Pub Date : 2023-11-24DOI: 10.1080/10826076.2023.2284707
Thi Kieu Tiên Do, Ilona Trettin, Mona Hänni, Eike Reich
Predicting chromatographic results is a difficult task for many analysts, especially in Thin-Layer Chromatography (TLC) where reproducibility is always a critical point. The availability of suitabl...
{"title":"Applying machine learning on high-performance thin-layer chromatography using the complementary developing solvents concept","authors":"Thi Kieu Tiên Do, Ilona Trettin, Mona Hänni, Eike Reich","doi":"10.1080/10826076.2023.2284707","DOIUrl":"https://doi.org/10.1080/10826076.2023.2284707","url":null,"abstract":"Predicting chromatographic results is a difficult task for many analysts, especially in Thin-Layer Chromatography (TLC) where reproducibility is always a critical point. The availability of suitabl...","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-11-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138540054","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}
Pub Date : 2023-11-23DOI: 10.1080/10826076.2023.2284729
Selvia M. Adly, Mohamed A. Elsayed, Safa’a M. Riad, Hany H. Monir
The ternary mixture of doxycycline hyclate (DOX), ambroxol hydrochloride (AMB), and ambroxol synthetic precursor and process impurity (IMP) as chemically identified in the British Pharmacopeia as 2...
{"title":"A modern chromatographic energy-saving approach for the analysis of doxycycline, ambroxol, and its precursor and impurity: Green metric assessment and comparison","authors":"Selvia M. Adly, Mohamed A. Elsayed, Safa’a M. Riad, Hany H. Monir","doi":"10.1080/10826076.2023.2284729","DOIUrl":"https://doi.org/10.1080/10826076.2023.2284729","url":null,"abstract":"The ternary mixture of doxycycline hyclate (DOX), ambroxol hydrochloride (AMB), and ambroxol synthetic precursor and process impurity (IMP) as chemically identified in the British Pharmacopeia as 2...","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138540068","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}
Pub Date : 2023-11-23DOI: 10.1080/10826076.2023.2284708
Gertrud E. Morlock, Fang Yang
Natural bee products are increasingly used in cosmetics, health products, and food supplements. Bee pollen and propolis are quite different products, although the processing by the bees is for the ...
{"title":"Effect-directed profiling of bee pollen versus propolis","authors":"Gertrud E. Morlock, Fang Yang","doi":"10.1080/10826076.2023.2284708","DOIUrl":"https://doi.org/10.1080/10826076.2023.2284708","url":null,"abstract":"Natural bee products are increasingly used in cosmetics, health products, and food supplements. Bee pollen and propolis are quite different products, although the processing by the bees is for the ...","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138543560","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}
Pub Date : 2023-11-22DOI: 10.1080/10826076.2023.2284722
Mohamed Ali Soussi, Youssef Mallek, Wiem Ben Ayed, Slah eddine Liouane, Wahiba Douki
A new, simple, rapid, low-cost, and robust thin layer chromatography-smartphone method has been developed for the qualitative and quantitative determination of carbamazepine in human plasma. Liquid...
