bluuebunny/crossref_metadata_2025_split huggingface dataset:
Validated Reversed-Phase Column High-Performance Liquid Chromatographic Method for Separation and Quantification of Polyphenolics and Furocoumarins in Herbal Drugs
Authors: Govindarajan Raghavan , Singh Dhirendra Pratap , Rawat Ajay Kumar Singh 
Published: February 2020

Abstract
A rapid column high-performance liquid chromatographic-photodiode array method has been developed for the separation and identification of secondary metabolites, especially different types of phenols and furocoumarins, in a 35 min chromatographic run. The method has been optimized and validated for selectivity, precision, recovery, and robustness with the aim of application for standardization of selected herbal drugs. Almost all of the tested compounds had linearity of &gt;98, with relative standard deviation &lt;10 in terms of variation of retention time. Interday and intraday variability was &lt;5. The developed method has been successfully applied in identification and quantification of phenols and furocoumarins present in different plants, viz., Artemisia pallens (whole plant), Hibiscus rosa-sinensis DC (flower), Heracleum candicans DC (fruit), and Ficus carica Linn (bark). The results indicate that the method is rapid, accurate, and robust for the analysis of different types of phenols and furocoumarins and, hence, can be successfully used in the quality control and standardization of plant extracts and herbal drugs.
Development and Validation of a High-Performance Thin-Layer Chromatographic Method, with Densitometry, for Quantitative Analysis of Ketorolac Tromethamine in Human Plasma
Authors: López-Bojórquez Ericka , Castañeda-Hernández Gilberto , Parra Mario González-de la , Namur Salvador 
Published: February 2020

Abstract
Ketorolac tromethamine is a potent nonsteroidal anti-inflammatory drug that is widely used in the treatment of moderate to severe pain. A new method was developed and validated for quantifying ketorolac (the free acid of the tromethamine salt) in human plasma by high-performance thin-layer chromatography. The stationary phase was silica gel 60, and the composition of the mobile phase was n-butanolchloroformacetic acidammonium hydroxidewater (9 3 5 1 2, v/v). The densitometric analysis of ketorolac was performed at 323 nm. The method was validated for precision (repeatability and reproducibility), accuracy, and sensitivity. Repeatability was 10.11% [coefficient of variation (CV)] and reproducibility was 12.18% (CV) as the maximum variation. Accuracy was determined at 3 different concentration levels, and results were within 15% of the predetermined range. Data were fitted by a linear mathematical function (linear regression). The calibration graph was linear in the range of 2002000 ng/mL. Average recovery was 73.67%. The method proved to be accurate, precise, and sensitive for the ketorolac tromethamine quantification.
Rapid High-Performance Thin-Layer Chromatographic Method for Detection of 5 Adulteration of Black Cohosh with Cimicifuga foetida, C. heracleifolia, C. dahurica, or C. americana
Authors: Ankli Anita , Reich Eike , Steiner Mario 
Published: February 2020

Abstract
Black cohosh (Cimicifuga racemosa) is used to treat discomfort during menopause and as a substitute for synthetic drugs in hormone replacement therapy. The mostly wildcrafted plant is ranked among the top-selling herbs in the United States. There is a risk for adulteration with the similar-looking C. americana, which grows in the same habitats of the eastern United States. Other adulterants found in today's global marketplace are the 3 Asian Cimicifuga species C. foetida, C. heracleifolia, and C. dahurica. A very practical, rapid, and reliable high-performance thin-layer chromatographic (HPTLC) method was developed for identification of C. racemosa and detection of its most common adulterants by fingerprint profiles. With specific derivatization reagents, mixtures of C. racemosa with a minimum of 5 of one of the adulterants can be detected. The proposed method was validated with respect to specificity, stability, precision, and robustness. It can be used for quality control of black cohosh raw material in a current Good Manufacturing Practices environment.
Comparative Evaluation of Methods Commonly Used to Determine Antimicrobial Susceptibility to Plant Extracts and Phenolic Compounds
Authors: King Thea , Dykes Gary , Kristianti Ruth 
Published: February 2020

