bluuebunny/crossref_metadata_2025_split huggingface dataset:
Validation of a Liquid Chromatographic/Tandem Mass Spectrometric Method for the Determination of Scopolamine Butylbromide in Human Plasma: Application of the Method to a Bioequivalence Study
Authors: Manfio Josélia Larger , dos Santos Mauricio Bedim , Favreto Wagner Alex Jann , Hoffmann Fabiane Ines , Mertin Adriana Cristina 
Published: February 2020

Abstract
A sensitive and specific LC/MS/MS method was developed and validated for the determination of scopolamine butylbromide in human plasma. Scopolamine butylbromide and propanolol (internal standard) were extracted from the plasma by liquidliquid extraction with dichloromethane as the extraction solvent and separated on a C18 analytical column (50 4.6 mm id) maintained at 40C. The analytes were eluted at a constant flow rate of 0.45 mL/min; the mobile phase consisted of acetonitrile and a buffer of 5 mM ammonium acetate and 0.1 formic acid (60 + 40, v/v). The mass spectrometer, equipped with an electrospray source in the positive ionization mode, was set up in the multiple-reaction monitoring mode to monitor the transitions m/z 360.6 &gt; 102.5 (scopolamine butylbromide) and m/z 259.7 &gt; 115.6 (propanolol). The chromatographic separation was obtained within 2.0 min, and the responses were linear over the concentration range of 0.1040.00 ng/mL. The mean extraction recoveries of scopolamine butylbromide and propanolol from plasma were 69.00 and 80.76, respectively. Method validation parameters, such as specificity, linearity, precision, accuracy, and stability, were within the acceptable range. Moreover, when the proposed method was successfully applied to a pharmacokinetic study of healthy human volunteers, the results showed that the two scopolamine butylbromide formulations tested are not bioequivalent in rate and extent of absorption.
Determination of Carmine Food Dye (E120) in Foodstuffs by Stripping Voltammetry
Authors: Alghamdi Ahmad H , Alshammery Hamed M , Abdalla Mohamed A , Alghamdi Ali F 
Published: February 2020

Abstract
The behavior of the food colorant agent carmine (E120) was studied by square-wave adsorptive stripping voltammetry (SW-AdSV) at the hanging mercury drop electrode. It was observed that carmine gave a sensitive stripping voltammetric peak at 350 mV in pH 3 acetate buffer. The cyclic voltammetric technique was also used to characterize the electrochemical reduction process of carmine. The adsorptive voltammetric signal was evaluated with respect to various experimental conditions, and the optimized values were supporting electrolyte, acetate buffer; buffer acidity, pH 3; dye concentration, 3 107 M; accumulation time, 150 s; accumulation potential, 0.2 V; scan rate, 300 mV/s; pulse amplitude, 185 mV; SW frequency, 20 Hz; working electrode area, 0.6 mm2; and convection rate, 2600 rpm. The SW-AdSV peak currents depended linearly on the concentration of carmine from 5 108 to 1.25 107 mol/L (r 0.99). A detection limit of 1.43 109 mol/L with an RSD of 2.2 and a mean recovery of 97.9 were obtained. Possible interferences by several substances usually present in food products such as food additive dyes (E102, E100, E123, E127, and E129), artificial sweeteners, preservatives, and antioxidants were also evaluated. The proposed electrochemical procedure was successfully applied to the determination of carmine food dye in spiked commercially available ice cream and soft drinks.
Improvement of AOAC Official Method 984.27 for the Determination of Nine Nutritional Elements in Food Products by Inductively Coupled Plasma-Atomic Emission Spectroscopy After Microwave Digestion: Single-Laboratory Validation and Ring Trial
Authors: Poitevin Eric , Nicolas Marine , Graveleau Laetitia , Richoz Janique , Andrey Daniel , Monard Florence ,   Collaborators:, Abrahamson A , Baillon A , Barrios J , Berger S , Berrocal R , Bos R , Brullebaut L , Caseiro C , Choo L F , Cole G , Daix G , Dekussche C , Dhillon G-S , Fortineau A , Gaudin C , Gonzales M J , Leal R , Mabiog R O , Noorlos T , Reba R , Senechal C 
Published: February 2020

