bluuebunny/crossref_metadata_2025_split huggingface dataset:
Development and Validation of a Novel Stability-Indicating Reversed-Phase High-Performance Liquid Chromatography Method for Assay of Loratadine and Determination of Its Related Compounds
Authors: Lu Jun , Wei Yu-Chien , Markovich Robert J , Rustum Abu M 
Published: February 2020

Abstract
Loratadine is an important active pharmaceutical ingredient used in a wide variety of prescription and over-the-counter products for the treatment and relief of allergy symptoms. A novel stability-indicating gradient ion-pair RP-HPLC method for assay of loratadine and determination of both of its degradation compounds and process impurities has been developed. This method can separate loratadine from its eight structurally related compounds; it can also separate all of the related compounds from each other in less than 20 min. The stability-indicating capability of this method has been demonstrated by analyzing aged stability samples of loratadine. A 15 cm 4.6 mm id YMC-Pack Pro C18 HPLC column was the primary column and a 15 cm 4.6 mm id SunFire C18 column has been identified as an alternate (truly equivalent) column for this method. This gradient method uses mobile phases consisting of acetonitrile and an aqueous solution of 10 mM sodium acetate and 5 mM sodium dodecyl sulfate at pH 5.5. The new HPLC method was validated according to International Conference on Harmonization guidelines and proved to be suitable for routine QC use.
Comparison of FoodChek E. coli Test and AOAC Research Institute Performance Tested Method 010603 for Detection of E. coli O157 in Raw Ground Beef
Authors: Flanagan Richard J , Martinez Gabriela 
Published: February 2020

Abstract
The FoodChek E. coli O157 assay [AOAC Research Institute (RI) Performance Tested Method (PTM) 060902] is a rapid detection system that incorporates the use of antibody-coated superparamagnetic nanoparticles in a lateral flow immunoassay format. The system comprises a commercially available enrichment medium, a magnetic nanoparticle immunoassay, and an automated reader for detection. Assay detection threshold is improved relative to traditional immunoassays through use of a magnetic nanoparticle label and a highly sensitive magnetic particle detector. FoodChek E. coli O157 is a reintroduction of the previously certified AOAC PTM 010603. The original assay was evaluated and approved in internal and independent laboratory studies. Vacci-Test Corp. has contracted with the original supplier of the PTM to remanufacture the test under identical conditions and with identical raw materials. This report is intended to show that FoodChek E. coli is identical in performance to the previously approved PTM. The results showed no difference for the parameters evaluated. Three kit lots along with three lots of media and media supplement were compared in lot-to-lot and stability testing. The results indicated no difference in performance across the three lots. The results showed sensitivity of &gt;99 and a specificity rate of &gt;98 for the FoodChek method and a significantly higher sensitivity than the reference method.
Correlation Between Aflatoxin Contamination and Various USDA Grade Categories of Shelled Almonds
Authors: Whitaker Thomas B , Slate Andy , Birmingham Tim , Adams Julie , Jacobs Merle , Gray Gary 
Published: February 2020

Abstract
The California almond industry is interested in determining if there is a correlation between aflatoxin contamination and almonds classified into various U.S. Department of Agriculture (USDA) grades. A 12 000 g sample was taken from each of 50 lots of shelled almonds. The almonds in each sample were then partitioned into five USDA grades: high quality (HQ), insect damage (ID), mold damage (MOD), mechanical damage (MED), and other defects (OD). Across all 50 samples, kernels in the HQ grade accounted for 83.7 of the kernel mass and 3.2 of the aflatoxin mass. Conversely, kernels in the remaining four damage grades (ID, MOD, MED, and OD) accounted for 16.3 of the kernel mass and 96.8 of the aflatoxin mass. ID kernels had the highest risk for aflatoxin contamination. Almonds in the ID grade accounted for 76.3 of the total aflatoxin mass and 7.2 of the kernel mass. Regression equations were developed to predict the aflatoxin concentration in each 12 000 g sample by measuring the aflatoxin mass in one or more of the four damage grades. Regression equations demonstrated that aflatoxin mass only in the insect damaged kernels was also an effective way to predict the aflatoxin concentration in each 12 000 g sample.
Validation of a Column Liquid Chromatographic Method for the Analysis of Pramipexole and Its Five Impurities
Authors: Malenović Andjelija , Jančić-Stojanović Biljana , Vemić Ana , Ivanović Darko , Medenica Mirjana 
Published: February 2020

