bluuebunny/crossref_metadata_2025_split huggingface dataset:
Study of Doxofylline and its Degradation Products in Bulk Drug by a Newly Developed Stability-Indicating HPLC Method
Authors: Patil Priti S , Hamrapurkar Purnima D , Phale Mitesh D , Desai Masti I , Pawar Sandeep B 
Published: August 2013

Abstract
The purpose of this work was to study the stability behavior of doxofylline under different stress conditions and to develop a sensitive stability-indicating HPLC assay method. The stress conditions applied included heat, moisture, acid-base hydrolysis, oxidation, and UV light. The drug was particularly labile under oxidative and thermal stress conditions, with 58.40 and 53.90% degradation, respectively. Good resolution of drug from degradation products formed under stress conditions was achieved on a C18 column using 10 mM KH2PO4 buffer solution (pH 6) methanol (40 + 60, v/v) as the mobile phase (pH 7.2). The flow rate was 1 mL/min, and the detection wavelength was 273 nm. The method was validated for linearity, range, precision, accuracy, LOD, and LOQ. The RSD was found to be &lt;2%. Since the method effectively separates the drug from its degradation products, it can be used as a stability-indicating method.
Kinetics Investigation and Determination of Pipoxolan Hydrochloride and Its Degradant Using Liquid Chromatography
Authors: Hadad Ghada M , Abdel Salam Randa A , Abdel Hamfeed Eman A 
Published: August 2013

Abstract
An LC method was developed for the quantitative determination of pipoxolan hydrochloride (PPH) and its degradant. Forced degradation studies were performed on bulk sample using acid (1 M hydrochloric acid), alkaline (0.2 M sodium hydroxide), oxidation (0.33% hydrogen peroxide), heat (70°C), and photolytic degradation. The chromatographic method was fine-tuned using the samples generated from forced degradation studies. Good resolution between the peaks corresponding to the degradants and the analyte was achieved on a Discovery® C18 LC column (25 cm × 4.6 mm id, 5 μm particle size). The mobile phase was methanol–10 mM sodium dihydrogen phosphate (60 + 40, v/v); pH was adjusted to 6.5 using 0.2 M sodium hydroxide. Quantitation was achieved with UV detection at 214 nm based on peak area. The proposed LC method was used to investigate the kinetics of acidic and alkaline degradation processes of PPH at different temperatures, and the apparent pseudo-first-order rate constant, half-life, and activation energy were calculated. The pH-rate profiles of degradation of PPH in Britton-Robinson buffer solutions within the pH range 2–12 were studied. The developed method was validated with respect to linearity, accuracy, precision, and robustness. Forced degradation studies proved the stability-indicating power of the method.
A Validated Stability-Indicating RP-LC Method for the Simultaneous Determination of Amlodipine and Perindopril in Tablet Dosage Form and Their Stress Degradation Behavior Under ICH-Recommended Stress Conditions
Authors: Gumustas Mehmet , Ozkan Sibel A 
Published: August 2013

Abstract
A stability-indicating RP-LC assay method was developed for the simultaneous determination of the cardiovascular drugs amlodipine and perindopril in the presence of degradation products generated from forced decomposition studies. The developed method is applicable for the determination of related substances in bulk drugs and simultaneous assay in a tablet pharmaceutical dosage form. Separation of the drugs and their degradation products was obtained using an RP Waters Spherisorb ODS1 column (250 × 4.6 mm id, 5 μm particle size) with the mobile phase acetonitrile–water (30 + 70, v/v) containing 15 mM phosphoric acid. The pH of the mobile phase was adjusted to 5.0. A flow rate of 1.2 mL/min was used for the separations, with detection at 215 nm. The chromatographic separation was performed at a column temperature of 45°C. Atenolol was chosen as the internal standard. Amlodipine and perindopril were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation studies showed that both compounds were degraded under these stress conditions. The method was found to be stability-indicating and can be used for the routine analysis of amlodipine and perindopril in the studied combined tablet dosage form.
Development and Validation of an Ultra-Performance Liquid Chromatography/Electrospray Ionization-Tandem Mass Spectrometry Bioanalytical Method for Quantifying Clonazepam in Human Plasma
Authors: Favreto Wagner Alex Jann , Pinto Ana Maria Pugens , Manfio Josélia Larger , Hoss Ivonete , Pristch Mariely Camila , Bordignon Solange Fátima 
Published: August 2013