Abstract
A single-laboratory validation (SLV) and a ring trial (RT) were undertaken to determine nine nutritional elements in food products by inductively coupled plasma-atomic emission spectroscopy in order to improve and update AOAC Official Method 984.27. The improvements involved optimized microwave digestion, selected analytical lines, internal standardization, and ion buffering. Simultaneous determination of nine elements (calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc) was made in food products. Sample digestion was performed through wet digestion of food samples by microwave technology with either closed or open vessel systems. Validation was performed to characterize the method for selectivity, sensitivity, linearity, accuracy, precision, recovery, ruggedness, and uncertainty. The robustness and efficiency of this method was proved through a successful internal RT using experienced food industry laboratories. Performance characteristics are reported for 13 certified and in-house reference materials, populating the AOAC triangle food sectors, which fulfilled AOAC criteria and recommendations for accuracy (trueness, recovery, and z-scores) and precision (repeatability and reproducibility RSD and HorRat values) regarding SLV and RT. This multielemental method is cost-efficient, time-saving, accurate, and fit-for-purpose according to ISO 17025 Norm and AOAC acceptability criteria, and is proposed as an improved version of AOAC Official Method 984.27 for fortified food products, including infant formula.
Multiresidue Analysis of Pesticides in Soil by High-Performance Liquid Chromatography with Tandem Mass Spectrometry
Authors: Fenoll José , Hellín Pilar , Martnez Carmen M , Flores Pilar 
Published: February 2020

Abstract
An analytical multiresidue method using HPLC/MS/MS with a triple-quadrupole mass spectrometer in the multiple reaction monitoring mode for the simultaneous determination of 54 pesticides in soil has been developed. The procedure involved initial single-phase extraction of soil sample with acetonitrile by sonication, followed by liquidliquid partitioning after addition of NaCl. The average recovery by the HPLC/MS/MS method obtained for these compounds varied from 63.2 to 113.8, with an RSD between 1.9 and 7.1. The method gave good linearity over the assay range of 10500 g/L (except famoxadone, 501000 g/L); the LOD and LOQ for the pesticides varied from 0.02 to 13.2 and from 0.1 to 43.9 g/kg, respectively. The proposed method was used to determine pesticide levels in soil samples from two experimental vineyards and two tomato greenhouses.
Measurement of Water-Soluble B Vitamins in Infant Formula by Liquid Chromatography/Tandem Mass Spectrometry
Authors: Huang Min , Winters Doug , Crowley Richard , Sullivan Darryl 
Published: February 2020

Abstract
A method has been developed for the simultaneous measurement of multiple B vitamins (i.e., B1, B2, B3, B5, and B6) in infant formulas by LC-MS/MS. The vitamins were extracted with acidic solvent, followed by protein precipitation at a pH range of 4.5 to 5.5, and filtered. This simplified procedure eliminates many of the potential sources of laboratory error and facilitates rapid and efficient analysis. As is common in most cases, isotope internal standards were added to account for variations in sample preparation, as well as changes in MS measurement. In this method, isotope-labeled internal standards of B1, B3, B5, and B6 were used. The factors affecting analytical performance were investigated and optimized. In addition, the stability of these vitamins in the extraction solution was investigated. An acidic condition (5 mM HCl) was applied to successfully stabilize B1, which had shown a decrease in signal when other solvents were used. The quantitative extraction and good stability allowed isotope standards to be added to the filtered sample solution, instead of to the extraction solvent. The addition of the isotope to the small portion of the filtered sample solution significantly reduces cost. A comprehensive evaluation of the analysis of the standard reference material and good spike recovery of the vitamins (100 6) demonstrates the accuracy of the method. The results for commercially available infant formula samples were also compared with those obtained using the current microbiological method.
GMOtrack: Generator of Cost-Effective GMO Testing Strategies
Authors: Novak Petra Kralj , Gruden Kristina , Morisset Dany , Lavrač Nada , Štebih Dejan , Rotter Ana , Žel Jana 
Published: February 2020

Abstract
Commercialization of numerous genetically modified organisms (GMOs) has already been approved worldwide, and several additional GMOs are in the approval process. Many countries have adopted legislation to deal with GMO-related issues such as food safety, environmental concerns, and consumers' right of choice, making GMO traceability a necessity. The growing extent of GMO testing makes it important to study optimal GMO detection and identification strategies. This paper formally defines the problem of routine laboratory-level GMO tracking as a cost optimization problem, thus proposing a shift from the same strategy for all samples to sample-centered GMO testing strategies. An algorithm (GMOtrack) for finding optimal two-phase (screeningidentification) testing strategies is proposed. The advantages of cost optimization with increasing GMO presence on the market are demonstrated, showing that optimization approaches to analytic GMO traceability can result in major cost reductions. The optimal testing strategies are laboratory-dependent, as the costs depend on prior probabilities of local GMO presence, which are exemplified on food and feed samples. The proposed GMOtrack approach, publicly available under the terms of the General Public License, can be extended to other domains where complex testing is involved, such as safety and quality assurance in the food supply chain.
Assurance GDS for Salmonella
Authors: Feldsine Phil , Hammack Thomas 
Published: February 2020

