{"title":"Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges.","authors":"Nidal Batrawi, Shorouq Wahdan, Murad Abualhasan","doi":"10.1177/1177390117690152","DOIUrl":"https://doi.org/10.1177/1177390117690152","url":null,"abstract":"<p><p>Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH) guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL (<i>R</i><sup>2</sup> > 0.999). The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form.</p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"12 ","pages":"1177390117690152"},"PeriodicalIF":0.0,"publicationDate":"2017-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1177/1177390117690152","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34966271","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Insight into Biochemical Characterization of Plant Sesquiterpene Synthases","authors":"Tom Manczak, H. T. Simonsen","doi":"10.4137/ACI.S40292","DOIUrl":"https://doi.org/10.4137/ACI.S40292","url":null,"abstract":"A fast and reproducible protocol was established for enzymatic characterization of plant sesquiterpene synthases that can incorporate radioactivity in their products. The method utilizes the 96-well format in conjunction with cluster tubes and enables processing of >200 samples a day. Along with reduced reagent usage, it allows further reduction in the use of radioactive isotopes and flammable organic solvents. The sesquiterpene synthases previously characterized were expressed in yeast, and the plant-derived Thapsia garganica kunzeaol synthase TgTPS2 was tested in this method. KM for TgTPS2 was found to be 0.55 μM; the turnover number, kcat, was found to be 0.29 s−1, kcat for TgTPS2 is in agreement with that of terpene synthases of other plants, and kcat/KM was found to be 0.53 s−1 μM−1 for TgTPS2. The kinetic parameters were in agreement with previously published data.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"22 1","pages":"1 - 7"},"PeriodicalIF":0.0,"publicationDate":"2016-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81794701","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
F. Ghamari, A. Bahrami, Y. Yamini, F. G. Shahna, A. Moghimbeigi
{"title":"Development of Hollow-Fiber Liquid-Phase Microextraction Method for Determination of Urinary trans,trans-Muconic Acid as a Biomarker of Benzene Exposure","authors":"F. Ghamari, A. Bahrami, Y. Yamini, F. G. Shahna, A. Moghimbeigi","doi":"10.4137/ACI.S40177","DOIUrl":"https://doi.org/10.4137/ACI.S40177","url":null,"abstract":"For the first time, hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography–ultraviolet was used to extract trans,trans-muconic acid, in urine samples of workers who had been exposed to benzene. The parameters affecting the metabolite extraction were optimized as follows: the volume of sample solution was 11 mL with pH 2, liquid membrane containing dihexyl ether as the supporter, 15% (w/v) of trioctylphosphine oxide as the carrier, the time of extraction was 120 minutes, and stirring rate was 500 rpm. Organic phase impregnated in the pores of a hollow fiber was extracted into 24 µL solution of 0.05 mol L−1 Na2CO3 located inside the lumen of the fiber. Under optimized conditions, a high enrichment factor of 153–182 folds, relative recovery of 83%–92%, and detection limit of 0.001 µg mL−1 were obtained. The method was successfully applied to the analysis of ttMA in real urine samples.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"13 1","pages":"65 - 71"},"PeriodicalIF":0.0,"publicationDate":"2016-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80439299","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A. Haidar, S. Kabiche, E. Majoul, I. Balde, J. Fontan, S. Cisternino, J. Schlatter
{"title":"Stability-Indicating High-Performance Liquid Chromatography Assay for the Determination of Sulthiame in Pharmaceutical Dosage Forms","authors":"A. Haidar, S. Kabiche, E. Majoul, I. Balde, J. Fontan, S. Cisternino, J. Schlatter","doi":"10.4137/ACI.S38656","DOIUrl":"https://doi.org/10.4137/ACI.S38656","url":null,"abstract":"A stability-indicating assay by reversed-phase high performance liquid chromatography method was developed and validated for the determination of sulthiame (STM). The chromatographic separation was achieved on a reversed-phase NovaPack C18 column and an isocratic mobile phase consisting of deionized water:methanol (70:30, v/v). The flow rate was 1.0 mL/min (ultraviolet detection at 210 nm). The STM was separated within 2.83 min. The linearity of the method was demonstrated in the range of 20.0–200.0 μg/mL and a coefficient of determination of r2 = 0.9999. The limits of detection and quantification were 4.2 and 9.5 μg/mL, respectively. The intraday and interday precisions were less than 1%. Accuracy of the method ranged from 98.3% to 101.7%, with a relative standard deviation of <1%. STM was degraded by accelerated breakdown in alkaline, acidic, or oxidative stress conditions. This method allows accurate and reliable determination of STM for drug stability assay in pharmaceutical studies.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"11 1","pages":"59 - 64"},"PeriodicalIF":0.0,"publicationDate":"2016-09-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87454391","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Thibaut Istasse, Nicolas Jacquet, Thomas Berchem, Eric Haubruge, Bach Kim Nguyen, Aurore Richel