Abstract
A sensitive, selective, and rapid ultra-performance LC (UPLC)/MS/MS method was validated for the confirmation and quantification of clonazepam in human plasma. The analyte was extracted from human plasma with diethyl ether, reaching an average recovery of 64.02 and 66.48% for clonazepam and the internal standard, respectively. The separation was performed on a Waters ACQUITY UPLC™ BEH C18 column (50 × 2.1 mm id, 1.7 μm particle size) with gradient elution at a flow rate of 0.25 mL/min using a 0.5% formic acid solution (mobile phase A) and acetonitrile–methanol–formic acid (75 + 25 + 0.5, v/v/v; mobile phase B). Detection was performed on a triple-quadruple tandem mass spectrometer in the multiple reaction monitoring mode via electrospray ionization. Linear calibration curves were obtained in the concentration range of 0.3–50.0 ng/mL, with an LOQ of 0.3 ng/mL. The intraday and interday precision (CV) values were below 10%, and accuracy (relative error) ranged from −2.6 to 6.6% at all QC levels. The suggested method was successfully applied for the determination of clonazepam in human plasma in a bioequivalence study.
Determination of Heavy Metals and Their Speciation in Street Dusts by Inductively Coupled Plasma-Optical Emission Spectrometry after a Community Bureau of Reference Sequential Extraction Procedure
Authors: Altundag Huseyin , Imamoglu Mustafa , Doganci Secil , Baysal Erkan , Albayrak Sinem , Tuzen Mustafa 
Published: August 2013

Abstract
Sequential selective extraction techniques are commonly used to fractionate the solid-phase forms of metals in soils. This procedure provides measurements of extractable metals from media, such as acetic acid (0.11 M), hydroxyl ammonium chloride (0.1 M), hydrogen peroxide (8.8 M) plus ammonium acetate (1 M), and aqua regia stages of the sequential extraction procedure. In this work, the extractable Pb, Cu, Mn, Sr, Ni, V, Fe, Zn, and Cr were evaluated in street dust samples from Sakarya, Turkey, between May and October 2009 using the three-step sequential extraction procedure described by the Community Bureau of Reference (BCR, now the Standards, Measurements, and Testing Programme) of the European Union. The sampling sites were divided into 10 categories; a total of 50 street dusts were analyzed. The determination of multielements in the samples was performed by inductively coupled plasma-optical emission spectrometry. Validation of the proposed method was performed using BCR 701 certified reference material. The results showed good agreement between the obtained and the certified values for the metals analyzed.
Displacement-Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Drop of Trace Amounts of Palladium in Water and Road Dust Samples Prior to Graphite Furnace Atomic Absorption Spectrometry Determination
Authors: Ghanbarian Maryam , Afzali Daryoush , Mostafavi Ali , Fathirad Fariba 
Published: August 2013

Abstract
A new displacement-dispersive liquid–liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(II) in road dust and aqueous samples. This method involves two steps of dispersive liquid–liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid–liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid–liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(II) replaces Cu(II) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(II)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(II) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.
Quantification of Melamine in Drinking Water and Wastewater by Micellar Liquid Chromatography
Authors: Beltrán-Martinavarro Beatriz , Peris-Vicente Juan , Rambla-Alegre Maria , Marco-Peiró Sergio , Esteve-Romero Josep , Carda-Broch Samuel 
Published: August 2013