建立了一种简便、快速、低成本、可靠的智能手机薄层色谱定量测定人血浆中卡马西平的方法。液体……
{"title":"Application of TLC-smartphone method for the analysis of carbamazepine in plasma","authors":"Mohamed Ali Soussi, Youssef Mallek, Wiem Ben Ayed, Slah eddine Liouane, Wahiba Douki","doi":"10.1080/10826076.2023.2284722","DOIUrl":"https://doi.org/10.1080/10826076.2023.2284722","url":null,"abstract":"A new, simple, rapid, low-cost, and robust thin layer chromatography-smartphone method has been developed for the qualitative and quantitative determination of carbamazepine in human plasma. Liquid...","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138540071","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}
Pub Date : 2023-11-09DOI: 10.1080/10826076.2023.2276283
Mahammad Ali Shaik, Krishna Moorthy Manchuri, Devanna Nayakanti
AbstractA selective and sensitive new reversed-phase method was developed and validated by using Waters Acquity UHPLC system coupled with Waters Micromass Quattro PremierXE (MS/MS) to identify and quantify the genotoxic impurity 2-(2-chloroethoxy) ethanol at trace level (∼2.0 ppm) in quetiapine fumarate. The method used positive ion electrospray ionization with a multiple reaction monitoring detection mode using ACE3 C18(100 mm × 4.6 mm × 3.0 µm) column. For analysis, an isocratic program was developed using 0.01 M ammonium acetate in Milli-Q water (mobile phase A) and methanol (mobile phase B) in 20:80v/v ratio. Elution of 2-(2-chloroethoxy) ethanol was monitored using triple quadrupole mass spectrometer with an injection volume of 10 μl, a column oven temperature of 40 °C, an auto-sampler temperature of 15 °C, and flow rate of 0.5 mL/min. The retention time of 2-(2-chloroethoxy) ethanol was observed at 2.38 min. The LOQ and LOD were determined at concentrations of 0.235 ppm and 0.070 ppm respectively. The correlation coefficient R2 was 0.9983 and the percent recoveries of method range from 98.1% to 114.0%. The method was successfully validated according to International Council for Harmonization requirements (ICH Q2(R1) and ICH M7(R1)) for genotoxic impurities. The method was sensitive, selective, accurate and precise and therefore can be used for identification and quantification of genotoxic impurity 2-(2-chloroethoxy) ethanol in quetiapine fumarate.Keywords: 2-(2-chloroethoxy) ethanolgenotoxic impurityquetiapineUHPLC-MS/MSMultiple reaction monitoring (MRM) Disclosure statementNo potential conflict of interest was reported by the author(s).AcknowledgementsThe authors thank the management of Kshetra Analytics Ltd (Hyderabad, TS, India) and Jawaharlal Nehru Technological University, Anantapur (AP, India) for their support and encouragement to conduct this research.The author’s own views were expressed in this paper. The authors Shaik Mahammad Ali and Manchuri Krishna Moorthy are currently working for Novartis Health Care Pvt Ltd, Hyderabad, India.
采用Waters Acquity UHPLC系统与Waters Micromass Quattro PremierXE (MS/MS)联用,建立了一种选择性灵敏的反相方法,对富马酸喹硫平中痕量(~ 2.0 ppm)的遗传毒性杂质2-(2-氯乙氧基)乙醇进行了鉴定和定量。方法采用正离子电喷雾电离,采用多反应监测检测方式,色谱柱为ACE3 C18(100 mm × 4.6 mm × 3.0µm)。采用0.01 M醋酸铵,以20:80v/v的比例溶于milliq水(流动相A)和甲醇(流动相B),建立了等温程序。采用三联四极杆质谱仪,进样量10 μl,柱箱温度40℃,自动进样器温度15℃,流速0.5 mL/min,监测2-(2-氯乙氧基)乙醇的洗脱。2-(2-氯乙氧基)乙醇的停留时间为2.38 min,在浓度为0.235 ppm和0.070 ppm时测定定量限和定量限。相关系数R2为0.9983,加样回收率为98.1% ~ 114.0%。该方法按照国际统一委员会(ICH Q2(R1)和ICH M7(R1))对遗传毒性杂质的要求成功验证。该方法灵敏度高、选择性好、准确度高、精密度好,可用于富马酸喹硫平中遗传毒性杂质2-(2-氯乙氧基)乙醇的鉴定和定量。关键词:2-(2-氯乙氧基)乙醇毒性杂质奎硫平hplc - ms / mms多反应监测(MRM)披露声明作者未报告潜在利益冲突。作者感谢Kshetra Analytics Ltd (Hyderabad, TS, India)和Jawaharlal Nehru Technological University, Anantapur (AP, India)的管理层对开展本研究的支持和鼓励。本文表达了作者自己的观点。作者Shaik mohammad Ali和Manchuri Krishna Moorthy目前在印度海得拉巴的诺华医疗保健私人有限公司工作。
