bluuebunny/crossref_metadata_2025_split huggingface dataset:
An Interlaboratory Investigation on the Use of High-Performance Thin Layer Chromatography to Perform Assays of LamivudineZidovudine, Metronidazole, Nevirapine, and Quinine Composite Samples
Authors: Kaale Eliangiringa , Risha Peter , Reich Eike , Layloff Thomas P 
Published: February 2020

Abstract
Two laboratories extensively investigated the use of HPTLC to perform assays on lamivudinezidovudine, metronidazole, nevirapine, and quinine composite samples. To minimize the effects of differences in analysts' technique, the laboratories conducted the study with automatic sample application devices in conjunction with variable-wavelength scanning densitometers to evaluate the plates. The HPTLC procedures used relatively innocuous, inexpensive, and readily available chromatography solvents used in the Kenyon or the Global Pharma Health Fund Minilabs&lt;sup/&gt; TLC methods. The use of automatic sample applications in conjunction with variable- wavelength scanning densitometry demonstrated an average repeatability or within-laboratory RSD of 1.90, with 73 less than 2 and 97 at 2.60 or less, and an average reproducibility or among-laboratory RSD of 2.74.
Method for the Direct Determination of Available Carbohydrates in Low-Carbohydrate Products Using High-Performance Anion Exchange Chromatography
Authors: Ellingson David , Potts Brian , Anderson Phillip , Burkhardt Greg , Ellefson Wayne , Sullivan Darryl , Jacobs Wesley , Ragan Robert 
Published: February 2020

Abstract
An improved method for direct determination of available carbohydrates in low-level products has been developed and validated for a low-carbohydrate soy infant formula. The method involves modification of an existing direct determination method to improve specificity, accuracy, detection levels, and run times through a more extensive enzymatic digestion to capture all available (or potentially available) carbohydrates. The digestion hydrolyzes all common sugars, starch, and starch derivatives down to their monosaccharide components, glucose, fructose, and galactose, which are then quantitated by high-performance anion-exchange chromatography with photodiode array detection. Method validation consisted of specificity testing and 10 days of analyzing various spike levels of mixed sugars, maltodextrin, and corn starch. The overall RSD was 4.0 across all sample types, which contained within-day and day-to-day components of 3.6 and 3.4, respectively. Overall average recovery was 99.4 (n = 10). Average recovery for individual spiked samples ranged from 94.1 to 106 (n = 10). It is expected that the method could be applied to a variety of low-carbohydrate foods and beverages.
Rapid Method for the Determination of Capsaicin and Dihydrocapsaicin in Gochujang Using Ultra-High-Performance Liquid Chromatography
Authors: Ha Jaeho , Seo Hye-Young , Shim You-Shin , Nam Hyun-Jin , Seog Homoon , Ito Masahito , Nakagawa Hiroaki 
Published: February 2020

Abstract
A sensitive and specific heating block method coupled with ultra-HPLC (u-HPLC) was developed for the analysis of capsaicin in Gochujang and validated by comparing with a conventional HPLC (AOAC Method 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The u-HPLC separation was performed on a reversed C18 column (50 2 mm id, particle size 2 m), followed by fluorescence detection (excitation 280 nm, emission 325 nm). Methanol was used as the extracting solvent, and the amount of sample taken was approximately 0.2 g; the optimum amount of extraction solvent and extraction time were 15 mL and 1 h, respectively. The recovery of capsaicin in Gochujang was more than 93, and the LOD and LOQ of the u-HPLC analysis were 0.05 and 0.16 g/g for capsaicin and 0.05 and 0.16 g/g for dihydrocapsaicin. The calibration graphs for capsaicin and dihydrocapsaicin were linear from 0.2 to 10.0 g/mL for u-HPLC. The interday and intraday precisions (RSD values) were &lt;6.27.
ELISA Kit for Determination of Egg White Proteins: Interlaboratory Study
Authors: Tomková Kvìta , Cuhra Petr , Rysová Jana , Hanák Petr , Gabrovská Dana ,   Collaborators:, Baranda A , Baršová S , Brychta J , Bulawová H , &#x84;en&#x85;i&#x85; A , Del Barco J A G , Dvorská P , Iametti S , Jimenez E , Karšulínová L , Kubík M , Langerholc T , Laukkanen M-L , Martínez de Marañon I , Suñen Pardo E , Angel Pardo M , Piknová L , Plicka J , Martínez Quesada J , Postigo Resa I , Štumr F , Takkinen K 
Published: February 2020