Abstract
A study was conducted to determine the efficacy of detecting low contamination levels of Salmonella in peanut butter using Assurance GDS for Salmonella (GDS). This study was conducted under the AOAC Research Institute Emergency Response Validation program. A set of samples was each analyzed by the GDS and the U.S. Food and Drug Administration's Bacteriological Analytical Manual reference method. Among the 45 total samples and controls, 26 samples were positive by the GDS and 24 were positive by the reference method. Statistical analyses of these unpaired samples indicated that, for all levels analyzed, the differences between the GDS and reference method results were not statistically different at the 5 level.
RapidChek SELECT Salmonella
Authors: Muldoon Mark T , Li Jingkun , Sutzko Meredith , Olsson-Allen Ann Christine , Teaney George , Gonzalez Verapaz , Hammack Thomas 
Published: February 2020

Abstract
RapidChek SELECT Salmonella was previously validated in the Performance Tested MethodsSM program for the detection of Salmonella spp. in raw ground chicken, chicken carcass rinse, sliced cooked turkey, and liquid eggs. The present matrix extension study conducted under the AOAC Research Institute Emergency Response Validation program compared the RapidChek SELECT Salmonella method to the U.S. Food and Drug Administration's Bacteriological Analytical Manual (FDA-BAM) method for the detection of Salmonella Typhimurium in peanut butter. Overall, 27 samples were found positive by the RapidChek SELECT Salmonella method and 27 were found to be positive by the reference method. All RapidChek SELECT Salmonella presumptive positives were confirmed positive by the cultural reference method; additionally, all presumptive negative results were confirmed negative by the cultural reference method. Accordingly 0 false-negative rate and 0 false-positive rate were found. No significant difference between the RapidCheck SELECT Salmonella and FDA-BAM reference method was found; calculated Chi-square was 0. Results indicate that a low level of Salmonella in peanut butter can be successfully recovered and detected in the minimum 24 h enrichment protocol.
Simultaneous Determination of Eight Sympathomimetic Amines in Urine by Gas Chromatography/Mass Spectrometry
Authors: Moawad Michael , Khoo Cheang S , Lee Samiuela , Hennell James R 
Published: February 2020

Abstract
A GC method was developed for the identification and quantitation of eight sympathomimetic amines in urine, i.e., amphetamine, methamphetamine, mephentermine, ephedrine, pseudoephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, and methylenedioxyethylamphetamine. Methoxyphenamine was used as the internal standard (IS). The assay is rapid, sensitive, and simple to perform. It involves a liquidliquid extraction procedure with simultaneous in-solution derivatization of the organic layer with pentafluorobenzoyl chloride (PFB-Cl), followed by GC/MS analysis. These derivatives and the IS were extracted from 1 mL alkaline urine into hexane before derivatization with PFB-Cl. The organic layer was then removed and evaporated to dryness before dissolution with hexane for GC/MS analysis. Calibration curves for each analyte showed linearity in the range of 255000 ng/mL (r2 ≥ 0.997). Recoveries ranged from 88 to 99, with the precision of recoveries typically ≤5%. The LOD values ranged from 7 to 28 ng/mL, and the LOQ values ranged from 23 to 94 ng/mL. At least four ions were available for each analyte for confirmation of identity by MS.
Determination of Metformin Hydrochloride and Glyburide in an Antihyperglycemic Binary Mixture Using High-Performance Liquid Chromatographic-UV and Spectrometric Methods
Authors: Salem Hesham 
Published: February 2020

Abstract
Three methods were developed for simultaneous determination of metformin hydrochloride and glyburide in an antihyperglycemic binary mixture without previous separation. In the first method, a reversed-phase HPLC column with acetonitrilewater (60 + 40, v/v) mobile phase at 0.9 mL/min flow rate was used to separate both compounds, with UV detection at 254 nm. Linearity was obtained in the concentration range of 0.060.24 µg/mL for glyburide and 1.56.0 µg/mL for metformin hydrochloride. The second method depended on first- and second-derivative UV spectrometry with zero-crossing measurements. The first-derivative amplitude at 261 nm was selected for the assay of glyburide, and the second-derivative amplitude at 235 nm was selected for the assay of metformin hydrochloride. The third method depended on measuring the first derivative of the ratio-spectra at 241 nm for glyburide and 227 nm for metformin hydrochloride. For the second and third methods, Beer's law was obeyed in the range of 1055 µg/mL for glyburide and 20200 µg/mL for metformin. The proposed methods were extensively validated and applied for the analysis of some pharmaceutical formulations containing binary mixtures of the mentioned drugs.
Determination of Polycyclic Aromatic Hydrocarbons in Airborne Particulate Matter by Gas ChromatographyTriple Quadrupole Tandem Mass Spectrometry
Authors: Frenich Antonia Garrido , Ocaña Rosa Martínez , Vidal José L Martínez 
Published: February 2020