{"title":"A novel UHPLC-MS/MS method for trace level identification and quantification of genotoxic impurity 2-(2-chloroethoxy) ethanol in quetiapine fumarate","authors":"Mahammad Ali Shaik, Krishna Moorthy Manchuri, Devanna Nayakanti","doi":"10.1080/10826076.2023.2276283","DOIUrl":"https://doi.org/10.1080/10826076.2023.2276283","url":null,"abstract":"AbstractA selective and sensitive new reversed-phase method was developed and validated by using Waters Acquity UHPLC system coupled with Waters Micromass Quattro PremierXE (MS/MS) to identify and quantify the genotoxic impurity 2-(2-chloroethoxy) ethanol at trace level (∼2.0 ppm) in quetiapine fumarate. The method used positive ion electrospray ionization with a multiple reaction monitoring detection mode using ACE3 C18(100 mm × 4.6 mm × 3.0 µm) column. For analysis, an isocratic program was developed using 0.01 M ammonium acetate in Milli-Q water (mobile phase A) and methanol (mobile phase B) in 20:80v/v ratio. Elution of 2-(2-chloroethoxy) ethanol was monitored using triple quadrupole mass spectrometer with an injection volume of 10 μl, a column oven temperature of 40 °C, an auto-sampler temperature of 15 °C, and flow rate of 0.5 mL/min. The retention time of 2-(2-chloroethoxy) ethanol was observed at 2.38 min. The LOQ and LOD were determined at concentrations of 0.235 ppm and 0.070 ppm respectively. The correlation coefficient R2 was 0.9983 and the percent recoveries of method range from 98.1% to 114.0%. The method was successfully validated according to International Council for Harmonization requirements (ICH Q2(R1) and ICH M7(R1)) for genotoxic impurities. The method was sensitive, selective, accurate and precise and therefore can be used for identification and quantification of genotoxic impurity 2-(2-chloroethoxy) ethanol in quetiapine fumarate.Keywords: 2-(2-chloroethoxy) ethanolgenotoxic impurityquetiapineUHPLC-MS/MSMultiple reaction monitoring (MRM) Disclosure statementNo potential conflict of interest was reported by the author(s).AcknowledgementsThe authors thank the management of Kshetra Analytics Ltd (Hyderabad, TS, India) and Jawaharlal Nehru Technological University, Anantapur (AP, India) for their support and encouragement to conduct this research.The author’s own views were expressed in this paper. The authors Shaik Mahammad Ali and Manchuri Krishna Moorthy are currently working for Novartis Health Care Pvt Ltd, Hyderabad, India.","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135290780","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 rapid and eco-friendly method for determination of dictamnine, obacunone, and fraxinellone in Cortex Dictamni by LC–MS and matrix solid-phase dispersion extraction","authors":"Zhengming Qian, Qinggui Lei, Chuanxi Wang, Qi Huang, Wenqing Li, Wenhao Wang","doi":"10.1080/10826076.2023.2274848","DOIUrl":"https://doi.org/10.1080/10826076.2023.2274848","url":null,"abstract":"","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135871458","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}
AbstractThe analytical chemistry community has prioritized the implementation of green analytical methods in recent years to minimize the adverse effect on the environment and human beings. The combination of Azelnidipine (AZD) and Olmesartan medoxomil (OLM) was used to manage hypertension. Thus, the present study aimed to develop an RP-HPLC technique to determine AZD and OLM simultaneously by the combined framework of design of experiments and green analytical principles. A central composite design (CCD) was employed for method optimization, with ethanol, and flow rate was selected as critical variables. The effective separation was performed by Agilent Eclipse Plus (C18, 250 × 4.6 mm i.d, 5 μm) with a mobile phase comprising ethanol and 1% v/v aqueous acetic acid in the ratio of 49.5:50.5 I flowing at 1 mL/min, the detection wavelength at 250 nm. The retention time for AZD and OLM were 6.362 and 3.323, respectively. Linearity was perceived over the concentration ranges of 6.4–9.6 and 16–24 μg/mL for AZD and OLM, respectively. The green character of the proposed method showed excellent green results. This innovative eco-friendly, design of experiment technology was adequate for regular analysis of AZD and OLM in pharmaceutical dosage form without harming the environment.Keywords: Azelnidipinecentral composite designgreen HPLColmesartan medoxomil AcknowledgementThe authors are grateful to SRM College of Pharmacy, SRM Institute of Science and Technology, Kattankulathur, for motivating us to carry out this research.Disclosure statementNo potential conflict of interest was reported by the author(s)
