{"title":"Hydrophilic molecularly imprinted chitosan microspheres based on deep eutectic solvents for micro-solid phase extraction of catechin","authors":"Mengdi Yuan, Chenglin Zhong, K. Row, Guizhen Li","doi":"10.1080/10826076.2023.2208201","DOIUrl":"https://doi.org/10.1080/10826076.2023.2208201","url":null,"abstract":"Abstract Hydrophilic molecularly imprinted chitosan microspheres (HMICS) were synthesized using deep eutectic solvents (DESs)-(3-aminopropyl) triethoxysilane (APTES) as co-functional monomer for the extraction of catechin from green tea with micro-solid phase extraction (micro-SPE). Various factors were studied to optimize the extraction condition during extraction process. The actual extraction amount under the optimal conditions (amount of adsorbent (20 mg), type and volume of washing (acetone, 1.2 mL) and eluting solvent (acetone/acetic acid, 1.0 mL), extraction time (30 min), extraction temperature (40 °C), and sample pH (4)) were obtained at 97.06 mg·g−1. The catechin recovery ranged with ranged with limit of detection (LOD) within 0.09–0.24 µg·mL−1, and limit of quantification (LOQ) within 0.18–0.28 µg·mL−1. From the experimental results in this system, the HMICS was proved to have higher extraction capacity, improving as a promising adsorbent for the extraction of catechin. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"46 1","pages":"48 - 55"},"PeriodicalIF":1.3,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41786708","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}
Xiaofeng Wang, Jing Wang, Guligena Sawuer, Min Jiang, Xueqin Zhai, Hui Fan, Yaonan Du, Pengcheng Zhu
{"title":"Metabonomics comparison of coronary heart disease with and without turbid phlegm syndrome","authors":"Xiaofeng Wang, Jing Wang, Guligena Sawuer, Min Jiang, Xueqin Zhai, Hui Fan, Yaonan Du, Pengcheng Zhu","doi":"10.1080/10826076.2023.2216771","DOIUrl":"https://doi.org/10.1080/10826076.2023.2216771","url":null,"abstract":"Abstract Objectives To help understand the pathogenesis of coronary heart disease (CHD) by doing blood metabonomics comparison on CHD patients with phlegm-turbidity syndrome and without syndrome, and healthy controls. Methods Ninety patients were involved. Among them, 60 patients with CHD were divided into the coronary heart disease with turbid phlegm syndrome group (HZTZ) and the coronary heart disease without turbid phlegm syndrome group (NHZTZ). The additional 30 subjects were the healthy controls (JKZ). The serum endogenous metabolites were determined and analyzed by Liquid chromatography—Mass spectrometry (LC-MS). Results In positive ion mode, there were three identical differential metabolites among the three groups: N2-ethyl-n4-isopropyl-6-(methylthio)-1,3,5-triazine-2,4-diamine, LysoPC (18:2), and methyl palmitate. In negative ion mode, two identical metabolites were identified, which were LysoPC (17:0) and fatty acyl ester of hydroxy fatty acids (FAHFA) (17:1/14:1). These five metabolites of the HZTZ group were higher than those in NHZTZ group and healthy controls. The results identified perturbations in the areas, such as phenylalanine, tyrosine, and tryptophan biosynthesis, starch and sucrose metabolism, carbohydrate digestion and absorption, and so on. Conclusions Metabonomics analysis of serum in patients with CHD with turbid phlegm syndrome uncovered the metabolic disorders of saturated and unsaturated fatty acids in comparison to the patients without turbid phlegm syndrome. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"46 1","pages":"67 - 78"},"PeriodicalIF":1.3,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48631173","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}
Paula de Oliveira Moretto, Graciela Carlos, F. S. Barbosa, C. V. Garcia, Tiago Franco de Oliveira, A. Mendez
{"title":"Simultaneous monitoring of ceftaroline fosamil and its active form ceftaroline during stability study of commercial sample - a new stability-indicating HPLC method, drug decomposition in clinical use conditions and degradation products by LC-MS","authors":"Paula de Oliveira Moretto, Graciela Carlos, F. S. Barbosa, C. V. Garcia, Tiago Franco de Oliveira, A. Mendez","doi":"10.1080/10826076.2023.2216750","DOIUrl":"https://doi.org/10.1080/10826076.2023.2216750","url":null,"abstract":"Abstract Ceftaroline fosamil (prodrug) and ceftaroline (active form; degradation product) were simultaneously determined by a new stability-indicating HPLC method. These two forms were monitored during stability investigation of drug formulation reconstituted solution following the same conditions used for clinical use (refrigeration and room temperature). In general terms, ceftaroline fosamil is stable when stored at refrigerator until 48 h, with a drug residual content of 93.99% (in saline diluent) and 97.18% (in 5% glucose diluent). At room temperature, its chemical stability is critical, being necessary attention in the time infusion. Ceftaroline free basis was formed during stability testing, and its concentration has increased along the time. A forced degradation study was also performed for evaluation of the main degradation products, which were identified by LC-MS analysis. Applying selected stress conditions, five degradation products were structurally identified, with variation on side chain and cephalosporinic ring. The opened β-lactam ring and ceftaroline free basis can be highlighted. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"46 1","pages":"56 - 66"},"PeriodicalIF":1.3,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49254987","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}