Abstract
A comparison was made to evaluate the ability of the most commonly used qualitative agar diffusion methods and a quantitative broth dilution assay to determine the antimicrobial activity of a plant extract and a variety of phenolic compounds. A disc and well diffusion technique and a microtiter broth microdilution (MBM) assay were used as antimicrobial susceptibility tests of a plant extract and several phenolic compounds against 7 bacterial species. In both the well and disc diffusion assays, the level of reproducibility was poor and a linear or logarithmic relationship did not exist between inhibition zone size and the concentration of the agents. The MBM method produced the most consistent results and allowed the determination of the relative sensitivities of each species and the relative antimicrobial activities of each agent. This study demonstrated that when a diffusion method is used, multiple concentrations of the agent must be assayed to ensure that a relationship exists between the concentration of the agent and inhibition zone size. When a relationship does not exist, antimicrobial activity should be determined by a quantitative dilution technique.
Determination of Flumorph Residues in Vegetables, Soil, and Natural Water by Solid-Phase Extraction Cleanup and High-Performance Liquid Chromatography with UV Detection
Authors: Hu Ji-Ye , Zhang Yu-Chao , Yan Hai 
Published: February 2020

Abstract
A method for high-performance liquid chromatographic (HPLC) determination of flumorph residues in cucumber, tomato, soil, and natural water was developed and validated. Primary secondary amine or octadecylsilyl (C18) solid-phase extraction cartridges were used for sample preparation. Reversed-phase HPLC with UV detection was used for separation and quantification of the pesticide. The combined cleanup and chromatographic method steps were sensitive and reliable for simultaneous determination of residues of the 2 isomers of flumorph in the studied samples. This method is characterized by recovery &gt;97.9, coefficient of variation &lt;6.2, and limit of quantification of 0.01 mg/kg, in agreement with directives for method validation in residue analysis. Flumorph residues in the samples were further confirmed by HPLC/mass spectrometry. The proposed method is fast, easy to perform, and could be used for monitoring of pesticide residues.
Quantitative Determination of Quinocetone and Its Metabolites in Chicken Plasma by Liquid Chromatography/Tandem Mass Spectrometry
Authors: Li Yong , Gao Zhi Xian , Dong FangTing , Cheng Yi Yong 
Published: February 2020

Abstract
A new method has been established for the simultaneous determination of the new veterinary drug quinocetone (3-methyl-2-cinnamoyl-N-1,4-dioxyquioxaline; QTN) and its 2 metabolites de-monoxy-quinocetone (3-methyl-2-cinnamoyl-N-1-monoxyquinoxaline; DMO-QTN) and de-dioxyquinocetone (3-methyl-2-cinnamoyl-N-quinoxaline; DDI-QTN) in chicken plasma by liquid chromatography/tandem mass spectrometry (LC/MS/MS). The detection was performed using electrospray ionization in multiple reaction monitoring mode. The analysis of the linearity, accuracy, and precision of the method is described. The limits of detection and quantification of the LC/MS/MS method used for testing QTN, DMO-QTN, and DDI-QTN were 0.002 and 0.008 g/mL; 0.002 and 0.008 g/mL; and 0.003 and 0.010 g/mL, respectively. The method was validated and can be used in future pharmacokinetic studies.
Identification of Cervidae DNAin Feedstuff Using a Real-Time Polymerase Chain Reaction Method with the New Fluorescence Intercalating Dye EvaGreen
Authors: Chen Ying , Wu Yajun , Wang Jing , Xu Baoliang , Zhong Zhengyu , Xia Jingshi 
Published: February 2020

Abstract
A real-time qualitative and quantitative polymerase chain reaction method (cer-194) using the fluorescence dye EvaGreen and aimed at the cytochrome b sequence was established for detection of cervidae DNA in feedstuff. Eight meat meal samples derived from deer, bovine, ovine, camel, pig, rabbit, fish, and chicken and 17 cervidae hair samples covering 2 subfamilies, 4 genera, and 7 species were tested to prove the specificity of the cer-194 system and its universality within the cervidae family. Detection limit of 0.1 deer meat in fish meal, blood powder, and feather powder matrixes was confirmed.
Progress on the Development and Single-Laboratory Validation of a High-Performance Liquid Chromatographic Method for the Determination of Carbadox and Pyrantel Tartrate in Type B and C Medicated Feeds
Authors: Sabbatini Jane Z 
Published: February 2020