Abstract
An interlaboratory study was conducted in 11 laboratories to validate an ELISA method developed for the quantitative determination of egg white proteins (EWPs) in foods. The ELISA kit used for this study is based on sheep polyclonal antibody. It does not produce any false-positive results or cross-reactivity in a broad food matrix range with zero EWP content. All participants obtained the Egg ELISA Kit-native with standard operational procedure and the list of samples, as well as the samples and a protocol for recording test results. The study included 10 food samples. Four samples of food matrix with zero EWP content showed EWP content lower than the first standard (EWP content 0.5 mg/kg). One sample of food matrix with zero EWP content revealed EWP content higher than standard 3 (1.5 mg EWP/kg). Five food samples containing EWP as an ingredient tested positive and one negative. The statistical tests (Cochran, Dixon, and Mandel) and analysis of variance were used to evaluate the interlaboratory study results. Repeatability and reproducibility limits, as well as LOQ (1.4 mg EWP/kg) and LOD (0.43 mg EWP/kg), were calculated for the kit.
A Simple HPLC Method for Quantitation of Quercetin in Herbal Extracts
Authors: D’Mello Priscilla M , Joshi Urmila J , Shetgiri Preetam P , Dasgupta Tarun K , Darji Kamil K 
Published: February 2020

Abstract
A reversed-phase HPLC method with UV detection was developed for the determination of quercetin. The method produced linear response over a wide concentration range, with an average accuracy of 95% and average intra- and interday variation of 0.75 and 0.3, respectively. The exactness of the method was proven by determining the recovery rates from 50 to 150% of standard concentration, which were found within the acceptable range of 95 to 105%. The method was used for quantitation of quercetin in the extracts of Psidium guajava, Vitis vinifera, and extracts rich in quercetin and other flavonols in the flavonoid family.
Reversed-Phase Ultra-Performance Liquid Chromatographic Method Development and Validation for Determination of Impurities Related to Torsemide Tablets
Authors: Patel Hitesh B , Mohan Arivozhi , Joshi Hitendra S 
Published: February 2020

Abstract
A simple RP-ultra-performance LC method was developed and validated for determination of impurities related to torsemide tablets. The rapid method provided adequate separation of all known related impurities and degradation products. Separation was achieved on a Zorbax SB-C18 column (50 × 4.6 mm id, 1.8 μm particle size) with binary gradient elution, and detection was performed at 288 nm. The drug product was subjected to oxidative, hydrolytic, photolytic, and thermal stress conditions to prove the specificity of the proposed method. The linearity and recovery were investigated for known impurities in the range of 0.025 to 1.0%, with respect to the drug concentration in the prepared sample. The linearity of the calibration curve for each of the impurities and torsemide was found to be very good (r2 &gt; 0.999). Relative response factors for each of the known impurities were established by the slope ratio method from the linearity study.
Single Laboratory Validation of a Microsatellite Marker-Based Method in Tomato Variety Identification
Authors: Srivastava Deepak K , Shoemaker Lauren S , Franks Craig E , Sussman Michael D 
Published: February 2020

Abstract
The objective of this study was to develop a systematic and flexible method for assembling multiplex simple sequence repeat marker panels for high-throughput genome analysis in the tomato, Solanum lycopersicum, for varietal identification and to demonstrate the technical viability of these genetic markers for use in the enforcement of U.S. Department of Agriculture marketing order-based identity preservation programs. GeneMapper, a semiautomated software tool, was used for designing multiplex panels, allele identification, and polymorphism pattern evaluation of diverse tomato cultivars. Semiautomated genotyping was performed on a set of 12 microsatellite markers providing genome-wide coverage of the tomato chromosomes. Microsatellites were detected with fluorescently labeled primers grouped into five multiplex panels, and each primer pair was assessed in replicated trials for reliability of allele size estimates. Allele sizes for each locus were compared, and a database for 34 tomato varieties was developed. The microsatellite marker set identified distinct allelic peaks and unique genetic fingerprints for each of the studied tomato varieties. A "blind testing" exercise with UglyRipe™ and Vintage Ripe™ tomato varieties, using the above set of markers and database, further established the usefulness of these microsatellite markers for tomato commodity marketing order enforcement.
Ultra High Pressure Liquid Chromatography for Crude Plant Extract Profiling
Authors: Eugster Philippe J , Guillarme Davy , Rudaz Serge , Veuthey Jean-Luc , Carrupt Pierre-Alain , Wolfender Jean-Luc 
Published: February 2020

