bluuebunny/crossref_metadata_2025_split huggingface dataset:
Development and Validation of a Reversed-Phase High-Performance Thin-Layer ChromatographyDensitometric Method for Determination of Atorvastatin Calcium in Bulk Drug and Tablets
Authors: Shirkhedkar Atul A , Surana Sanjay J 
Published: February 2020

Abstract
Atorvastatin calcium is a synthetic HMGCoA reductase inhibitor that is used as a cholesterol-lowering agent. A simple, sensitive, selective, and precise RP-HPTLCdensitometric determination of atorvastatin calcium both as bulk drug and from pharmaceutical formulation was developed and validated according to International Conference on Harmonization guidelines. The method used aluminum sheets precoated with silica gel 60 RP18F254s as the stationary phase, and the mobile phase consisted of methanolwater (3.5 + 1.5, v/v). The system gave a compact band for atorvastatin calcium with an Rf value of 0.62 0.02. Densitometric quantification was carried out at 246 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with r = 0.9992 in the working concentration range of 100-800 ng/band. The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, LOD, and LOQ. The LOD and LOQ were 6 and 18 ng, respectively. The drug underwent hydrolysis when subjected to acidic conditions and was found to be stable under alkali, oxidation, dry heat, and photodegradation conditions. Statistical analysis proved that the developed RP-HPTLCdensitometry method is reproducible and selective and that it can be applied for identification and quantitative determination of atorvastatin calcium in bulk drug and tablet formulation.
Development and Validation of an HPTLC Method for Determination of Olanzapine in Formulations
Authors: Patel Rashmin B , Patel Mrunali R , Bhatt Kashyap K , Patel Bharat G 
Published: February 2020

Abstract
A new, simple, and rapid HPTLC method was developed and validated for quantitative determination of olanzapine on silica gel 60F254 layers using methanolethyl acetate (8.0 + 2.0, v/v) as the mobile phase. Olanzapine was quantified by densitometric analysis at 285 nm. The method was found to give compact bands for the drug (Rf = 0.35 0.02). The linear regression analysis data for the calibration plots showed a good linear relationship with r2 = 0.9997 in the concentration range of 100600 ng/band. The method was validated for precision, recovery, repeatability, and robustness as per the International Conference on Harmonization guidelines. The LOD was found to be 23.90 ng/band, and the LOQ was 91.04 ng/band. Statistical analysis of the data showed that the method is precise, accurate, reproducible, and selective for the analysis of olanzapine. The method was successfully used for the determination of equilibrium solubility and quantification of olanzapine as a bulk drug, in a commercially available preparation, and in in-house developed mucoadhesive microemulsion formulations and solution.
Quantification of Phospholipids in Infant Formula and Growing Up Milk by High-Performance Liquid Chromatography with Evaporative Light Scattering Detector
Authors: Braun Marcel , Flück Brigitte , Cotting Claudia , Monard Florence , Giuffrida Francesca 
Published: February 2020

Abstract
Phospholipids (PLs) are well known for their excellent emulsifier properties and more recently for their biological functions, such as cell signing, brain development, immune function, heart health, and cancer prevention, besides their physiological role in membrane composition. In dairy products, PLs represent 0.21 of milk fat. The milk PLs comprise phosphatidylcholine (PC), phosphatidylethanolamine (PE), and sphingomyelin (SPH) as the major compounds; phosphatidylinositol and phosphatidylserine are minor PLs. A new generation of dairy products claiming PL family content, such as SPH, is being produced; therefore, a validated method for quantifying PL families in dairy products is needed. In this study, an HPLC-evaporative light scattering detector method to quantify the most abundant milk PL families, i.e., PC, PE, and SPH, in infant formula and growing up milk was developed and validated.
Sugar and Nonvolatile Acid Composition of Blackberries
Authors: Fan-Chiang Ho-Ju , Wrolstad Ronald E 
Published: February 2020