Abstract
An accurate and sensitive method for the identification and the quantification of 24 polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter has been developed and validated using GC/MS/MS with a triple quadrupole analyzer. Ultrasonic extraction (USE) and pressurized liquid extraction (PLE) were evaluated. PLE was selected because it provided better recoveries and reduced treatment time and use of solvents compared to USE. Cleanup of PLE extracts was not necessary. The accuracy of the optimized method was tested using a standard reference material of urban dust (SRM 1649a). PAH recoveries were between 70 and 99 (except for naphthalene, which was lower than 20) with RSDs ranging from 2.6 to 15.3. Linearity in the range 5500 ng/mL provided R2 values higher than 0.99 for all compounds. LODs for PAHs ranged from 0.001 to 0.435 ng/mL and LOQs ranged from 0.003 to 0.757 ng/mL. The proposed method was applied to the analysis of real samples collected in the city of Almera, Spain, where some PAHs were found at levels lower than the legislated limit.
Immunochromatographic Assay with Photometric Detection for Rapid Determination of the Herbicide Atrazine and Other Triazines in Foodstuffs
Authors: Byzova Nadezhda A , Zherdev Anatoly V , Zvereva Elena A , Dzantiev Boris B 
Published: February 2020

Abstract
An immunochromatographic system for detection of the herbicide atrazine and its structural analogues has been developed. The assay is based on the competition of atrazine and immobilized atrazine-protein conjugate for binding with anti-atrazine monoclonal antibodies. The antibodies are immobilized on colloidal gold particles with an average diameter of 30 nm under conditions providing stability of these complexes. Concentrations of reagents and regimens of their immobilization have been optimized in order to reach the minimal limit of atrazine detection. The assay is initiated by contact of the test strip with a liquid sample and does not need any additional reactants or treatment. Duration of the assay was 10 min. The colored line formed on the test strip was assessed quantitatively with a portable photometric device; the RSD in a series was 4.8-13.0%. The range of photometrically determined concentrations of atrazine was 130 ng/mL. Visual qualitative assay permitted detection of the disappearance of the colored line for atrazine concentrations starting at 100 ng/mL. Cross-reactivities of structurally similar herbicides correlated well for the proposed assay and traditional microplate ELISA. The applicability of the developed system for atrazine detection in milk and juices was confirmed.
Analysis of DDT Isomers with Enzyme-Linked Immunosorbent Assay and Optical Immunosensor Based on Rat Monoclonal Antibodies as Biological Recognition Elements
Authors: Krämer Petra M , Weber Cristina M , Forster Stephan , Rauch Peter , Kremmer Elisabeth 
Published: February 2020

Abstract
New rat monoclonal antibodies (mAbs) for DDT [1,1,1-trichloro-2,2-bis (4-chlorophenyl) ethane], namely DDT 7C12, DDT 1C1, and DDT 1B2, were developed, characterized, and applied in ELISA both in coating antigen and in enzyme-tracer format. The latter used horseradish peroxidase (HRP) or glucose oxidase as enzymes. The lowest concentration of p,p-DDT was determined with mAb DDT 7C12 and DDT-hapten HRP, with a test midpoint (IC50) of 0.5 ± 0.2 µg/L (n = 10) in 40 mM PBS (phosphate-buffered saline). The mouse anti-rat immunoglobulin lambda-light chain mAb LA1B12 was used as capture mAb. The best IC50 for o,p´-DDT in 40 mM PBS was 1.0 ± 0.3 µg/L (n = 12) and was obtained with mAb DDT 1C1 and DDT-hapten HRP, whereas mAb DDT 1B2 was very selective for p,p-DDT with an IC50 of 4.2 ± 1.6 µg/L (in 40 mM PBS, n = 9). An optical immunosensor was optimized and applied for the analysis of DDT (or DDT equivalents). This immunosensor consists of a bench-top optical readout device and disposable sensor chips, which include the fluidic system. Evanescent field excitation and emission of the fluorophore Oyster&lt;sup/&gt;-645 was used. An IC50 for p,p´-DDT [in 5 (v/v) isopropanol in 40 mM PBS] of 4 µg/L was obtained using DDT 7C12-Oyster-645. ELISA and immunosensor were used for the analysis of p,p-DDT in unspiked and spiked surface water samples. Within the working ranges of these immunotechniques, recoveries ranged from 80 to 120.
Validation and Uncertainty Analysis of a Multiresidue Method for 67 Pesticides in Made Tea, Tea Infusion, and Spent Leaves Using Ethyl Acetate Extraction and Gas Chromatography/Mass Spectrometry
Authors: Kanrar Bappaditya , Mandal Sudeb , Bhattacharyya Anjan 
Published: February 2020