Abstract
Ultra high pressure liquid chromatography (UHPLC) systems operating at very high pressures and using sub-2 μm packing columns have allowed a remarkable decrease in analysis time and increase in peak capacity, sensitivity, and reproducibility compared to conventional HPLC. This technology has rapidly been widely accepted by the analytical community and is being gradually applied to various fields of plant analysis such as QC, profiling and fingerprinting, dereplication, and metabolomics. For many applications, an important improvement of the overall performances has been reported. In this review, the basic principles of UHPLC are summarized, and practical information on the type of columns used and phase chemistry available is provided. An overview of the latest applications to natural product analysis in complex mixtures is given, and the potential and limitations as well as some new trends in the development of UHPLC are discussed.
Binary HPLC-Diode Array Detector and HPLC-Evaporative Light-Scattering Detector Fingerprints of Methanol Extracts from the Selected Sage (Salvia) Species
Authors: Sajewicz Mieczysław , Staszek Dorota , Wojtal Łukasz , Kowalska Teresa , Hajnos Michał Ł , Waksmundzka-Hajnos Monika 
Published: February 2020

Abstract
This study is focused on an important family of the sage (Salvia) species, with Salvia officinalis L. having a long-established position in European traditional medicine. Binary fingerprints (chromatographic profiles) of six different sage species were compared using HPLC coupled with two different detectors: the diode-array detector and the evaporative light-scattering detector. Advantages of using binary fingerprinting over single-detector fingerprinting are demonstrated and discussed, with selected examples. Experimental data are provided for a comparison of the chemical composition of sage samples originating from two harvesting seasons (2007 and 2008). A number of phytochemical standards (i.e., certain phenolic acids, flavonoids, and coumarin) were used that allowed identification and semiquantitative estimation of these particular compounds in the analyzed methanol extracts.
Flow Injection Mass Spectroscopic Fingerprinting and Multivariate Analysis for Differentiation of Three Panax Species
Authors: Chen Pei , Harnly James M , Harrington Peter de B 
Published: February 2020

Abstract
This study describes the use of spectral fingerprints acquired by flow injection (FI)-MS and multivariate analysis to differentiate three Panax species: P. ginseng, P. quinquefolius, and P. notoginseng. Data were acquired using both high resolution and unit resolution MS, and were processed using principal component analysis (PCA), soft independent modeling of class analogy (SIMCA), partial least squares-discriminant analysis (PLS-DA), and a fuzzy rule-building expert system (FuRES). Both high and unit resolution MS allowed discrimination among the three Panax species. PLS-DA and FuRES provided classification with 100% accuracy while SIMCA provided classification accuracies of 77 and 88% by high- and low-resolution MS, respectively. The method does not quantify any of the sample components. With FI-MS, the analysis time was less than 2 min.
Validated Determination of Eight Antibiotic Substance Groups in Cattle and Pig Muscle by HPLC/MS/MS
Authors: Bohm Detlef A , Stachel Carolin S , Gowik Petra 
Published: February 2020

Abstract
The described multimethod is suited for the determination of 53 substances of eight antibiotic groupstetracyclines, quinolones, macrolides, sulfonamides, diphenylsulfones, diamino-pyrimidine derivatives, pleuromutilines, and lincosamidesin cattle and pig muscle. All substances were analyzed simultaneously with the same sample preparation and in one HPLC/MS/MS run. The validation of the multimethod was successfully accomplished with the help of an alternative in-house validation concept requiring only 48 experiments. The substances were validated at concentrations of 0.25, 0.5, 1.0, 1.5, and 2.0 MRL (maximum residue limit) or 5, 10, 20, 30, and 40 g/kg for substances without an MRL. The calculated relevant validation parameters were based on and comply with the requirements of Commission Decision 2002/657/EC, i.e., the decision limit, detection capability, repeatability, within-laboratory reproducibility, and recovery. The robustness of the method was demonstrated by varying seven factors of the analytical procedure. Several proficiency tests were carried out successfully to provide evidence for the applicability of the method.
Simultaneous Determination of 20 -Agonists in Pig Muscle and Liver by High-Performance Liquid Chromatography/Tandem Mass Spectrometry
Authors: Liu Chang , Ling Wenting , Xu Weidong , Chai Yifeng 
Published: February 2020