Abstract
Because of the large potential health impact caused by deliberate contamination with the synthetic chemical melamine of different products for human and animal consumption, the World Health Organization and the Food and Agriculture Organization of the United Nations provided a range of recommendations in order to facilitate obtaining needed data, among which was the determination of the background levels of melamine in drinking water and wastewater (December 4, 2008). A chromatographic procedure using a C18 column, a micellar mobile phase consisting of sodium dodecyl sulfate (0.1 M), and 1-propanol (7.5%) buffered at pH 3, and detection by absorbance at 210 nm is reported in this paper for the quantification of melamine in drinking water and wastewater. Samples were filtered and directly injected into the chromatographic system, thus avoiding an extraction procedure. The optimal mobile phase composition was obtained by a chemometrics approach that considered the retention factor, efficiency, and peak shape. Melamine was eluted in about 6.2 min without interferences. Validation was performed following U.S. Food and Drug Administration guidelines. The analytical parameters studied were linearity (0.03–5 μg/mL, R2 = 0.998), LOD (13 ng/mL), intraday and interday accuracy (between 4.1 and 12.2%), intraday and interday precision (less than 14.8%), and robustness (RSD &lt; 5.1% for retention time and &lt;9.0% for area). The proposed methodology was successfully applied for analysis of local wastewater and drinking water, in which no melamine was found.
Validation of the ANSR™ Salmonella Method for Detection of Salmonella spp. in Selected Foods and Environmental Samples
Authors: Mozola Mark , Norton Paul , Alles Susan , Gray R Lucas , Tolan Jerry , Caballero Oscar , Pinkava Lisa , Hosking Edan , Luplow Karen , Rice Jennifer 
Published: August 2013

Abstract
ANSR™ Salmonella is a new molecular diagnostic assay for detection of Salmonella spp. in foods and environmental samples. The test is based on the nicking enzyme amplification reaction (NEAR™) isothermal nucleic acid amplification technology. The assay platform features simple instrumentation, minimal labor, and, following a single-step 10–24 h enrichment (depending on sample type), an extremely short assay time of 30 min, including sample preparation. Detection is real-time using fluorescent molecular beacon probes. Inclusivity testing was performed using a panel of 113 strains of S. enterica and S. bongori, representing 109 serovars and all genetic subgroups. With the single exception of the rare serovar S. Weslaco, all serovars and genetic subgroups were detected. Exclusivity testing of 38 nonsalmonellae, mostly Enterobacteriaceae, yielded no evidence of cross-reactivity. In comparative testing of chicken carcass rinse, raw ground turkey, raw ground beef, hot dogs, and oat cereal, there were no statistically significant differences in the number of positive results obtained with the ANSR and the U.S. Department of Agriculture-Food Safety and Inspection Service or U.S. Food and Drug Administration/Bacteriological Analytical Manual reference culture methods. In testing of swab or sponge samples from five different environmental surfaces, four trials showed no statistically significant differences in the number of positive results by the ANSR and the U.S. Food and Drug Administration/Bacteriological Analytical Manual reference methods; in the trial with stainless steel surface, there were significantly more positive results by the ANSR method. Ruggedness experiments showed a high degree of assay robustness when deviations in reagent volumes and incubation times were introduced.
Determination of Whey Protein Content in Bovine Milk-Based Infant Formula Finished Products Using Amino Acids Calculation Method: AOAC First Action 2012.08
Authors: Feng Ping , Baugh Steve 
Published: August 2013

Abstract
A method for the calculation of the whey protein fraction was developed for milk-based infant formula products based upon amino acid ratio calculated from asparagine/aspartic acid, alanine, proline, and phenylalanine amino acid data. Historical and literature amino acid data were combined to establish the reference amino acid values used in the validation study. This method has been evaluated for accuracy versus label claim for 12 products, with results from 90 to 107.5% of label claim and an overall average of 98.7%. Repeatability and intermediate precision were determined over 4 different days. Repeatability results were 4.75, 2.06, 4.18, and 2.44% RSD, respectively, with an overall intermediate precision of 3.68% RSD. Since the amino acid profile of infant formula finished products depends on the amino acid profile of ingredients used, the applicability of the method needs to be confirmed for specific types of infant formula, for which data will be gathered. Additional reference material data are being gathered for better estimation of milk and whey reference values, which are based on being normalized to total amino acid content, during the two year AOAC INTERNATIONAL Official Methods of Analysis method approval process.
Total Iodine in Infant Formula and Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: First Action 2012.14
Authors: Pacquette Lawrence H , Levenson Alan M , Thompson Joseph J , Dowell Dawn 
Published: August 2013