Marco M. Z. Sharkawi, Mark T. Safwat, Eglal A. Abdelaleem, Nada S. Abdelwahab
{"title":"TLC densitometric analysis of triple antibiotic therapy; Erythromycin, Sulfadiazine and Trimethoprim in different edible chicken tissues","authors":"Marco M. Z. Sharkawi, Mark T. Safwat, Eglal A. Abdelaleem, Nada S. Abdelwahab","doi":"10.1080/10826076.2023.2220126","DOIUrl":"https://doi.org/10.1080/10826076.2023.2220126","url":null,"abstract":"Abstract Erythromycin (ERY) is one of the macrolides used abundantly in veterinary medicines to treat various infections including respiratory, skin and bones. Combination of sulfadiazine (SFD) and trimethoprim (TMP) has proven efficacy and is widely used in the treatment of many infectious diseases, due to the efficiency of SFD as a bactericidal and TMP as a bacteriostatic. On the other hand, those residues of antibiotics like ERY, SFD and TMP in animal tissues may pose health hazards to humans. A simple and cost effective TLC densitometeric method has been developed to analyze the above mentioned drugs in their dosage form and in spiked chicken muscle and liver samples. A mixture of chloroform: methanol: ammonia hydroxide solution (33%, v/v) (8.5:1.5:0.1, by volume) was the developing system. In order to obtain the highest possible sensitivity, the separated bands were exposed to iodine vapors in well closed container for 15 min and then detection was immediately done at 220 nm. Linearity was achieved in the ranges of 0.5–10, 0.1–2 µg/band for ERY and SFD, respectively in both spiked muscle and liver samples while for TMP, linearity was proved over the ranges of 0.1–1.8 µg/band for spiked muscle samples and 0.1–1.6 for spiked liver samples. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"46 1","pages":"79 - 88"},"PeriodicalIF":1.3,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48766538","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}
Meghavi Mashar, Shreya Chawla, Fangyue Chen, Baker Lubwama, Kyle Patel, Mihir A Kelshiker, Patrik Bachtiger, Nicholas S Peters
{"title":"Artificial Intelligence Algorithms in Health Care: Is the Current Food and Drug Administration Regulation Sufficient?","authors":"Meghavi Mashar, Shreya Chawla, Fangyue Chen, Baker Lubwama, Kyle Patel, Mihir A Kelshiker, Patrik Bachtiger, Nicholas S Peters","doi":"10.2196/42940","DOIUrl":"10.2196/42940","url":null,"abstract":"<p><p>Given the growing use of machine learning (ML) technologies in health care, regulatory bodies face unique challenges in governing their clinical use. Under the regulatory framework of the Food and Drug Administration, approved ML algorithms are practically locked, preventing their adaptation in the ever-changing clinical environment, defeating the unique adaptive trait of ML technology in learning from real-world feedback. At the same time, regulations must enforce a strict level of patient safety to mitigate risk at a systemic level. Given that ML algorithms often support, or at times replace, the role of medical professionals, we have proposed a novel regulatory pathway analogous to the regulation of medical professionals, encompassing the life cycle of an algorithm from inception, development to clinical implementation, and continual clinical adaptation. We then discuss in-depth technical and nontechnical challenges to its implementation and offer potential solutions to unleash the full potential of ML technology in health care while ensuring quality, equity, and safety. References for this article were identified through searches of PubMed with the search terms \"Artificial intelligence,\" \"Machine learning,\" and \"regulation\" from June 25, 2017, until June 25, 2022. Articles were also identified through searches of the reference list of the articles. Only papers published in English were reviewed. The final reference list was generated based on originality and relevance to the broad scope of this paper.</p>","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"32 1","pages":"e42940"},"PeriodicalIF":0.0,"publicationDate":"2023-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11041443/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81677566","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. A. Salih, K. H. Hama Aziz, Dlivan Fatah Aziz, H. Kivrak