Abstract
A method was developed to determine 20 illegal residual -agonists in pork tissues, including muscle and liver simultaneously. The samples were hydrolyzed by -glucuronidase, purified by PCX SPE cartridges, and detected by HPLC coupled with electrospray ionization MS/MS operating in the positive ion mode. Matrix-fortified calibration was performed to compensate for the matrix effect and loss in sample preparation. Decision limit ranged from 0.05 to 0.23 g/kg in muscle and 0.05 to 0.57 g/kg in liver. Decision capacity ranged from 0.11 to 0.4 g/kg in muscle and 0.16 to 0.79 g/kg in liver. In Food Analysis Performance Assessment Scheme proficiency test 0287, a pig liver test material containing 13 -agonists was analyzed using the method developed, and clenbuterol and ractopaime were confirmed as being present. Z-scores for clenbuterol and ractopaime were 0.2 and 0.6, respectively.
Validated Stability-Indicating HPLC-UV Method for Simultaneous Determination of Glipizide and Four Impurities
Authors: Gupta Sakshi , Bansal Gulshan 
Published: February 2020

Abstract
A selective stability-indicating HPLC-UV method for simultaneous determination of glipizide and four impurities (DPs IIV) formed under hydrolytic conditions was developed and validated. The drug and impurities were resolved on an XTerra C18 column (250 4.5 mm id) in a single gradient run using buffer (0.005 M KH2PO4; pH 3.0)methanol (60 40, v/v; mobile phase A) and (20 80, v/v; mobile phase B) at a flow rate of 0.5 mL/min with 230 nm detection wavelength. The method was linear across concentration ranges of 0.2100, 0.1100, 0.5100, 0.2100, and 0.150 0000g/mL for glipizide and DPs IIV, respectively. The RSD for intraday and interday precision for the drug and impurities was &lt;1 and &lt;1.2, respectively. Satisfactory recoveries (96.5899.97) of each of the three concentrations selected across the linearity range of each analyte were obtained, proving the method was sufficiently accurate. The LOD was 0.07, 0.05, 0.16, 0.08, and 0.05 g/mL and the LOQ was 0.20, 0.14, 0.50, 0.23, and 0.14 g/mL for the drug and DPs IIV, respectively. Each peak was resolved with resolution of &gt;2 from the nearest peak. Insignificant changes in retention time (&lt;4) and calculated amount (&lt;1.65) of drug and each impurity upon small but deliberate changes in various chromatographic parameters were observed, suggesting the method was robust. The method was applied successfully to stability testing of glipizide tablets.
High-Throughput Analysis of Amnesic Shellfish Poisoning Toxins in Shellfish by Ultra-Performance Rapid Resolution LC-MS/MS
Authors: Iglesia Pablo De La , Barber Esther , Giménez Gemma , Rodríguez-Velasco María Luisa , Villar-González Adriano , Diogéne Jorge 
Published: February 2020

Abstract
The application of ultra-performance rapid resolution LC on a 1.8 m particle-size column coupled with tandem MS (RRLC-MS/MS) is described for the analysis of amnesic shellfish poisoning (ASP) toxins in shellfish. Complete resolution among domoic acid (DA) and the isomers was achieved in less than 3 min. The method was intralaboratory validated for direct analysis of crude extracts without further cleanup. It showed LODs ranging from 0.05 to 0.09 mg/kg and a working range that complied with the current regulatory level for DA of 20 mg/kg, and with the level of 4.5 mg/kg recently proposed by the European Food Safety Authority. Confirmatory capabilities were demonstrated according to the Commission Decision 2002/657/EC criteria. The results obtained by RRLC-MS/MS agreed with those provided by the reference LC-UV method, both intralaboratory for the analysis of blind samples (R2 0.9751) and interlaboratory through participation in the proficiency test for ASP toxins during 2009 (z-score 0.962 and 0.177 for low- and high-contaminated samples, respectively). RRLC-MS/MS provided fast analysis and additional confirmatory capabilities for direct analysis of crude extracts while the performance and reliability of the results were maintained, even in very complex matrixes.
Validation Study of Immunoaffinity Column Chromatography Coupled with Solution Fluorometry or HPLC for the Detection of Aflatoxin in Peanuts and Corn
Authors: Lupo Anthony , Quain Anna , Fitzsimmons Alan , Allan Andrew , Popping Bert , Trucksess Mary , Shephard Gordon 
Published: February 2020