Abstract
Carbadox, an antimicrobial agent, and pyrantel tartrate, an anthelmintic, are feed additives that are often used in combination in the United States. The current AOAC methods for these analytes are spectrophotometric, using standard addition techniques. These methods are labor-intensive and prone to variability as well as matrix interferences. Published methods for both analytes that use high-performance liquid chromatography were evaluated and a test method was developed. The method uses a water prewetting step to enhance extraction of pyrantel followed by extraction with acetonitrileethanol (50 + 50). Sample extracts are filtered through a glass fiber filter and purified using alumina solid-phase extraction columns. Chromatography is performed on a C18 column with a gradient mobile phase of dibutylamine acetate and acetonitrile. The data show that both analytes exhibit acceptable peak shape when a C18 column that is both acid- and base-deactivated is used. Linearity has been established and initial recovery studies on medicated swine feeds are promising.
Determination of 142 Pesticides in Fruit- and Vegetable-Based Infant Foods by Liquid Chromatography/Electrospray Ionization-Tandem Mass Spectrometry and Estimation of Measurement Uncertainty
Authors: Wang Jian , Leung Daniel 
Published: February 2020

Abstract
A liquid chromatographic/electrospray ionization-tandem mass spectrometric method was developed and validated to determine 142 pesticides in fruit- and vegetable-based infant foods, including apples, apples and bananas, pears, bananas, apple juice, peas, sweet potatoes, creamed corn, squash, and carrots. Pesticides were extracted from infant foods by using the procedure known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Quantification was based on matrix-matched standard calibration curves with the use of an isotopically labeled standard or a chemical analogue as the internal standard to obtain method accuracy. The method performance parameters, including overall recovery, intermediate precision, and measurement uncertainty, were evaluated on the basis of a nested design. The performance results were calculated by using a compiled SAS program that provided a semiautomated procedure for handling a large number of calculations in a few seconds. In general, the overall recoveries, for spiking levels of 10, 50, and 80 g/kg, fell in a range of 81110, intermediate precisions were &lt;20, and measurement uncertainties were &lt;40. Chlorimuron-ethyl, ethofenprox, haloxyfop, naptalam, primisulfuron-methyl, pyridalyl, pyridate, quizalofop, and tebufenozide were the method problematic pesticides that had large measurement uncertainty (&gt;40) due to low recovery and/or poor repeatability. The method provided an analytical range of 1100 g/kg with the lowest concentration level at 1 g/kg for all pesticides (signal-to-noise ratio of &gt;10), except for aclonifen at 5 g/kg.
Determination of 7B3 Residues in Cotton Plants by Liquid Chromatography/Mass Spectrometry
Authors: Yan Xiao-Jing , Liang Xiao-Mei , Xu Yan-Jun , Jin Shu-Hui , Wang Dao-Quan 
Published: February 2020

Abstract
A method was developed for the determination of 7B3 (12-propyloxyimino-1,15-pentadecanlactam), a novel macrolactam fungicide, by liquid chromatography/mass spectrometry (LC/MS) with positive electrospray ionization (ESI+). The method used a reversed-phase C18 column and acetonitrilewater (60 + 40, v/v) mobile phase. The quick, easy, cheap, effective, rugged, and safe method was used for extraction of 7B3 from cotton plants, which involved the extraction of 10 g homogenized sample with 10 mL acetonitrile, followed by the addition of 4 g anhydrous MgSO4 and 1.0 g NaCl. After centrifugation, 1 mL of the buffered acetonitrile extract was transferred into a tube containing 50 mg primary secondary amine sorbent and 100 mg anhydrous MgSO4. After shaking and centrifugation, the final extract was transferred to an autosampler vial for concurrent analysis by LC/MS. The results of 7B3 determined by LC/MS in the selective ion monitoring mode were linear, and the matrix effect of the method was evaluated. The average recoveries of 7B3 fortified at different levels were within 84.1100.2, and the relative standard deviations were &lt;7.5 for all samples analyzed. The method limit of detection and the limit of quantitation values were 0.03 and 0.1 mg/kg, respectively. The proposed method was successfully applied to determine 7B3 residues in practical samples. This method is sensitive, accurate, reliable, simple, and safe.
Analytical Determination of Virginiamycin Drug Residues in Edible Porcine Tissues by LC-MS with Confirmation by LC-MS/MS
Authors: Boison Joe , Lee Stephen , Gedir Ron 
Published: February 2020