{"title":"Extraction of Honey Polyphenols: Method Development and Evidence of Cis Isomerization.","authors":"Thibaut Istasse, Nicolas Jacquet, Thomas Berchem, Eric Haubruge, Bach Kim Nguyen, Aurore Richel","doi":"10.4137/ACI.S39739","DOIUrl":"https://doi.org/10.4137/ACI.S39739","url":null,"abstract":"<p><p>Honey polyphenols have been studied with the objective of relating honeys to their floral sources. Initially synthesized by plant, these polyphenols can be found in the plant's nectar, which are collected by bees, which convert the nectar into honey. Consequently, polyphenols constitute minor components of honey. The development of a solid-phase extraction method for honey polyphenols is presented in this study. The technique employs Amberlite XAD-2 adsorbent and was tested on monofloral honeys from six different plants: acacia, chestnut, eucalyptus, thyme, sunflower, and wild carrot. Analyses were performed using high-performance liquid chromatography coupled with UV detection and mass spectrometry. Several phenolic acids and flavonoids were identified: caffeic and p-coumaric acids, quercetin, kaempferol, naringenin, chrysin, and pinocembrin. Generally, the quantity of a given polyphenol in the honey was around 0.2 mg/100 g of honey, except for chestnut honey, which contained around 3.0 mg of p-coumaric acid/100 g of honey. Analyses highlighted significant formation of cis isomers for phenolic acids during the extraction despite protection from light. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"11 ","pages":"49-57"},"PeriodicalIF":0.0,"publicationDate":"2016-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4137/ACI.S39739","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34324497","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Tonu Reinot, Jinhai Chen, Adam Kell, Mahboobe Jassas, Kevin C Robben, Valter Zazubovich, Ryszard Jankowiak
{"title":"On the Conflicting Estimations of Pigment Site Energies in Photosynthetic Complexes: A Case Study of the CP47 Complex.","authors":"Tonu Reinot, Jinhai Chen, Adam Kell, Mahboobe Jassas, Kevin C Robben, Valter Zazubovich, Ryszard Jankowiak","doi":"10.4137/ACI.S32151","DOIUrl":"https://doi.org/10.4137/ACI.S32151","url":null,"abstract":"<p><p>We focus on problems with elucidation of site energies [Formula: see text] for photosynthetic complexes (PSCs) in order to raise some genuine concern regarding the conflicting estimations propagating in the literature. As an example, we provide a stern assessment of the site energies extracted from fits to optical spectra of the widely studied CP47 antenna complex of photosystem II from spinach, though many general comments apply to other PSCs as well. Correct values of [Formula: see text] for chlorophyll (Chl) a in CP47 are essential for understanding its excitonic structure, population dynamics, and excitation energy pathway(s). To demonstrate this, we present a case study where simultaneous fits of multiple spectra (absorption, emission, circular dichroism, and nonresonant hole-burned spectra) show that several sets of parameters can fit the spectra very well. Importantly, we show that variable emission maxima (690-695 nm) and sample-dependent bleaching in nonresonant hole-burning spectra reported in literature could be explained, assuming that many previously studied CP47 samples were a mixture of intact and destabilized proteins. It appears that the destabilized subpopulation of CP47 complexes could feature a weakened hydrogen bond between the 13(1)-keto group of Chl29 and the PsbH protein subunit, though other possibilities cannot be entirely excluded, as discussed in this work. Possible implications of our findings are briefly discussed. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"11 ","pages":"35-48"},"PeriodicalIF":0.0,"publicationDate":"2016-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4137/ACI.S32151","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34452744","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Removal of 4-Nitrophenol from Water Using Ag-N-P-Tridoped TiO2 by Photocatalytic Oxidation Technique.","authors":"Temesgen Achamo, O P Yadav","doi":"10.4137/ACI.S31508","DOIUrl":"https://doi.org/10.4137/ACI.S31508","url":null,"abstract":"<p><p>Photocatalytic oxidation using semiconductor nanoparticles is an efficient, eco-friendly, and cost-effective process for the removal of organic pollutants, such as dyes, pesticides, phenols, and their derivatives in water. In the present study, nanosize Ag-N-P-tridoped titanium(IV) oxide (TiO2) was prepared by using sol-gel-synthesized Ag-doped TiO2 and soybean (Glycine max) or chickpea (Cicer arietinum) seeds as nonmetallic bioprecursors. As-synthesized photocatalysts were characterized using X-ray diffraction, Fourier transform infrared, and ultra violet (UV)-visible spectroscopic techniques. Average crystallite size of the studied photocatalysts was within 39-46 nm. Whereas doped Ag in TiO2 minimized the photogenerated electron-hole recombination, doped N and P extended its photoabsorption edge to visible region. Tridoping of Ag, N, and P in TiO2 exhibited synergetic effect toward enhancing its photocatalytic degradation of 4-nitrophenol (4-NP), separately, under UV and visible irradiations. At three hours, degradations of 4-NP over Ag-N-P-tridoped TiO2 under UV and visible radiations were 73.8 and 98.1%, respectively. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"11 ","pages":"29-34"},"PeriodicalIF":0.0,"publicationDate":"2016-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4137/ACI.S31508","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34404738","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Development and Validation of Stability-Indicating RP-HPLC Method for Simultaneous Determination of Metformin HCl and Glimepiride in Fixed-Dose Combination","authors":"Pradnya N. Vaingankar, P. Amin","doi":"10.4137/ACI.S38137","DOIUrl":"https://doi.org/10.4137/ACI.S38137","url":null,"abstract":"A simple reversed-phase high-performance liquid chromatography method was developed and validated for simultaneous determination of Metformin hydrochloride (MET) and Glimepiride (GLM) in combination and estimation of their principal degradation products. The separation was achieved using JASCO Finepak SIL (250 mm × 4.6 mm i.d. 5 μm) at ambient temperature. The optimized mobile phase composed of an aqueous phase (20 mM phosphate buffer, adjusted to pH 3.0) and an organic phase (methanol:acetonitrile; 62.5:37.5) in the ratio of 80:20. The flow rate was 1 mL/minute, and the analytes were detected at 230 nm. The developed method was validated for accuracy, precision, specificity, linearity, and sensitivity. The chromatographic analysis time was approximately six minutes with the complete resolution of MET (Rt = 2.75 minutes) and GLM (Rt = 5.87 minutes). The method exhibited good linearity over the range of 5–30 μg/mL for MET and 1–10 μg/mL for GLM. The drugs in combination were subjected to various stress degradation studies as per the International Conference Harmonization (ICH) guidelines. Results obtained from the stress degradation studies revealed that the developed method is applicable for stability studies.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"107 1","pages":"13 - 20"},"PeriodicalIF":0.0,"publicationDate":"2016-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77441406","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Electrochemical Behavior and Voltammetric Determination of a Manganese(II) Complex at a Carbon Paste Electrode","authors":"Sophia Karastogianni, S. Girousi","doi":"10.4137/ACI.S32150","DOIUrl":"https://doi.org/10.4137/ACI.S32150","url":null,"abstract":"Investigation of the electrochemical behavior using cyclic voltammetry and detection of [Mn2+(thiophenyl-2-carboxylic acid)2 (triethanolamine)] with adsorptive stripping differential pulse voltammetry. The electrochemical behavior of a manganese(II) complex [Mn2+(thiophenyl-2-carboxylic acid)2(triethanolamine)] (A) was investigated using cyclic and differential pulse voltammetry in an acetate buffer of pH 4.6 at a carbon paste electrode. Further, an oxidation–reduction mechanism was proposed. Meanwhile, an adsorptive stripping differential pulse voltammetric method was developed for the determination of manganese(II) complex.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"6 1","pages":"1 - 11"},"PeriodicalIF":0.0,"publicationDate":"2016-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89746139","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Sample Preparation of Eggs From Laying Hens Using QuEChERS Dispersive Extraction for the Simultaneous Determination of Melamine and Cyromazine Residues by HPLC-DAD","authors":"Niki Tsartsali, V. Samanidou","doi":"10.4137/ACI.S31727","DOIUrl":"https://doi.org/10.4137/ACI.S31727","url":null,"abstract":"A quick, easy, cheap, effective, rugged, and safe (QuEChERS) dispersive extraction method is proposed herein for the isolation and cleanup of melamine and cyromazine from chicken egg yolk. Analytes are determined by high-performance liquid chromatography using photodiode array detector after separation on a LiChroCART® (250 × 4 mm)—LiChrospher® RP-8e, 5 μm analytical column using a mobile phase of 0.1% trifluoracetic acid and methanol (80:20 v/v) delivered isocratically at a flow rate of 1 mL/minute. Extraction of isolated compounds was achieved by methanol and acetonitrile mixture (1:1 v/v). Recovery rates ranged between 74.5% and 115.8%. The method was validated in terms of 657/2002/EC decision. The within-laboratory reproducibility, expressed as a relative standard deviation, was <11%. Decision limits (CCalfa) were 2.56 mg/kg for melamine and 0.22 mg/kg−1 for cyromazine, and the corresponding results for detection capability (CCbeta) were 2.8 mg/kg for melamine and 0.24 mg/kg for cyromazine. Ruggedness was estimated according to the Youden approach studying egg yolk mass, sorbent mass, centrifugation time, organic solvents volume, evaporation temperature, and vortex time.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":"24 1","pages":"53 - 58"},"PeriodicalIF":0.0,"publicationDate":"2015-12-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72636809","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}