Abstract
Neogen Corp. has developed the Neocolumn for Aflatoxin DR for the detection of total aflatoxin by HPLC or solution fluorometry. The purpose of this study was to validate the method under the requirements of the AOAC Research Institute Performance Tested MethodsSM (PTM) program. There are several AOAC Official MethodsSM for detection of total aflatoxin in corn; they consist of rapid and analytical-based methods and two rapid methods (PTMs 030701 and 050901) that have been performance tested by the AOAC Research Institute. A widely used reference method, however, is AOAC Official MethodSM 991.31, which uses immumoaffinity cleanup followed by HPLC or solution fluorometry and is referred to as the reference method in this document. In internal studies, the Neocolumn method coupled with solution fluorometry demonstrated a relative recovery from peanuts of 101.6 of the reference value, with a CV of 3.9 across all levels analyzed; when coupled with HPLC, the Neocolumn method demonstrated a relative recovery from peanuts of 103.0 of the reference value with a CV of 3.5 across all levels analyzed. The Neocolumn method coupled with solution fluorometry demonstrated a relative recovery from corn of 116.9 of the reference value with a CV of 6.1 across all levels analyzed; when coupled with HPLC, the Neocolumn method demonstrated a relative recovery from corn of 91.2 of the reference value, with a CV of 5.4 across all levels analyzed. Calculations were made by comparison with the mean result obtained by the HPLC reference method, which showed respective CV values of 3.9 and 2.0 for recoveries from peanuts and corn, respectively.
Confirmatory Method for the Determination of Volatile Congeners and Methanol in Turkish Raki According to European Union Regulation (EEC) No. 2000R2870: Single-Laboratory Validation
Authors: Yilmaztekin Murat , Cabaroglu Turgut 
Published: February 2020

Abstract
A method described by European Union Regulation (EEC) No. 2000R2870 was validated and supported by GC/MS analysis for the determination of volatile congeners and methanol in Turkish raki. The method was validated in terms of specificity, accuracy, precision, LOD, LOQ, linearity, and robustness. The specificity of the method was demonstrated, and the method showed excellent accuracy (97.5100.1). Linearity was checked in the ranges of 0.20026.390 mg/100 mL for more volatile compounds and 1.15548.00 mg/100 mL for less volatile compounds, after concentrations found in Turkish raki were taken into account. The calibration curves of all analytes showed good linearity (R2 &gt; 0.998). The within- and between-day precision (RSD) values of 11 analytes were in the range of 0.184.50. The LOD and LOQ values were in the range of 0.0140.362 and 0.0451.085 mg/100 mL, respectively. The method can be used as an absolute quantification method for the determination of volatile congeners and methanol in Turkish raki and for QC.
An Easy and Practical Method for Detection and Estimation of Microcrystalline Cellulose in Pasteurized Milk
Authors: Zhang Chi , Yang Jun , Qiao Ling 
Published: February 2020

Abstract
Microcrystalline cellulose (MCC) is suspected to be a new adulteration in pasteurized milk in China, yet an efficient method for MCC detection in dairy has not been established. This study presents a novel procedure to detect and estimate MCC in pasteurized milk using dialysis, cellulase hydrolysis, and a reducing sugar assay. The background value of reducing sugar was eliminated by dialysis, and cellulase activity toward MCC was stable in dialyzed milk. A criterion for MCC detection and an empirical formula for MCC estimation were summarized based on the reducing sugar variation after hydrolysis. The detection sensitivity was below 0.5 g/L. Reducing sugar distribution after cellulase-catalyzed hydrolysis was examined by HPLC, and revealed that most of the detected sugar was glucose. This paper describes a practical method for detection of MCC in pasteurized milk that might benefit dairy QC.
Rapid Determination of Fumagillin Residues in Honey by Liquid Chromatography–Tandem Mass Spectrometry Using the QuEChERS Method
Authors: Kanda Maki , Sasamoto Takeo , Takeba Kazue , Hayashi Hiroshi , Kusano Tomoko , Matsushima Yoko , Nakajima Takayuki , Kanai Setsuko , Takano Ichiro 
Published: February 2020

Abstract
A new, rapid, and efficient method for determining the fumagillin residues in honey was developed. The samples extracted were analyzed using LC/MS/MS. Chromatographic separation of fumagillin was performed in gradient mode on a C8 column (100 × 2.0 mm, 5 μm) at 40°C. The mobile phase consisted of a mixture of 2 mM ammonium formate–0.01% formic acid solution and methanol; the flow rate was set to 0.2 mL/min. Under these conditions, it was possible to measure fumagillin and its isomers as a single peak. The sample preparation procedure used is based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which is fast (approximately 30 min) and uses less organic solvent. The fumagillin was extracted with acetonitrile containing 0.1% formic acid, then purified using a solid-phase extraction method with an Oasis® mixed-mode weak anion-exchange cartridge. The overall recovery of fumagillin ranged from 88.1 to 99.4%; the intra- and interassay CVs were &lt;4.5% and &lt;4.9%, respectively. The LOQ was 0.1 μg/kg. LC/MS/MS coupled with the QuEChERS method showed strong potential as a method for determining fumagillin residues in honey.