Abstract
Sugar and nonvolatile acid analyses were conducted on 52 samples of blackberries (Rubus spp), the objective being to develop a compositional database for evaluating authenticity and quality. Brix ranged from 6.88 to 16.83, with a mean of 10.82. Titratable acidity ranged from 0.52 to 2.24 g citric acid/100 mL, with a mean of 1.35. Sucrose levels (range, 012.9; mean, 4.6) were highly variable. The overall glucose:fructose ratio ranged from 0.81 to 1.17, with a mean of 1.01. Malic, isocitric, lactoisocitric, citric, shikimic, and fumaric acids were identified, with succinic acid being present in some samples. Malic acid ranged from 5.2 to 35.3 of total acids (87.5603 mg/100 g), with a mean of 16.4 (280 mg/100 g). Isocitric acid ranged from 4.7 to 71.6, with a mean of 34.7 (599 mg/100 g), and lactoisocitric acid ranged from 3.4 to 32.6 with a mean of 17.3 (293 mg/100 g). Citric acid ranged from 1.3 to 80.2, with a mean of 31.6 (572 mg/100 g). Shikimic, fumaric, and succinic were present in trace quantities. Two patterns of nonvolatile acid compositions were evident. Ten commercial blackberry juice samples were analyzed, and it was possible to determine whether they were Marion, Evergreen, or a mixture of the two from their acid profiles.
Reversed-Phase HPLC Analysis of Levetiracetam in Tablets Using Monolithic and Conventional C18 Silica Columns
Authors: Can Nafiz O , Arli Goksel 
Published: February 2020

Abstract
Development and validation of an RP-HPLC method for determination of levetiracetam in pharmaceutical tablets is described. The separation and quantification of levetiracetam and caffeine (internal standard) were performed using a single analytical procedure with two different types of stationary phases, conventional Phenomenex Gemini C18 (100 4.6 mm, 5 m) and Merck Chromolith Performance RP18e (100 4.6 mm, macropore size 2 mm, micropore size 13 nm) monolithic silica. Five-microliter aliquots of samples were injected into the system and eluted using wateracetonitrile (90 + 10, v/v) mobile phase pumped at the rate of 1 mL/min. The analyte peaks were detected at 200 nm using a diode array detector with adequate resolution. Validation studies were performed using the method recommended by the International Conference on Harmonization, the U.S. Pharmacopeia, and AOAC INTERNATIONAL, which includes accuracy, precision, range, limits, robustness, and system suitability parameters. Levetiracetam and caffeine were detected in about 7 min using the conventional column, whereas less than 5 min was required when the monolithic column was used. Calibration plots had r values close to unity in the range of 0.88.0 g/mL. Assay of levetiracetam in a tablet formulation was demonstrated as an application to real samples.
Development of an Ion-Pair Reversed-Phase HPLC Method with Indirect UV Detection for Determination of Phosphates and Phosphites as Impurities in Sodium Risedronate
Authors: Brezovska Katerina , Dimitrovska Aneta , Kitanovski Zoran , Petrusevska Jelena , Ribarska Jasmina Tonic , Jolevska Suzana Trajkovic 
Published: February 2020

Abstract
A method based on RP-HPLC with indirect UV detection was developed for the determination of phosphates and phosphites as impurities in sodium risedronate. RP separation of the phosphates and phosphites was achieved by adding tetrabutylammonium hydroxide as an ion-pairing agent in the mobile phase. Potassium hydrogen phthalate was added to the mobile phase as an ionic chromophore in order to obtain high background absorption of the mobile phase. Separation was performed on a C18 column using a mixture of pH 8.2 buffer (containing 0.5 mM tetrabutylammonium hydroxide and 1 mM phthalate) and acetonitrile (95 + 5, v/v) as the mobile phase, with indirect UV detection at 248 nm. The validation of the method included determination of specificity/selectivity, linearity, LOD, LOQ, accuracy, precision, and robustness. The LOD was 0.86 g/mL for phosphates and 0.76 g/mL for phosphites. The LOQ was 2.60 g/mL for phosphates and 2.29 g/mL for phosphites. The developed method is suitable for quantitative determination of phosphates and phosphites as impurities in QC of sodium risedronate.
Analysis of Salazinic, Norstictic, and Usnic Acids in Xanthoparmelia chlorochroa by Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry
Authors: Dailey Rebecca , Siemion Roger , Raisbeck Merl , Jesse Chris 
Published: February 2020