Abstract
A liquid chromatographic-mass spectrometric (LC-MS) method was developed and validated for the determination and confirmation of virginiamycin (VMY) M1 residues in porcine liver, kidney, and muscle tissues at concentrations 2 ng/g. Porcine liver, kidney, or muscle tissue is homogenized with methanolacetonitrile. After centrifugation, the supernatant is diluted with phosphate buffer and cleaned up on a C18 solid-phase extraction cartridge. VMY in the eluate is partitioned into chloroform and the aqueous upper layer is removed by aspiration. After evaporating the chloroform in the residual mixture to dryness, the dried extract is reconstituted in mobile phase and VMY is quantified by LC-MS. Any samples eliciting quantifiable levels of VMY M1 (i.e., at concentrations 2 ng/g) are subjected to confirmatory analysis by LC-MS/MS. VMY S1, a minor component of the VMY complex, is monitored but not quantified or confirmed.
Single-Laboratory Validation for the Quantification of Neomycin B and Neomycin C in Animal Feeds by Liquid Chromatography Fluorescence Detection with Post-Column Derivatization
Authors: Driver Julee Lynn , Thiex Nancy , Raynie Douglas , Ofitserova Maria , Pickering Michael 
Published: February 2020

Abstract
Amethod using ion-exchange liquid chromatographic (LC) separation, post-column derivatization, and fluorescence detection to quantify neomycin B and neomycin C in animal feeds has been developed and validated. Improved methodology is required to achieve positive identification of antibiotics present and to more accurately determine the amount of antibiotics in feeds. The method sample range covers additive levels found in type A, B, and C medicated feed products (500.005 wt/wt neomycin base). The linear range for the method covers 50150 of expected sample concentrations. Average recovery from type A and B feeds, n = 9, was 100.4 neomycin with RSD = 2.28. Average recovery from type C feeds and milk replacers, n = 9, was 97.5 neomycin with RSD = 4.36. There were no interferences from soybean meal and milk replacer matrix components, oxytetracycline, or other aminoglycosides, with the exception of one gentamicin isomer, which co-elutes with neomycin B. However, neomycin and gentamicin are not a legal feed combination, and the presence of gentamicin can easily be discerned by the appearance of the 3 gentamicin homologs that do not interfere. Comparison of the proposed LC method to the microbiological method shows that the LC method provides comparable recoveries of neomycin from feed products throughout the range of concentrations found commercially.
Colorimetric Assay of Cimetidine in the Presence of Its Oxidative Degradates
Authors: Amin Alaa S , Dessouki Hassan A , Shama Sayed A , Gouda Eslam A 
Published: February 2020

Abstract
Three simple, accurate, and sensitive colorimetric methods for the determination of cimetidine (Cim) in pure form, in dosage forms, and in the presence of its oxidative degradates were developed. These methods are indirect, involve the addition of excess oxidant N-bromosuccinimide (NBS) for method A; cerric sulfate Ce(SO4)2 for methods B and C of known concentration in acid medium to Cim, and the determination of the unreacted oxidant by measurement of the decrease in absorbance of amaranth dye for method A, chromotrope 2R for method B, and rhodamine 6G, for method C at a suitable maximum wavelength, max: 520, 528, and 525 nm, for the 3 methods, respectively. Regression analysis of the Beer plots showed good correlation in the concentration ranges of 0.24.4 g/mL for method A, and 0.23.4 g/mL for methods B and C. The apparent molar absorptivity, Sandell sensitivity, and detection and quantitation limits were evaluated. The stoichiometric ratio between the drug (Cim) and the oxidant (NBS or Ce 4) was estimated. The validity of the proposed methods was tested by analyzing pure and dosage forms containing Cim with relative standard deviation 1.18. The proposed methods could successfully determine the studied drug with varying excess of its oxidative degradation products, with recovery between 99.2 and 101.8, 100.2 and 102.8, and 99.8 and 102.0 for methods AC, respectively.
Development and Validation of a Simple Method for Routine Analysis of Ractopamine Hydrochloride in Raw Material and Feed Additives by HPLC
Authors: Freire Ellen Figueiredo , Borges Keyller Bastos , Tanimoto Hélio , Nogueira Raquel Tassara , Bertolini Lucimara Cristiane Toso , de Gaitani Cristiane Masetto 
Published: February 2020

Abstract
A simple method was optimized and validated for determination of ractopamine hydrochloride (RAC) in raw material and feed additives by HPLC for use in quality control in veterinary industries. The best-optimized conditions were a C8 column (250 4.6 mm id, 5.0 m particle size) at room temperature with acetonitrile100 mM sodium acetate buffer (pH 5.0; 75 + 25, v/v) mobile phase at a flow rate of 1.0 mL/min and UV detection at 275 nm. With these conditions, the retention time of RAC was around 5.2 min, and standard curves were linear in the concentration range of 160240 g/mL (correlation coefficient 0.999). Validation parameters, such as selectivity, linearity, limit of detection (ranged from 1.60 to 2.05 g/mL), limit of quantification (ranged from 4.26 to 6.84 g/mL), precision (relative standard deviation 1.87), accuracy (ranged from 96.97 to 100.54), and robustness, gave results within acceptable ranges. Therefore, the developed method can be successfully applied for the routine quality control analysis of raw material and feed additives.
Estimation of Catechin in Ayurvedic Oil Formulations Containing Acacia catechu
Authors: Dubey Nidhi , Dubey Nitin , Mehta Rajendra , Saluja Ajay 
Published: February 2020