Abstract
In this paper, a previously optimized method for HPLC analysis of pramipexole and its impurities was subjected to method validation in accordance with official regulations. The optimized chromatographic conditions were as follows: mobile phase acetonitrilewater phase [15 + 85, v/v, water phase contained 1 triethylamine (TEA), pH adjusted to 7.0 with orthophosphoric acid]; detection at 262 nm for pramipexole, BI-II 751 xx, BI-II 786 BS, BI-II 820 BS, and 2-aminobenzothiazole and at 326 nm for BI-II 546 CL; column temperature, 25C; and flow rate, 1 mL/min. Acetonitrile and TEA content, pH of the water phase, flow rate, column temperature, and column type were factors studied in robustness testing. According to the experimental plan defined by a Plackett-Burman design, five dummy variables were added in order to have 12 factors. As output, resolution factor was chosen. Robustness was assessed by graphical (half-normal probability plots and Pareto charts) and statistical (t-test) methods. Also, nonsignificance intervals for significant factors were estimated, and limits for the system suitability test were determined. Finally, linearity, accuracy, and precision of the proposed HPLC method were defined. LOD and LOQ values for analyzed impurities were determined. The method was completely defined by these experiments.
High-Performance Liquid Chromatographic Determination of Pantoprazole and Its Main Impurities in Pharmaceuticals
Authors: Letica Jelena , Marković Slavko , Zirojević Jelena , Nikolić Katarina , Agbaba Danica 
Published: February 2020

Abstract
An RP-HPLC method for simultaneous separation and quantification of pantoprazole and its five main impurities in pharmaceutical formulations was developed and validated. The separation was accomplished on a Zorbax Eclipse XDB C18 column (5 m particle size, 150 4.6 mm id) using a gradient with mobile phase A [bufferacetonitrile (70 + 30, v/v)], and mobile phase B [bufferacetonitrile (30 + 70, v/v)]. The buffer was 0.01 M ammonium acetate solution with addition of 1 mL triethylamine/L of the solution, adjusted to pH 4.5 with orthophosphoric acid. The eluent flow rate was 1 mL/min, the temperature of the column was 30C, and the eluate was monitored at 290 nm. Linearity (r = 0.999), recovery (97.6105.8), RSD (0.551.90), and LOQ (0.0991.48 g/mL) were evaluated and found to be satisfactory. The proposed method can be used for simultaneous identification and quantification of the analyzed compounds in pharmaceutical formulations.
Determination of Fumonisin B1 in Botanical Roots by Liquid Chromatography with Fluorescence Detection: Single-Laboratory Validation
Authors: Oles Carolyn J , Trucksess Mary W 
Published: February 2020

Abstract
The accuracy, repeatability, and reproducibility characteristics of a published method for measuring levels of fumonisin B1(FB1) in botanical root products were determined by an AOAC single-laboratory validation procedure. Replicates of 10 test portions of each powdered root product (black cohosh, echinacea, ginger, ginseng, valerian, dong quai, and turmeric) at each spiking level (FB1 at 0, 50, 100, and 200 ng/g) were analyzed on 3 separate days. Test samples were extracted with methanolacetonitrilewater (25 + 25 + 100, v/v/v). The extracts were centrifuged, the supernatants diluted with phosphate-buffered saline (PBS) containing 1 Tween 20 and filtered, and the filtrates applied to an immunoaffinity column containing antibodies specific for fumonisins. After the column was washed sequentially with PBS and water, the toxin was eluted from the column with 80 methanol, and the eluate dried by lyophilization. The residue was reconstituted with 50 acetonitrile. FB1 was derivatized with a mixture of O-phthaldialdehyde and mercaptoethanol by using an LC autoinjector. Separations were performed with an RP-LC column, and the FB1 derivative was quantified by fluorescence detection. All root products were found to contain FB1 at &lt;10 ng/g. Average within- and between-day recoveries of FB1 from the botanical roots ranged from 67 to 95 and from 68 to 100, respectively. Total RSD values for within- and between-day repeatability ranged from 5.5 to 26.4. HorRat values were &lt;1.3 for all of the matrixes examined. The method meets the AOAC method performance criteria at levels of &gt;50 ng/g for the seven botanical roots tested.
Determination of Deoxynivalenol in Processed Foods
Authors: Trucksess Mary W , Bao Lei , Weaver Carol M , White Kevin D 
Published: February 2020

