Mehdi Ashraf-Khorassani, Thomas A Perfetti, Mike F Dube, William M Coleman, John M Ferraro, Weston J Umstead
{"title":"Qualitative and Quantitative Analyses of the Enantiomers of Nicotine and Nornicotine Employing Chiral Supercritical Fluid Chromatography.","authors":"Mehdi Ashraf-Khorassani, Thomas A Perfetti, Mike F Dube, William M Coleman, John M Ferraro, Weston J Umstead","doi":"10.1093/chromsci/bmad048","DOIUrl":"10.1093/chromsci/bmad048","url":null,"abstract":"<p><p>An optimized method employing chiral supercritical fluid chromatography with diode array UV-VIS detection has been developed for the quantitative analysis of nicotine and nornicotine enantiomer distributions. The method parameters that were optimized included: column type (stationary phases, Chiralpak IG-3), column temperature (40°C), modifier types and concentration (isopropyl alcohol, 10%), additive types and concentrations (diethylamine, 0.2%), elution times (<6 min, flow rate 3 mL/min) and resolution factor (>1.2). These optimized conditions led to nicotine and nornicotine enantiomer detection limits of ~5 ng/μL with accompanying %RSD values of <2% from the analyses of commercially available nicotine-containing formulations.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"492-497"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9834328","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Effect of Vinegar on the Oxidative Stability of Mayonnaise During its Storage.","authors":"Afraa Alnokkari","doi":"10.1093/chromsci/bmad036","DOIUrl":"10.1093/chromsci/bmad036","url":null,"abstract":"<p><p>Mayonnaise is an emulsion of oil that is susceptible to lipid oxidation, which can cause spoilage and the formation of harmful compounds. This study aims to evaluate the impact of Syrian apple and grape vinegar on the oxidative stability of mayonnaise and compare the use of natural antioxidants to synthetic ones such as butylated hydroxyanisole and butylated hydroxytoluene. The study measured total phenol content, radical scavenging activity, and identified some phenolic compounds by High Performance Liquid Chromatography (HPLC). The rancidity of mayonnaise was examined using peroxide value and thiobarbituric acid number. The fatty acids content in the mayonnaise samples was examined using gas chromatography. Vinegar samples containing high concentrations of phenolic antioxidants showed high ability to scavenge free radicals. The antioxidants in vinegar protected the mayonnaise samples from primary and secondary oxidation, and there was no statistically significant difference between the ratio of unsaturated fatty acids in the samples containing vinegar at the beginning and at the end of the storage period. The study shows the significance of using vinegar to protect mayonnaise from deterioration and increase its shelf life, in addition to its role as a dressing.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"406-413"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9871967","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Zixu Wang, Yue Liu, Guoqing Sun, Liu Yang, Shuai Huang, Lin Chen, Xianli Zhou
{"title":"A Simple and Rapid High-Performance Liquid Chromatography Method for Preparation and Content Detection of the Mainly Numbing Taste Substances of Zanthoxylum bungeanum Maxim.","authors":"Zixu Wang, Yue Liu, Guoqing Sun, Liu Yang, Shuai Huang, Lin Chen, Xianli Zhou","doi":"10.1093/chromsci/bmad087","DOIUrl":"10.1093/chromsci/bmad087","url":null,"abstract":"<p><p>As the characteristic numbing taste substances, hydroxyl-α-sanshool (HAS) and hydroxyl-β-sanshool (HBS) were considered vital indicators to evaluate the quality of Zanthoxylum bungeanum Maxim. However, it is very difficult to obtain their high-purity monomers individually, as the only difference between HAS and HBS is that C-6 cis-trans isomerism. In our study, a simple and rapid Ag +-HPLC method was developed to pure the standard chemicals of Z. bungeanum with numbing taste, and 1H NMR and 13C NMR were employed to determine the purity and structure. Moreover, an HPLC method was established to determine the content of numbing taste components of 16 varieties of Z. bungeanum from different regions. The analytical methods were validated for accuracy, precision, and linearity, respectively. The validated method was accurate (spiked recoveries 0.94-1.10), precise in terms of peak area (intra-day RSDs <1.25% and inter-day RSDs <1.61%), and linear (r2 ≥ 0.999). It was found that there were significant differences in the content of HAS and HBS among different types of Z. bungeanum, with HAS content ranging from 60.06 ± 1.14 to 164.13 ± 3.28 mg/g and HBS ranging from 7.81 ± 0.36 to 21.11 ± 0.75 mg/g. The RSDs of HAS range were 1.73-3.80% and that of HBS range 2.03-4.73% (RSDs ≤5%), which indicated that the measurements of HAS and HBS were reliable.