Abstract
A sensitive, simple, rapid, and efficient HPTLC method was developed and validated for the analysis of catechin in marketed Ayurvedic oil formulations containing Acacia catechu. Chromatography of methanolic0.1 formic acid (7:3, v/v) extracts of these formulations was performed on silica gel 60 F254 aluminum-backed TLC plates of 0.2 mm layer thickness. The plate was developed up to 85 mm with the ternarymobile phase chloroformacetone0.1 formic acid (7.7 + 1.5 + 0.8, v/v/v) at 22 2C with 20 min of chamber saturation. The system produced compact spots of catechin at an Rf value of 0.36. The marker, catechin, was quantified at its maximum absorbance of 296 nm. The limit of detection and quantitation values were 6 and 20 ng/spot, respectively. The linear regression analysis data for the calibration plot showed a good linear relationship with a correlation coefficient of 0.9993 in the concentration range of 2001200 ng/spot for catechin with respect to peak area. Repeatability of the method was 0.88 RSD. Recovery values from 97 to 102 indicate excellent accuracy of the method. The developed HPTLC method is accurate, precise, and cost-effective, and it can be successfully applied for the determination of catechin in marketed Ayurvedic oil formulations containing Acacia catechu.
Development of a Sensitive High-Performance Liquid Chromatographic Method with Simple Extraction for Simultaneous Determination of Huperzine A and Huperzine B in the Species Containing Lycopodium Alkaloids
Authors: Zhang Yanqing , Xie Junbo , Chen Wen-Qian , Zhou Tian-Yan , Lu Wei 
Published: February 2020

Abstract
A sensitive HPLC method with simple extraction was developed for simultaneous determination of huperzine A (HupA) and huperzine B (HupB) in Huperzia serrata, H. crispata, H. miyoshiana, and Lycopodiastrum casuarinoides. In order to avoid conventional multiple-step and time-consuming sample preparation methods, direct reflux extraction with alkaline chloroform was adopted. The quantitative determination was conducted by reversed-phase HPLC with a photodiode array detector set at 308 nm. Separation was performed on a Luna C18 column (250 4.6 mm id, 5 m) with methanol0.2 aqueous acetic acid (18 + 82, v/v) mobile phase. The method was validated for accuracy, reproducibility, precision, and limits of detection and quantification. Quantification of the two active compounds in the samples was performed by this newly developed method, and the content of HupA and HupB varied substantially among four different species. The satisfactory results indicated that the developed method can readily be utilized for quality control of the species of Huperziaceae and Lycopodiaceae containing the two compounds.
Determination of Ketoconazole in Capsules by High-Performance Liquid Chromatography and Microbiological Assay
Authors: Lima Paulo Marcelo Andrade , Prado Nathália Duque , Silva Maria-Luiza Martins , Diniz Rosiane Dias Lopes , Queiroz Kelly Marques , Da Costa César Isabela , Pianetti Gérson Antônio , Santos Daniel Assis 
Published: February 2020

Abstract
The development and validation of an HPLC-UV method and a microbiological assay were performed for the analysis of ketoconazole in capsule formulations. The bioassay was developed using a specific agar diffusion technique with the strain of Candida albicans ATCC 18804 as the test organism. The effect of the mobile phase pH in the range of 2.57.5 on the retention and tailing factors of the ketoconazole peak was analyzed in the chromatography method and a pH value of 4.5 was considered to be adequate. A prospective validation of both methods showed adequate linearity (r2 &gt; 0.99 for the two methods), precision, (RSD = 2.42 for intraday and 2.69 for interday precision for bioassay; RSD = 0.74 for intraday and 0.66 for interday precision for HPLC-UV), and accuracy (mean recoveries were 103 1.0 for bioassay and 99 1.0 for HPLC-UV). Student's t-test revealed no significant difference between the results obtained by the two methods (P &lt; 0.05). The contents found for three capsule samples showed a strong correlation, as attested by Pearson's coefficient value (r = 0.9998), which also evidenced the concordance between the studied methodologies.