{"title":"Development of a stability-indicating HPLC method for the simultaneous quantification of antazoline nitrate and naphazoline sulfate in a commercial ophthalmic formulation","authors":"M. A. Salih, K. H. Hama Aziz, Dlivan Fatah Aziz, H. Kivrak","doi":"10.1080/10826076.2023.2202220","DOIUrl":"https://doi.org/10.1080/10826076.2023.2202220","url":null,"abstract":"Abstract In this work, an RP-HPLC method was established for the simultaneous quantification of antazoline sulfate and naphazoline nitrate in commercial ophthalmic formulations. The proposed method was validated for sensitivity, selectivity, linearity, accuracy, precision, and stability, and was found to be suitable for routine analysis of these two active ingredients in the presence of degradation products. The optimized conditions using a C18 column, a mobile phase (phosphate buffer: methanol, 80:20), a flow rate of 1.5 mL/min, and detection at 285 nm at room temperature. The quantification method for antazoline sulfate and naphazoline nitrate in the pharmaceutical formulation was validated in accordance with International Conference on Harmonization (ICH) Q2 (R1) guidelines for the quantitative measurement of these pharmaceuticals. Under optimal conditions, a linear relationship with high correlation coefficients (0.9999 for Antazoline Sulfate and 0.9997 for Naphazoline Nitrate) was established between the concentration ranges of 0.11 to 0.35 mg/mL for Antazoline sulfate and 0.006–0.02 mg/mL for Naphazoline nitrate. The detection limits of Antazoline sulfate and Naphazoline nitrate were determined to be 0.3 and 0.06 μg/mL, respectively. The developed method can be useful for quality control and stability testing of ophthalmic formulations containing antazoline nitrate and naphazoline sulfate. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"45 1","pages":"284 - 293"},"PeriodicalIF":1.3,"publicationDate":"2022-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44489776","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}
Katie A. Carnes, Lee D. Oliver, T. A. Brown, Roberto F. Delgadillo, Michelle S. Ward, Sina Mortazavi, Michael J. Morris, Justin W. Shearer, J. Fuller
{"title":"A Platform analytical method for intact polysorbates in protein-containing biopharmaceutical products via HPLC-CAD","authors":"Katie A. Carnes, Lee D. Oliver, T. A. Brown, Roberto F. Delgadillo, Michelle S. Ward, Sina Mortazavi, Michael J. Morris, Justin W. Shearer, J. Fuller","doi":"10.1080/10826076.2023.2207024","DOIUrl":"https://doi.org/10.1080/10826076.2023.2207024","url":null,"abstract":"Abstract Polysorbate (also known as “Tween”) 80 (PS80) is the most common surfactant in biopharmaceuticals. Here, we report a sensitive, and specific platform analytical method using reversed-phase high performance liquid chromatography employing a charged aerosol detector (HPLC-CAD), that offers the ability to quantitate intact PS80 and can distinguish between low recovery of PS80 and degraded PS80 by also monitoring several PS80 degradants which offers multiple improvements over various previously reported polysorbate analytical methods. The method employs protein/monoclonal antibody precipitation and is designed to be a quality control (QC) lab-friendly method. The method is distinguishable from other published methods because the quantification of the PS80 mono-esters is free from interference from known PS80 degradants. The method has demonstrated acceptable accuracy, precision, specificity, and sensitivity through qualification studies. The specificity afforded by the method allows for employment in forced degradation studies to discern kinetic information. Lastly, the method also has promising applications with other polysorbates (PS60, PS40, and all-laurate PS20) and shows acceptable performance with several types of biopharmaceutical proteins. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"45 1","pages":"259 - 270"},"PeriodicalIF":1.3,"publicationDate":"2022-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47945588","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}
Hai-Wen Zhang, Jie Wang, Chang-Zhao Wang, Chun-Mei Guo, Jin-Zhu Chen, Xue-Min Xiong, Qidong Tu, Xin Qin, D. Peng