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"426-431"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136397610","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chandni Chandarana, Heli Desai, Ayushi Chauhan, Vijaykumar Parmar, Parixit Prajapati
{"title":"Development and Validation of Chromatographic Methods for Simultaneous Estimation of Aspirin and Pantoprazole Sodium in Pure and Mixture Form.","authors":"Chandni Chandarana, Heli Desai, Ayushi Chauhan, Vijaykumar Parmar, Parixit Prajapati","doi":"10.1093/chromsci/bmae012","DOIUrl":"10.1093/chromsci/bmae012","url":null,"abstract":"<p><p>This technique is employed for the simultaneous quantification of aspirin (ASP) and pantoprazole sodium in both pure powder form and formulations. The high performance liquid chromatography (HPLC) method uses a C-18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase consisting of 0.05 M disodium hydrogen phosphate and methanol in a 40:60% v/v ratio. The flow rate is maintained at 1.0 mL/min. On a layer of silica gel 60F254 with an aluminum backing, the high performance thin layer chromatography (HPTLC) separation was carried out with ethyl acetate and methanol (8: 1.5 v/v) as the mobile phase. With a mean recovery of 100.54% and 99.55% for ASP and PNT, respectively, quantification was accomplished using the HPLC method with UV detection at 286 nm over the concentration range of 0.1-0.6 g/mL for PNT and 0.4-2.4 g/mL for ASP. With a mean recovery of 99.44% and 99.01% for ASP and PNT, respectively, quantification was achieved using the HPTLC method with UV detection at 298 nm over the concentration range of 400-2400 ng/spot for ASP and 100-600 ng/spot for PNT, respectively. The methods can be used for the simultaneous determination of ASP and PNT in pure powder form and formulations as they are simple, accurate and sensitive.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"477-482"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140326634","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Novel Validated GC-MS/MS Method for the Estimation of N-Nitroso Dimethyl Amine and N-Nitroso Diethyl Amine in Zidovudine.","authors":"Narayanareddy Papadasu, Ramakrishnareddy Kotanka, Raghuram Pannala","doi":"10.1093/chromsci/bmae008","DOIUrl":"10.1093/chromsci/bmae008","url":null,"abstract":"<p><p>A novel method has been developed for the estimation of N-Nitroso dimethyl amine impurities (NDMA) and N-Nitroso diethyl amine (NDEA) in Zidovudine by using Gas chromatograph Triple Quadrupole Mass with Liquid autosampler (GC-MS/MS) and the method is validated as per International Conference on Harmonization recommendations. Sample analysis was executed for Zidovudine by developed method. Both NDMA and NDEA were detected in below quantitation limit for the Zidovudine batches. Efficient chromatographic separation was achieved on a DB-WAX 30 m length × 0.25 mm internal diameter, 0.5-μm film thickness, Triple quad-8040 GC-MS/MS. Quantification was carried out at Triple quad electron ionization source was at a column flow of 1.5 mL/min at a column oven temperature 50°C. The precision was in the range of 0.9-2.5% for NDMA and 0.8-2.3% for NDEA, and regression analysis shows as r value (correlation coefficient) of is >0.99. This method is capable to detect the NDMA and NDEA impurities in Zidovudine at a level of 0.006 ppm for limit of detection and 0.018 ppm for limit of quantitation with respect to test concentration of 66.66 mg/mL.