid Chromatography with Tandem Mass Spectrometry
Authors: Kaufmann Anton , Maden Kathryn 
Published: February 2020

Abstract
A method using liquid chromatography with tandem mass spectrometry was developed for the determination of 11 commonly used aminoglycoside antibiotics in meat. The proposed method is sufficiently sensitive (detection limits of 15 to 40 ppb for the various antibiotics) and highly selective. It is suitable for the quantitation and confirmation of aminoglycosides in a variety of matrixes (pork muscle, fish, and veal liver). Any multiresidue method for aminoglycosides must take into account their high affinity toward sample proteins and the significantly different pK values of the various analytes. The developed method uses a low-pH extraction with trichloracetic acid to ensure complete extraction of the analytes from the matrix. An anion-exchange step is used to remove the acid from the centrifuged extract. Aminoglycosides in this solution of low ionic strength can be quantitatively retained and afterwards eluted from a weak cation-exchanger solid-phase extraction (SPE) cartridge. The highly selective SPE steps produce clean extracts, which minimize possible suppression of the mass spectrometer signal.