Abstract
Deoxynivalenol (DON), commonly referred to as vomitoxin, belongs to a class of naturally occurring mycotoxins produced by Fusarium fungi. The presence of DON in foods is a human health concern. The frequency of occurrence of DON in wheat is high, although cleaning prior to milling can reduce DON concentration in final products, and food processing can partially degrade the toxin. This paper describes a method for the determination of DON in some major wheat food products, including bread, breakfast cereals, pasta, pretzels, and crackers. Test samples containing 5 polyethylene glycol were extracted with water. After blending and centrifuging, the supernatant was diluted with water and filtered through glass microfiber filter paper. The filtrate was then passed through an immunoaffinity column and the toxins eluted with methanol. The toxins were then subjected to RPLC separation and UV detection. The accuracy and repeatability characteristics of the method were determined. Recoveries of DON spiked at levels from 0.5 to 1.5 g/g in the five processed foods were &gt;70. SD and RSD values ranged from 2.0 to 23.5 and from 2.0 to 23.2, respectively. HorRat values were &lt;2 for all of the matrixes examined. The method was found to be acceptable for the matrixes examined. LC/MS/MS with multiple-reaction monitoring was used to confirm the identity of DON in naturally contaminated test samples.
Simple Gas Chromatographic Method for the Quantification of Total Cholesterol in Fish Meats
Authors: Memon Nusrat N , Sherazi Syed Tufail H , Talpur Farah N , Bhanger Muhammad I 
Published: February 2020

Abstract
Six fish speciesCirrhinus mrigala (Morakhi), Labeo rohita (Danbhro), Catla catla (Thalli), Wallago attu (Jarko), Ctenopharyngodon idella (Grass), and Cyprimus carpio (Gulfam)commonly found in the Pakistani Indus river, were selected for fat and cholesterol evaluation. Fat content was quantified by the Folch method and cholesterol content was determined by a simple GC method. The application of the proposed method to quantify cholesterol content revealed variations among the six breeds evaluated. The breeds studied contained 0.801.95 fat, indicating that all investigated fishes were lean; significant variation was found in cholesterol content, and ranged between 72 and 392 mg/100 g. Standard addition analyses showed that the method was accurate, as the recovery of cholesterol varied from 95 to 103, with a coefficient of variance not more than 5.6. The results showed that, after the development of suitable calibration, within 11 min, the cholesterol could be accurately determined by GC.
Rapid Determination of Fluoroquinolone Residues in Honey by a Microbiological Screening Method and Liquid Chromatography
Authors: Kanda Maki , Kusano Tomoto , Kanai Setsuko , Hayashi Hiroshi , Matushima Yoko , Nakajima Takayuki , Takeba Kazue , Sasamoto Takeo , Nagayma Toshijiro 
Published: February 2020

Abstract
A rapid and efficient method was developed for the simultaneous determination of seven fluoroquinolone (FQ) residues: norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin in honey. The samples were first screened with a microbiological method by using test plates made from metal-free purified agar seeded with Bacillus subtilis BGA. When a sample was found to contain FQ residues by using the microbiological method, it was analyzed by LC with fluorescence detection (LC/FL). FQs were extracted with Na2EDTA-McIlvaine buffer and purified by a dual SPE method in which a cation-exchange cartridge was connected to an anion-exchange cartridge. The overall recoveries of the seven FQs ranged from 70.0 to 92.1. The intra-assay and interassay CVs were 7.8 and 5.1, respectively. For the microbiological method, the LOD values ranged from 2 to 9 g/kg. For LC/FL, the LOQ values ranged from 2 to 7 g/kg. The developed method was used to analyze 70 honey samples. In 14 samples in which the microbiological method detected the presence of FQ residues, norfloxacin, ciprofloxacin, and enrofloxacin were identified by LC/FL.
Modern HPTLCA Perfect Tool for Quality Control of Herbals and Their Preparations
Authors: Meier Beat , Spriano Daniela 
Published: February 2020