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"399-405"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140193920","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"An Eco-Friendly RP-HPLC Method Development and Validation for Quantification of Favipiravir in Bulk and Tablet Dosage Form Followed by Forced Degradation Study.","authors":"Monika B Sangani, Nirav Patel","doi":"10.1093/chromsci/bmad093","DOIUrl":"10.1093/chromsci/bmad093","url":null,"abstract":"<p><p>In this work, an eco-friendly simple, precise reverse phase high-performance liquid chromatography (HPLC) method has been developed and validated for Favipiravir in bulk and tablet dosage form followed by its force degradation study. The proposed method was validated to obtain official requirements including stability, accuracy, precision, linearity, robustness and selectivity as per International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Guidelines. The estimation was developed on C (18) column reversed-phase using the mobile phase composition as methanol:water (10:90 v/v). The flow rate was set as 1 ml/min, and the maximum absorption was observed at 323 nm using Shimadzu Photo Diode Array detector. The Favipiravir, drug showed a precise and good linearity at the concentration ranges of 10-50 μg/mL. The Revearse Phase High Perforance Liquid Chromatography assay showed the highest purity ranging from 99.90 to 100.02% for Favipiravir, tablet dosage form, and 100.15% was the mean percentage purity. The percent recovery was found within the acceptance limit of (98.6-100.0%). Intra- and inter-day precision studies of the method were less than the maximum allowable limit percentage of relative standard deviation ≤ 2.0. The Favipiravir retention time was found to be 5.00 min. To examine the stability of the drug, various forced degradation studies were conducted on Favipiravir Active Pharmaceutical Ingredient. The developed method was validated according to the ICH guidelines. A very quick, cost-effective, precise and accurate HPLC method for the determination of Favipiravir has been developed and validated in compliance with ICH guidance Q2.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"432-438"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139544735","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
DasameswaraRao Kavitapu, Nagadeep Jaishetty, Arthanareeswari Maruthapillai, J N S R C Murty
{"title":"Identification of Two Novel Hydroperoxide Impurities in Fluocinolone Acetonide Topical Solution by Liquid Chromatography Mass Spectrometry.","authors":"DasameswaraRao Kavitapu, Nagadeep Jaishetty, Arthanareeswari Maruthapillai, J N S R C Murty","doi":"10.1093/chromsci/bmad003","DOIUrl":"10.1093/chromsci/bmad003","url":null,"abstract":"<p><p>Fluocinolone acetonide topical is used to treat skin discomforts such as swelling, itching and redness by activating the natural substances in the skin. Several process-related impurities and degradation products are identified and reported. But hydroperoxide impurities in Fluocinolone acetonide topical solution are not reported anywhere. In this study, we identify two potential genotoxic isomeric hydroperoxide impurities in Fluocinolone acetonide topical solution by Liquid Chromatography Mass Spectrometry analysis. A possible mechanism for the formation of these two novel hydroperoxide impurities is based on the neighboring group participation effect of adjacent hydroxyl group (Internal SN2) which results in the loss of fluorine atom and formation of epoxide intermediate followed by the addition of the HOOH group. Since most of the hydroperoxide impurities are genotoxic in nature, one should eliminate these impurities from Active Pharmaceutical Ingredient (API) or protect the formulation product from these oxidative impurities.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"414-425"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9104846","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Robust HPLC Method for Easily Oxidizable Phosphine Ligand Analysis.","authors":"Lauren Weisel, Liam Corcoran, Steve Castro, Yu He","doi":"10.1093/chromsci/bmad008","DOIUrl":"10.1093/chromsci/bmad008","url":null,"abstract":"<p><p>Phosphine ligands are widely used in the manufacture of small molecule active pharmaceutical ingredients, for they play a key role in transition-metal-catalyzed cross-coupling. However, chromatographic analysis of phosphine ligands can be challenging because of the easily oxidizable nature of this class of compounds. This manuscript describes an out-of-specification (OOS) investigation study of XPhos raw material analysis by high performance liquid chromatography (LC). It is concluded that on-column degradation/oxidation is the culprit behind this OOS result. In addition, a slightly modified yet much improved new LC method is developed by adding a trace amount of tris(2-carboxyethyl)phosphine (TCEP) into the aqueous mobile phase. TCEP is also a phosphine compound and is commonly used as a reducing reagent in molecular biology. The trace amount of TCEP serves as a surrogate reagent to passivate the LC column and eliminate the on-column degradation/oxidation. As a result, a much more robust performance is achieved with greatly improved method precision and sensitivity. This is a general approach and can be applied to the LC analysis of many other phosphine ligands in the same manner.