{"title":"Determination of clobetasol propionate in cosmetics by high performance liquid chromatography with pre-column fluorescence derivatization of 4-hydrazino-7-nitrobenzo [C] [1,2,5] oxadiazole","authors":"Hai-Wen Zhang, Jie Wang, Chang-Zhao Wang, Chun-Mei Guo, Jin-Zhu Chen, Xue-Min Xiong, Qidong Tu, Xin Qin, D. Peng","doi":"10.1080/10826076.2023.2194967","DOIUrl":"https://doi.org/10.1080/10826076.2023.2194967","url":null,"abstract":"Abstract In this study, a fluorescent labeling reagent 4-hydrazino-7-nitrobenzo [c] [1,2,5] oxadiazole (NBD-NHNH2) was synthesized and used for fluorescence detection of clobetasol propionate in cosmetics by high performance liquid chromatography. In the presence of acidic catalyst (pH = 6.0), NBD-NHNH2 reacted at 45 °C for 30 min, and clobetasol propionate can be labeled quickly and efficiently. These derivatives have excellent stability and fluorescent properties. The maximum excitation wavelength was 450 nm, and the emission wavelength was 550 nm. The four cosmetic formulations were completely separated on a Waters e2695 HPLC C18 column by gradient elution. Under the optimal conditions, the standard curve showed a good linear response, and the correlation coefficient of r 2 = 0.9999. The LOD and LOQ were 0.01 ng/mL and 0.03 ng/mL, respectively. Therefore, NBD-NHNH2 was successfully applied in the detection of clobetasol propionate illegal added in cosmetics. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"45 1","pages":"237 - 246"},"PeriodicalIF":1.3,"publicationDate":"2022-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43770915","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 DoE-based fast and synchronous quantification of rhein, aceclofenac, and diclofenac by RP-HPLC-DAD method in spiked Wistar rat plasma: application to pharmacokinetic studies","authors":"Taufik M. Kazi, P. Dandagi, P. Biradar","doi":"10.1080/10826076.2023.2202231","DOIUrl":"https://doi.org/10.1080/10826076.2023.2202231","url":null,"abstract":"Abstract A fixed-dose combination of diacerein and aceclofenac (ACF) is commonly used in the treatment of osteoarthritis for their disease-modifying and analgesic effects, respectively. We introduce a simple, fast, sensitive, and green HPLC method for synchronous quantification of rhein (RH) (a primary metabolite of diacerein), ACF, and diclofenac (DL) (an active metabolite of ACF) in rat plasma using fenofibric acid as an internal standard (IS). The chromatographic conditions were optimized using Fractional Factorial and Box-Behnken design. Drugs were extracted by acetonitrile-methanol-based simple protein precipitation technique. The separation was performed on C18 column (Phenomenex, 250 × 4.6 mm), using acetonitrile: phosphate buffer pH 3.5 (60:40, v/v) at a 1 mL/min flow rate in a 10 min run time and detected at 264 nm. As per the USFDA guidelines, the established method was validated. RH, ACF, and DL showed good linearity in the 25–3000, 50–6000, and 50–6000 ng/mL concentration ranges respectively. The precision and accuracy results were found to be well within the acceptable range, with average recovery ranging between 92.27 and 96.10%. The developed method was found to be stable and successfully used to determine the pharmacokinetic parameters in Wistar rats after oral administration of Dycerin A tablet. Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"45 1","pages":"304 - 316"},"PeriodicalIF":1.3,"publicationDate":"2022-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49250357","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":"Determination of ointments active ingredients and parabens by one analytical method – capillary GC with cool-on-column injection and FID detection","authors":"A. Ioutsi, L. Utkina, M. Sumtsov","doi":"10.1080/10826076.2023.2202222","DOIUrl":"https://doi.org/10.1080/10826076.2023.2202222","url":null,"abstract":"Abstract In the field of quality control of medicines every pharmaceutical is tested for compliance with the requirements of the normative document for this drug to assess the quality. Among the quality indicators are the content of active ingredients and the excipients content. The more analytical methods used in a normative document, the greater the time and effort of people in all areas where a drug is developed, manufactured and controlled. A fast, precise, accurate and sensitive method has been developed for the simultaneous determination of the active ingredients of ointments of camphor, L-menthol, methyl salicylate, benzyl nicotinate, nonivamide, capsaicin, dihydrocapsaicin, nordihydrocapsaicin together with excipients, which are often para-hydroxybenzoic acid esters (parabens). The proposed gas chromatographic technique was validated. Good sensitivity for the application area (fractions of µg/mL for active ingredients and units of µg/mL for parabens), high reproducibility (relative standard deviation (RSD) doesn’t significantly exceed 2%) and the accuracy of the proposed method were demonstrated. The practical application was shown on the example of commercially available ointments. Also several assumptions about retention mechanism of such compounds were given. It seemed interesting to us for adapting proposed GC method to other components of ointments (or another dosage forms). Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"45 1","pages":"294 - 303"},"PeriodicalIF":1.3,"publicationDate":"2022-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49319899","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}