Abstract
Herbals and herbal preparations are complex mixtures with numerous natural compounds in an uncharacterized matrixtruly multicomponent systems. This is in contrast to most of the samples of the pharmaceutical and, in part, the food industry, where primarily single compounds have to be analyzed. Recently, models for the characterization of multicomponent systems with near-IR, NMR, and MS combined with chemometric tools have been developed. However, the complexity and sophistication of such methods still prevent their general applicability to the QC of herbals. On the other hand, modern TLC is a well-established method with a long tradition. The typical chromatograms visualize even complex multicomponent systems in a special manner. The technique is rapid, comparatively simple, robust, and extremely versatile. HPTLC can not only confirm but also establish identity. It is also an ideal screening tool for adulterations and is highly suitable for evaluation and monitoring of cultivation, harvesting, and extraction processes and testing of stability. To substantiate these claims, several examples taken from daily work are provided and discussed in this paper.
Simultaneous Determination of Seven Alkaloids in Phellodendron chinense Schneid by High-Performance Liquid Chromatography
Authors: Liu Yong , Chen Juan , Li Xue-Hu , Shi Yan-Ping 
Published: February 2020

Abstract
By optimizing the extraction, separation, and analytical conditions, a reliable and accurate HPLC method coupled with a photodiode array detector was developed for simultaneous detection and quantification of seven alkaloids, i.e., (-)-(R)-platydesmin, noroxyhydrastinine, berberine, skimmianine, canthin-6-one, chilenine, and pteleine in huangbo (the bark of Phellodendron chinense), a commonly used herb in Traditional Chinese Medicine. The optimal condition for separation was achieved on a reversed-phase C18 column with a stepwise mobile phase gradient prepared from 0.1% phosphoric acid and acetonitrile. For all the alkaloids, a good linear regression relationship (r &gt; 0.9997) was obtained between the peak area and concentration at the range of 0.5700 µg/mL. The LODs and LOQs for the analytes ranged from 0.07 to 0.28 µg/mL and from 0.28 to 1.12 µg/mL, respectively. The optimized method was applied to the determination of alkaloids in several P. chinense samples, and found to be feasible and reliable. This method and quantitative results can provide scientific and technical bases for setting up QC standards to assure the safety and quality of P. chinense bark raw material, as well as for proprietary Chinese medicine products containing P. chinense bark.
Fast HPLC Method Using Ion-Pair and Hydrophilic Interaction Liquid Chromatography for Determination of Phenylephrine in Pharmaceutical Formulations
Authors: Douòa Michal , Gibala Petr 
Published: February 2020

Abstract
A rapid procedure based on a direct extraction and HPLC determination with fluorescence detection of phenylephrine in pharmaceutical sachets that include a large excess of paracetamol (65 + 1, w/w), ascorbic acid (5 + 1, w/w), and other excipients (aspartame and sucrose) was developed and validated. The final optimized chromatographic method for ion-pair chromatography used an XTerra RP18 column, 3 µm particle size, 50 ⨯ 3.0 mm id. The mobile phase consisted of a mixture of acetonitrile and buffer (10 mM sodium octane-1-sulfonate, adjusted with H3PO4 to pH 2.2; 200 + 800, v/v), with a constant flow rate of 0.3 mL/min. The separation was carried out at 30C, and the injection volume was 3 µL. Fluorescence detection was performed at excitation and emission wavelengths of 275 and 310 nm, respectively. The mobile phase parameters, such as the organic solvent fraction (acetonitrile) in mobile phase as an organic modifier, the concentration of sodium octane-1-sulfonate as a counter-ion, temperature, and pH of mobile phase, were studied. As an alternative to ion-pair chromatography, hydrophilic interaction liquid chromatography (HILIC) was investigated using a Luna HILIC column, 3 m, 100 ⨯ 4.6 mm id. The mobile phase consisted of acetonitrile and buffer (5 M potassium dihydrogen phosphate, adjusted with H3PO4 to pH 2.5; 750 + 250, v/v) at a flow rate of 0.8 mL/min. The separation was carried out at 25°C, and the injection volume was 5 µL. The proposed method has an advantage of a very simple sample pretreatment, and is much faster than the currently utilized HPLC methods using gradient elution and UV detection. Commercial samples of sachets were successfully analyzed by the proposed HPLC method.
Rapid Determination of Fumonisins in Corn-Based Products by Liquid Chromatography/Tandem Mass Spectrometry
Authors: Li Wei , Herrman Timothy J , Dai Susie Y 
Published: February 2020