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"471-476"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10761288","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pintu B Prajapati, Bhavesh M Sheta, Veerashakar Pulusu, Shailesh A Shah
{"title":"Analytical Quality Risk Assessment and Design of Experiments to Green HPTLC Method for Simultaneous Estimation of Sildenafil Citrate and Dapoxetine Hydrochloride.","authors":"Pintu B Prajapati, Bhavesh M Sheta, Veerashakar Pulusu, Shailesh A Shah","doi":"10.1093/chromsci/bmad057","DOIUrl":"10.1093/chromsci/bmad057","url":null,"abstract":"<p><p>A green and robust high-performance thin-layer chromatographic method has been developed for the simultaneous estimation of sildenafil citrate and dapoxetine hydrochloride. A fractional factorial design was applied for analytical quality risk assessment of potential analytical risk factors. The identified critical analytical risk factors were optimized using the design of experiment-based response surface analysis by full factorial design. The analytical design space was navigated for the optimization of the method and the control strategy was framed for low-risk life-cycle management of the chromatographic method. The chromatographic analysis of sildenafil and dapoxetine was carried out on a TLC plate coated with silica gel G60 F254 using n-butanol:ethyl acetate:ethanol (8.0 + 2.0 + 0.5, v/v) as mobile phase. The chromatographic peaks of sildenafil and dapoxetine were found to be at Rf 0.29 and 0.69, respectively. The method was found to be accurate, precise, robust, specific and sensitive. The fixed-dose combinations of sildenafil and dapoxetine were assayed and results were found in compliance with their labeled claim. The present method was developed using safe and eco-friendly organic solvents for the safety of analysts and the protection of the environment. The greenness profiles of developed and reported methods were evaluated using the NEMI scale and AGREE software.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"454-464"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9929909","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hong-Na Li, Tao Wang, Zhao-di Kang, Yan-Ge Yang, Tao Li, Fei Yuan
{"title":"Determination of Whole Molecular of Thermostable Direct Hemolysins in Milk Powder by HPLC-ESI-TOF.","authors":"Hong-Na Li, Tao Wang, Zhao-di Kang, Yan-Ge Yang, Tao Li, Fei Yuan","doi":"10.1093/chromsci/bmad094","DOIUrl":"10.1093/chromsci/bmad094","url":null,"abstract":"<p><p>Although Vibrio parahaemolyticus (V. parahaemolyticus) is a pathogen frequently found in seafood, there is a possibility of its presence in other foods, such as dairy products. The main virulence factors of V. parahaemolyticus are thermostable direct hemolysins (TDHs) which are lethal toxins, so it is necessary to establish qualitative and quantitative methods for determining TDHs. HPLC-ESI-TOF was employed to establish a method for identifying TDHs. The identification and quantification ions of TDHs were confirmed by HPLC-ESI-TOF. The method was developed for detecting TDHs in milk powder using HPLC-ESI-TOF in this paper, and limits of detection (were between 0.20 and 0.40 mg/kg, limits of quantitation were between 0.5 and 1.0 mg/kg and recoveries of all TDHs were between from 78% to 94% with relative standard deviation lower than 10%. This research will provide a reference for developing methods of HPLC-MS/MS to detect TDHs in food samples, which can provide a tool for the government to monitor TDHs contamination in foods.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"465-470"},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139424864","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}