Abstract
The lichen species Xanthoparmelia chlorochroa is toxic when consumed by domestic sheep, cattle, and Rocky Mountain elk. Clinical signs exhibited by poisoned animals include red urine, ataxia, and muscular weakness that rapidly progresses to recumbency. Elk are unable to recover once becoming recumbent; however, most affected cattle can recover if offered suitable feed shortly following the onset of signs. At present, the pathogenesis and specific toxin(s) are unknown. As part of an effort to elucidate the proximate toxin, a method using ultra-performance LC coupled to MS/MS with negative-ion electrospray ionization has been developed to compare salazinic, norstictic, and usnic acid concentrations in X. chlorochroa collected from locales associated with lichen poisonings. Compounds were extracted from lichen samples with acetone and sonication. The stationary phase was a Waters Acquity UPLCTM BEH C18 (50 2.1 mm; 1.7 m particle size) column. The mobile phase consisted of an acetonitrilewater gradient. The precision of the method was confirmed by an SD below 0.4 (n = 9) for triplicate samples. LOD values were 200, 100, and 50 ng/mL for salazinic, norstictic, and usnic acids, respectively.
A Practical Approach for Linearity Assessment of Calibration Curves Under the International Union of Pure and Applied Chemistry (IUPAC) Guidelines for an In-House Validation of Method of Analysis
Authors: Sanagi M Marsin , Nasir Zalilah , Ling Susie Lu , Hermawan Dadan , Ibrahim Wan Aini Wan , Naim Ahmedy Abu 
Published: February 2020

Abstract
Linearity assessment as required in method validation has always been subject to different interpretations and definitions by various guidelines and protocols. However, there are very limited applicable implementation procedures that can be followed by a laboratory chemist in assessing linearity. Thus, this work proposes a simple method for linearity assessment in method validation by a regression analysis that covers experimental design, estimation of the parameters, outlier treatment, and evaluation of the assumptions according to the International Union of Pure and Applied Chemistry guidelines. The suitability of this procedure was demonstrated by its application to an in-house validation for the determination of plasticizers in plastic food packaging by GC.
Determination of Bithionol, Bromophen, Nitroxynil, Oxyclozanide, and Tribromsalan in Milk with Liquid Chromatography Coupled with Tandem Mass Spectrometry
Authors: Sakamoto Miho , Takeba Kazue , Sasamoto Takeo , Kusano Tomoko , Hayashi Hiroshi , Kanai Setsuko , Kanda Maki , Nagayama Toshihiro 
Published: February 2020

Abstract
LC/MS/MS was developed to determine the residues of bithionol (BTN), bromofen (BMF), nitroxynil (NTX), oxyclozanide (OCZ), and tribromsalan (TBS) in milk. Samples were extracted with ethyl acetate and cleaned up by liquidliquid separation with acetonitrile and n-hexane. The compounds were determined by RP-LC using a C18 column with 0.1 formic acidmethanol. Mass spectral acquisition was performed in the negative mode by applying selected-reaction monitoring. The method was validated in milk spiked with these compounds at 5600 g/kg; average recoveries were in the range 83.897.1, with RSD values of 1.48.0. The interassay RSDs were less than 11. The LODs of these compounds in milk were 0.1 g/kg. The method was applied to 24 raw milk samples. The concentration of these compounds in all samples was lower than the Japanese maximum residue limits. The method is rapid, sensitive, and specific for monitoring residues of BTN, BMF, NTX, OCZ, and TBS in milk.
Use of High-Performance Thin Layer Chromatography by the American Herbal Pharmacopoeia
Authors: Upton Roy T 
Published: February 2020

Abstract
TLC characterizations are among the key identity tests in most pharmacopoeial monographs. Pharmacopoeial standards are typically used by industry as a basis for meeting QC requirements and current good manufacturing practices (cGMPs). TLC is a relatively low-cost, highly versatile tool for developing specifications for raw materials, as well as for the various preparations for which pharmacopoeial standards are created. In addition to its use in the development of identity tests, TLC is a valuable tool for screening plant samples that pharmacopoeias must review in the development of monographs and botanical reference materials (BRMs). Specifically, HPTLC is the ideal TLC technique for these purposes because of its increased accuracy, reproducibility, and ability to document the results, compared with standard TLC. Because of this, HPTLC technologies are also the most appropriate TLC technique for conformity with GMPs. This article highlights the manner in which HPTLC is used by the American Herbal Pharmacopoeia (AHP) in the development of AHP monograph identity standards, the identification of adulterating species, and the development of AHP-verified BRMs.
Fingerprint Analysis and the Application of HPTLC to the Determination of Identity and Quality of Botanicals, from an Industry Perspective
Authors: Sudberg Sidney , Sudberg Elan M , Terrazas Jennifer , Sudberg Sandra , Patel Kirtal , Pineda Jose , Fine Bryan 
Published: February 2020