Abstract
A simple, fast, and robust method was developed for the determination of fumonisin B1 (FB1), fumonisin B2 (FB2), and fumonisin B3 (FB3) in corn-based human food and animal feed (cornmeal). The method involves a single extraction step followed by centrifugation and filtration before analysis by ultra-performance liquid chromatography/electrospray ionization (UPLC/ESI)-MS/MS. The LC/MS/MS method developed here represents the fastest and simplest procedure (&lt;30 min) among both conventional HPLC methods and other LC/MS methods using SPE cleanup. The potential for high throughput analysis makes the method particularly beneficial for regulatory agencies and analytical laboratories with a high sample volume. A single-laboratory validation was conducted by testing three different spiking levels (200, 500, and 1000 ng/g for FB1 and FB2; 100, 250, and 500 ng/g for FB3) for accuracy and precision. Recoveries of FB1 ranged from 93 to 98% with RSD values of 3-8%. Recoveries of FB2 ranged from 104 to 108, with RSD values of 2-6%. Recoveries of FB3 ranged from 94% to 108%, with RSD values of 2-5%.
Determination of Vitamin A (Retinol) in Infant and Medical Nutritional Formulas with AOAC Method 992.06 Using a Modified Extraction Procedure: Single-Laboratory Validation
Authors: Thompson Linda B , Schimpf Karen J , Stiner Lisa A , Schmitz Daniel J 
Published: February 2020

Abstract
The applicability of AOAC Official MethodSM 992.06, Vitamin A (Retinol) in Milk-Based Infant Formula can be extended to specialty infant formulas, and medical and adult nutritional products with a few minor modifications to the sample preparation procedure. Currently, AOAC Official MethodSM9 92.06 is only applicable to milk-based infant formulas containing &gt;500 IU vitamin A per reconstituted quart. When this method is used as written to test specialty infant formulas, vitamin A recoveries are low compared to results generated with alternate validated vitamin A methods. AOAC Method 992.06 vitamin A recoveries can be improved significantly in specialty infant formulas if the amount of potassium hydroxide used during the saponification step is doubled. With this one minor modification to the sample preparation procedure, AOAC Method 992.06 demonstrates acceptable precision and accuracy for the quantitation of vitamin A (retinol) in specialty infant formulas, milk- and soy-based infant formulas, and adult and medical nutritionals. Because increasing the amount of potassium hydroxide can cause emulsions to form, 24 mL aliquots of reagent alcohol may need to be added to some samples to separate the organic and aqueous layers during the extraction step. A single-laboratory validation of these modifications was completed. During validation, 15 different product matrixes were analyzed. The intermediate precision averaged 2.70% RSD, and spike recovery data averaged 96.3%.
SYBR Green Real-Time PCR Used to Detect Celery in Food
Authors: Wu Yajun , Chen Ying , Wang Bin , Gao Yunhua , Bai Liqun , Wang Haiyan 
Published: February 2020

Abstract
Celery was found to provoke human allergenic response in some countries. Labeling of celery ingredients was required by the European Union, and the threshold set at 10 mg/kg (0.001%). In our study, a celery mannitol transporter (Mat3) gene-based detection method was established by means of SYBR Green real-time PCR technique. No cross-reactivity was found between celery and the other food materials. Absolute detection limit (LODa), relative detection limit (LODr), and practical detection limit (LODp) of the method were determined through experiments on pure celery DNA, DNA mix, and spiked food samples. The method was able to detect 0.001 raw food sample and 0.01 heated food sample. The utility of the method was confirmed by the investigation of 13 commercial foods.
Determination of Quaternary Ammonium Compounds by Potentiometric Titration with an Ionic Surfactant Electrode: Single-Laboratory Validation
Authors: Price Randi , Wan Ping 
Published: February 2020

Abstract
A potentiometric titration for determining the quaternary ammonium compounds (QAC) commonly found in antimicrobial products was validated by a single laboratory. Traditionally, QACs were determined by using a biphasic (chloroform and water) manual titration procedure. Because of safety considerations regarding chloroform, as well as the subjectivity of color indicator-based manual titration determinations, an automatic potentiometric titration procedure was tested with quaternary nitrogen product formulations. By using the Metrohm Titrando system coupled with an ionic surfactant electrode and an Ag/AgCl reference electrode, titrations were performed with various QAC-containing formulation products/matrixes; a standard sodium lauryl sulfate solution was used as the titrant. Results for the products tested are sufficiently reproducible and accurate for the purpose of regulatory product enforcement. The robustness of the method was measured by varying pH levels, as well as by comparing buffered versus unbuffered titration systems. A quantitation range of 11000 ppm quaternary nitrogen was established. Eight commercially available antimicrobial products covering a variety of matrixes were assayed; the results obtained were comparable to those obtained by the manual titration method. Recoveries of 94 to 104% were obtained for spiked samples.