Abstract
After an assessment of data generated from a single-laboratory validation study published in the Journal of AOAC INTERNATIONAL 95, 169–176 (2012), a method for determining the total level of iodine in infant formula and nutritional products was presented for consideration for adoption by AOAC during the AOAC Annual Meeting held September 30–October 3, 2012 in Las Vegas, NV. An Expert Review Panel on Infant Formula and Adult Nutritionals concluded that the method met the established standard method performance requirements, and approved the method as AOAC Official First Action. The method involves digestion of the sample with nitric acid in a closed vessel microwave oven, followed by determination by inductively coupled plasma/MS using tellurium as the internal standard. The method LOQ for total iodine was 1.5 μg/100 g, but a practical LOQ was used at 5 μg/100 g total iodine. The analytical range of the method was 5–100 μg/100 g total iodine. The recoveries from 15 spiked nutritional products ranged from 90 to 105%.
Vitamin C in Infant Formula and Adult/Pediatric Nutritional Formula by HPLC with UV Detection: First Action 2012.21
Authors: Schimpf Karen , Thompson Linda , Baugh Steve 
Published: August 2013

Abstract
This method for the determination of vitamin C by HPLC allows for the separation and quantitation of L-ascorbic acid in infant, pediatric, and adult nutritional products. Liquids, semisolids, and powders ranging from 2 to 1000 mg/kg in their consumable forms were analyzed during the method validation. The method met the standard method performance requirements and was approved by an AOAC Expert Review Panel on Infant Formula and Adult Nutritionals on October 2, 2012. During validation, the overall intermediate precision was 2.1% RSD (triplicate determinations on 7–10 days); the within-day precision, or repeatability, was 1.54% RSD (triplicate determinations). Accuracy, as spike recovery, ranged from 97.0 to 100.9%. The method detection and quantitation limits were determined experimentally to be 0.02 and 0.06 mg/L, respectively, in prepared samples.
Second family with the boston‐type craniosynostosis syndrome: Novel mutation and expansion of the clinical spectrum
Authors: Janssen Alexander , Hosen Mohammad J. , Jeannin Philippe , Coucke Paul J. , De Paepe Anne , Vanakker Olivier M. 
Published: August 2013

AbstractCraniosynostosis, caused by early fusion of one or more cranial sutures, can affect the coronal or lambdoid sutures, or include premature fusion of the sagittal (scaphocephaly) or metopic suture (trigonocephaly). Often occurring as isolated finding, their co‐existence in a craniosynostosis syndrome is infrequent. We describe a four‐generation family with variable expression of a craniosynostosis phenotype with scaphocephaly and a particularly severe trigonocephaly. Molecular analysis revealed a missense mutation in the MSX2—associated with the Boston‐type craniosynostosis syndrome—affecting the same amino‐acid residue as in the original Boston family. Besides unique features such as the cranial sutures involved, minor limb abnormalities and incomplete penetrance, our patients share with the original family autosomal dominant inheritance and the presence of multiple endocranial erosions on CT imaging. Though these findings appear to be important diagnostic clues for MSX2‐related craniosynostosis, it is noteworthy that the first affected generation in this family presented merely with isolated sagittal or unicoronal craniosynostosis and cutaneous syndactyly. Molecular analysis of MSX2 should therefore be considered in patients with isolated scaphocephaly/unicoronal synostosis, especially in the presence of a family history for craniosynostosis or syndactyly. © 2013 Wiley Periodicals, Inc.
De novo complex X chromosome rearrangement unmasking maternally inherited CSF2RA deletion in a girl with pulmonary alveolar proteinosis
Authors: Auger Julie , Bonnet Céline , Valduga Mylène , Philippe Christophe , Bertolo‐Houriez Emmanuelle , Beri‐Dexheimer Mylène , Schweitzer Cyril , Leheup Bruno , Jonveaux Philippe 
Published: August 2013