Abstract
There are many examples of botanical identity methodology currently in use today; all have associated levels of confidence and, hence, application for their intended purpose. This paper addresses the application of some of these methods to identify and qualify commonly traded herbs. The relevance of botanical identity and quality within the dietary supplement industry has seen a dramatic increase in the last several years, and now with the current Good Manufacturing Practices (cGMPs) recently published and the requirement for 100% identity testing, there is an increased need for reliable methods of analysis and subsequent interpretation of the results or data derived from these methods, given the diversity of samples and matrixes seen on a daily basis in a commercial setting. Example applications of methods described herein illustrate how one can confidently and effectively satisfy the 100% identity rule of the cGMPs to identify crude raw materials and their powdered or liquid extracts as well as identify a majority of such ingredients in finished products with diverse matrixes. The three techniques discussed in this paper are viewed from a qualitative perspective with primary emphasis on the application of HPTLC to a variety of complex samples with varying degrees of difficulty of analysis and interpretation. The three methods discussed are (1) HPTLC, for its fingerprint/pattern recognition capabilities as well as marker compound analysis; (2) microscopy, for identification/recognition of unique cellular, anatomic features and characteristics of the target plant or adulterants; and (3) HPLC for marker compound identification, quantitation, and/or other fingerprint qualities it may contribute to the data set. To support the applications and methods described herein, this paper presents four key approaches to assist in the interpretation of the data collected in order to correctly determine the identity of botanicals and their powdered extracts: the marker approach, the multicomponent-based approach, the pattern approach, and the multipattern approach, and how these approaches can be used with a vanguard/rearguard strategy in analytical testing as well as forming a basis for the functional fingerprint and the concept of phytoequivalence.
Evaluation of Culture Media for Selective Enrichment and Isolation of Salmonella in Seafood
Authors: Kumar Rakesh , Surendran Poothuvallil K , Thampuran Nirmala 
Published: February 2020

Abstract
Seafood, including fish, shrimp, clam, crab, mussel, oyster, lobster, squid, octopus, and cuttlefish samples, was used to compare the recovery of Salmonella serovars by different selective enrichment and isolation media. The samples were selectively enriched in Rappaport-Vassiliadis (RV) broth and tetrathionate broth (TT), followed by selective isolation on Hektoen enteric (HE) agar, xylose lysine desoxycholate (XLD) agar, bismuth sulfite (BS) agar, and Brilliant Green (BG) agar media. Of 443 seafood samples analyzed, 108 were found to be contaminated with Salmonella. The role of selective enrichment in Salmonella spp. recovery with RV medium was distinctly high (70%) compared to TT broth (30%). The selective enrichment in RV broth followed by selective isolation on XLD, HE, BS, and BG agar recovered Salmonella at levels of 56, 41, 28, and 16%, respectively. Similarly, after enrichment in TT broth, XLD and HE agars recovered 27 and 23 respectively. The recovery of Salmonella with enrichment in TT followed by isolation on BS and BG was abysmally low at 4.6 and 5, respectively. There was no significant difference (P &gt; 0.05) in the recovery of Salmonella using the combinations of XLD and HE media with selective enrichment in RV broth. However, performance difference (P &lt;0.05) was observed in the recovery when BS and BG with RV, and XLD, HE, BS, and BG agars with TT broth were used. The present study showed that the combination of RV with XLD was the most efficient media for isolation of Salmonella from seafood when compared to other isolation media combinations.
Rapid Determination of Banned Sudan I in Foodstuffs Using a Mesoporous SiO2 Modified Electrode
Authors: Yang Xiaofeng , He Dihua 
Published: February 2020

Abstract
Rapid determination of Sudan I in foodstuffs is very important because it was found to be a carcinogen and its use in the food industry was banned. A rapid, sensitive, and convenient electrochemical method was developed for the determination of Sudan I based on the distinctive properties of mesoporous SiO2. The electrochemical responses of Sudan I were investigated. A sensitive oxidation peak was observed for Sudan I, and the peak currents greatly increased at the mesoporous SiO2-modified electrode, which can be attributed to its large surface area and high accumulation efficiency. The effects of pH, amount of mesoporous SiO2, scan rate, accumulation potential, and time were examined on the oxidation signals of Sudan I. The linear range was from 4.00 ⨯ 108 to 2.00 ⨯ 105 M, and the LOD was 7.50 ⨯ 109 M. The newly developed method was successfully used to detect and quantify Sudan I in hot chili powder and juice samples.
Bioanalytical Methods for Food Contaminant Analysis
Authors: Van Emon Jeanette M 
Published: February 2020