Abstract
A rapid, specific, and sensitive multiresidue method to determine 67 pesticides in made tea, tea infusion, and spent leaves was developed and validated for routine analysis by GC/MS with an approximately 29 min GC run time. The method was reproducible (HorRat &lt;0.5 at 50 ng/g) when validated at 50 and 100 ng/g. The samples were extracted with ethyl acetatecyclohexane (9 + 1, v/v), and the extracts were cleaned up by dispersive SPE with primary-secondary amine sorbent + graphitized carbon black + Florisil. The recoveries of all the pesticides were within 70120 with an RSD of &lt;20 at 50 ng/g and R2 &gt; 0.99. The matrix effect on the signals of the compounds was corrected by using matrix-matched calibration standards. The LOQ met the requirements of the maximum residue limits for pesticides in tea as recommended by the European Union.
Differentiating Cross-Reacting Allergens in the Immunological Analysis of Celery (Apium graveolens) by Mass Spectrometry
Authors: Fæste Christiane K , Jonscher Karen R , Sit Louis , Klawitter Jelena , Løvberg Kjersti E , Moen Lena H 
Published: February 2020

Abstract
Celery is acknowledged as a major food allergen in Europe, and mandatory labeling for preprocessed foods has been implemented. However, no methods for the specific detection of celery protein in foods have been published. In the present study, a sandwich celery ELISA using polyclonal anticelery antibodies for capture and detection was developed and validated. The method has an LOD of 0.5 mg/kg in buffer; however, it is applicable only for the screening of food products because of extensive cross-reactivity with potato and carrot proteins. Using nanoLCion-trap MS/MS, a number of proteins in the three vegetable species were identified as candidates for causing cross-reactions due to amino acid sequence homologies. Among others, a novel patatin (Sola t 1)-like protein was detected in celery and a flavin adenine dinucleotide binding domain-containing protein (Api g 5)-like protein was identified in carrot. The utility of triple-quadrupole MS/MS for specific and quantitative analysis of celery, potato, and carrot allergens was evaluated using whole protein extracts. Several unique precursor ion-to-product ion transitions were determined for each species, suggesting the feasibility of developing an MS-based screening method to specifically detect celery allergens in foods.
Determination of Indoxacarb Enantiomer Residues in Vegetables, Fruits, and Soil by High-Performance Liquid Chromatography
Authors: Cheng Li , Dong Feng-Shou , Liu Xingang , Chen Wuying , Li Yuanbo , Zheng Yongquan , Qin Dongmei , Gong Yong 
Published: February 2020

Abstract
An effective chiral analytical method was developed for the resolution and determination of indoxacarb enantiomers in cucumber, tomato, apple, pear, and soil samples. Indoxacarb enantiomers were separated on a Chiralpak AS-H column with n-hexaneethanol (95 + 5, v/v) as the mobile phase. Validation involved complete resolution of each enantiomer, plus determination of linearity, precision, LOD, and LOQ. The estimated LOD was 0.0250.035 mg/kg, and the LOQ was 0.05 mg/kg for each indoxacarb enantiomer in different matrixes. The average recoveries of the pesticide from all matrixes ranged from 87.0 to 116.9 for fortification levels of 0.05, 0.1, and 5 mg/kg. The precision values associated with the analytical method, expressed as RSDr values, were &lt;10.1 for the pesticide in all matrixes. This method can be used to evaluate environmental residues and the safety of agricultural products.
Review of HPTLC in Drug Analysis: 1996-2009
Authors: Sherma Joseph 
Published: February 2020

Abstract
Analytical methods for drug substances, formulations, and clinical samples developed and validated on HPTLC plates during the period 19962009 are reviewed. Procedures, materials, and instrumentation for the different steps in the HPTLC procedure and validation of results; applications to bulk drugs, formulations, stability studies, biological samples (e.g., urine and plasma), and hydrophobicity studies; and prospects for the use of HPTLC for drug analysis in the future are described.