AbstractWe report on a 3‐year‐old girl with a de novo complex X chromosome rearrangement associated with congenital pulmonary alveolar proteinosis (PAP) and short stature. Array comparative genome hybridization and FISH analyses contributed to characterize the complex rearrangement consisting of a 7.37 Mb terminal deletion of Xp22.33p22.2, a 17.3 Mb interstitial inverted duplication of Xp22.2p21.3, and a 10.14 Mb duplication of Xq27.3q28. PCR analysis of microsatellite markers supported a paternal origin of the X chromosome rearrangement. A pre‐meiotic two‐step mechanism may explain the occurrence of this complex X rearrangement: an inverted duplication deletion event on Xp, and duplication of the Xq27.3qter region through a telomere capture event stabilizing the broken chromosome Xp end. The girl has also inherited from her healthy mother an X chromosome with a colony stimulating factor 2 receptor, alpha (CSF2RA) gene deletion. Consistent with the recessive mode of inheritance, the de novo paternal Xp22.33p22.2 deletion combined to the maternally inherited CSF2RA gene deletion led to homozygous deletion of CSF2RA and PAP diagnosis in the girl. The Xp deletion encompasses the pseudoautosomal region 1 (PAR1) which contains genes that escape X inactivation. Short stature homeobox (SHOX) haploinsufficiency explains growth retardation. Absence of other symptoms in relation to the X deletion/amplification is most probably due to skewed X inactivation. Finally, inherited deletions may unmask rare pathogenic genomic rearrangement and contribute to clinical phenotypes by a recessive mode of gene action. © 2013 Wiley Periodicals, Inc.
Multiple Lupus‐Associated ITGAM Variants Alter Mac‐1 Functions on Neutrophils
Authors: Zhou Yebin , Wu Jianming , Kucik Dennis F. , White Nathan B. , Redden David T. , Szalai Alexander J. , Bullard Daniel C. , Edberg Jeffrey C. 
Published: August 2013

ObjectiveMultiple studies have demonstrated that single‐nucleotide polymorphisms (SNPs) in the ITGAM locus (including the nonsynonymous SNPs rs1143679, rs1143678, and rs1143683) are associated with systemic lupus erythematosus (SLE). ITGAM encodes the protein CD11b, a subunit of the β2 integrin Mac‐1. The purpose of this study was to determine the effects of ITGAM genetic variation on the biologic functions of neutrophil Mac‐1.MethodsNeutrophils from ITGAM‐genotyped and ‐sequenced healthy donors were isolated for functional studies. The phagocytic capacity of neutrophil ITGAM variants was probed with complement‐coated erythrocytes, serum‐treated zymosan, heat‐treated zymosan, and IgG‐coated erythrocytes. The adhesion capacity of ITGAM variants, in adhering to either purified intercellular adhesion molecule 1 or tumor necrosis factor α–stimulated endothelial cells, was assessed in a flow chamber. Expression levels of total CD11b and activation of CD11b were assessed by flow cytometry.ResultsMac‐1–mediated neutrophil phagocytosis, determined in cultures with 2 different complement‐coated particles, was significantly reduced in individuals with nonsynonymous variant alleles of ITGAM. This reduction in phagocytosis was related to variation at either rs1143679 (in the β‐propeller region) or rs1143678/rs1143683 (highly linked SNPs in the cytoplasmic/calf‐1 regions). Phagocytosis mediated by Fcγ receptors was also significantly reduced in donors with variant ITGAM alleles. Similarly, firm adhesion of neutrophils was significantly reduced in individuals with variant ITGAM alleles. These functional alterations were not attributable to differences in total receptor expression or activation.ConclusionThe nonsynonymous ITGAM variants rs1143679 and rs1143678/rs113683 contribute to altered Mac‐1 function on neutrophils. These results underscore the need to consider multiple nonsynonymous SNPs when assessing the functional consequences of ITGAM variation on immune cell processes and the risk of SLE.