Abstract
Foods are complex mixtures of lipids, carbohydrates, proteins, vitamins, organic compounds, and other naturally occurring substances. Sometimes added to this mixture are residues of pesticides, veterinary and human drugs, microbial toxins, preservatives, contaminants from food processing and packaging, and other residues. This milieu of compounds can pose difficulties in the analysis of food contaminants. There is an expanding need for rapid and cost-effective residue methods for difficult food matrixes to safeguard our food supply. Bioanalytical methods are established for many food contaminants such as mycotoxins and are the method of choice for many food allergens. Bioanalytical methods are often more cost-effective and sensitive than instrumental procedures. Recent developments in bioanalytical methods may provide more applications for their use in food analysis.
Real-Time Polymerase Chain Reaction Detection of Fishmeal in Feedstuffs
Authors: Martí Irene , García Teresa , Rojas Maria , Pegels Nicolette , Pavón Miguel ángel , Hernández Pablo E , González Isabel , Martín Rosario 
Published: February 2020

Abstract
A SYBR&lt;sup/&gt; Green PCR system was developed for detection of fishmeal in feedstuffs. The real-time PCR method combines the use of fish-specific primers that amplify an 87 base pair (bp) fragment of the mitochondrial 12S ribosomal RNA gene from fish species, and a positive control primer pair that amplifies a 99 bp fragment of the nuclear 18S ribosomal RNA gene in all eukaryotic organisms. The specificity of the primers was tested against 52 animal species and six plant species. Reference feedstuff samples were successfully tested for the presence of fishmeal, demonstrating the applicability of the assay to feedstuffs.
Quantitative Determination of Chemical Constituents from Seeds of Nigella sativa L. Using HPLC-UV and Identification by LC-ESI-TOF
Authors: Avula Bharathi , Wang Yan-Hong , Ali Zulfiqar , Khan Ikhlas A 
Published: February 2020

Abstract
An HPLC method was developed for the simultaneous determination of nine compounds of Nigella sativa L. The separation was achieved within 23 min by using C18 column material, a wateracetonitrile mobile phase, both containing 0.1 acetic acid gradient system and a temperature of 35C. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of nine compounds were in the range of 0.0910 and 0.325 g/mL, respectively. The wavelength used for quantification with the diode array detector was 205 and 260 nm. LC/MS coupled with electrospray ionization interface method is described for the identification of compounds in N. sativa L. samples. This method involved the use of [MH]&lt;sup/&gt; and [MNa]&lt;sup/&gt; ions in the positive ion mode with extracted ion chromatogram.
Ultra-Fast Gradient LC Method for Omeprazole Analysis Using a Monolithic Column: Assay Development, Validation, and Application to the Quality Control of Omeprazole Enteric-Coated Pellets
Authors: Borges Keyller Bastos , Snchez Antonio Jos Macas , Pupo Mnica Tallarico , Bonato Pierina Sueli , Collado Isidro Gonzlez 
Published: February 2020

Abstract
A method was optimized for the analysis of omeprazole (OMZ) by ultra-high speed LC with diode array detection using a monolithic Chromolith Fast Gradient RP 18 endcapped column (50 2.0 mm id). The analyses were performed at 30C using a mobile phase consisting of 0.15 (v/v) trifluoroacetic acid (TFA) in water (solvent A) and 0.15 (v/v) TFA in acetonitrile (solvent B) under a linear gradient of 5 to 90 B in 1 min at a flow rate of 1.0 mL/min and detection at 220 nm. Under these conditions, OMZ retention time was approximately 0.74 min. Validation parameters, such as selectivity, linearity, precision, accuracy, and robustness, showed results within the acceptable criteria. The method developed was successfully applied to OMZ enteric-coated pellets, showing that this assay can be used in the pharmaceutical industry for routine QC analysis. Moreover, the analytical conditions established allow for the simultaneous analysis of OMZ metabolites, 5-hydroxyomeprazole and omeprazole sulfone, in the same run, showing that this method can be extended to other matrixes with adequate procedures for sample preparation.