{"title":"Eco-friendly design of experiment based approach for estimation of azelnidipine and olmesartan medoxomil in RP-HPLC: Greenness appraisal","authors":"Naveenarani Dharuman, Lakshmi Karunanidhi Santhana, Manikandan Krishnan","doi":"10.1080/10826076.2023.2270734","DOIUrl":"https://doi.org/10.1080/10826076.2023.2270734","url":null,"abstract":"AbstractThe analytical chemistry community has prioritized the implementation of green analytical methods in recent years to minimize the adverse effect on the environment and human beings. The combination of Azelnidipine (AZD) and Olmesartan medoxomil (OLM) was used to manage hypertension. Thus, the present study aimed to develop an RP-HPLC technique to determine AZD and OLM simultaneously by the combined framework of design of experiments and green analytical principles. A central composite design (CCD) was employed for method optimization, with ethanol, and flow rate was selected as critical variables. The effective separation was performed by Agilent Eclipse Plus (C18, 250 × 4.6 mm i.d, 5 μm) with a mobile phase comprising ethanol and 1% v/v aqueous acetic acid in the ratio of 49.5:50.5 I flowing at 1 mL/min, the detection wavelength at 250 nm. The retention time for AZD and OLM were 6.362 and 3.323, respectively. Linearity was perceived over the concentration ranges of 6.4–9.6 and 16–24 μg/mL for AZD and OLM, respectively. The green character of the proposed method showed excellent green results. This innovative eco-friendly, design of experiment technology was adequate for regular analysis of AZD and OLM in pharmaceutical dosage form without harming the environment.Keywords: Azelnidipinecentral composite designgreen HPLColmesartan medoxomil AcknowledgementThe authors are grateful to SRM College of Pharmacy, SRM Institute of Science and Technology, Kattankulathur, for motivating us to carry out this research.Disclosure statementNo potential conflict of interest was reported by the author(s)","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136381260","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}
Pub Date : 2023-10-18DOI: 10.1080/10826076.2023.2269233
Robert Minkner, Udo Burger, Louis Malz, Susanne Doerks, Hermann Wätzig
AbstractCapillary electrophoresis-sodium dodecyl sulfate (CE-SDS) is a modern form of SDS-PAGE that uses capillary electrophoresis to separate proteins by size. The technique is based on the sieving effect of net-like structures in the capillary. In this study, we compared the Maurice Turbo CE-SDS Cartridge™ with the established Maurice CE-SDS PLUS Cartridge, both developed for the Maurice CE system. The Turbo cartridge was found to be up to 4–5 times faster than the PLUS cartridge, while maintaining similar separation efficiency. The limit of quantitation (LOQ) for the Turbo cartridge was estimated to be 0.1 mg/mL with a signal-to-noise ratio (S/N) of 18.55. The linearity of the cartridge was verified in the range of 0.1–4 mg/mL, with correlation coefficient (R2) values of at least 0.99. The separation efficiency remained constant over long series of measurements, and the relative migration time of proteins in a mixture remained stable over 1,000 injections. These results demonstrate that the Turbo CE-SDS Cartridge is a very useful tool for fast and efficient analysis of protein (mixtures). The shorter analysis time can save significant resources by reducing the time and consumables required for analysis, while the high LOQ and linearity ensure that the method is sensitive and accurate.Keywords: CECE-SDScomparisongel electrophoresisvalidation Disclosure StatementThe authors declare there is no Complete of Interest at this study.AcknowledgmentsNot applicableAuthors’ contributionsRM performed the experiments, wrote the manuscript, and designed the study. UB participated in study design and partly supervised the project. LM carried out repetitive experiments as instructed. SD partly supervised the project. HW supervised the entire project and revised the manuscript. All authors read and approved the final manuscript.Availability of data and materialsAll relevant data generated or analyzed during this study are included in this published article and its additional file. The missing datasets used and/or analyzed during the current study are available from the corresponding author upon reasonable request.Competing interestsUdo Burger and Susanne Doerks are employes of ProteinSimple (a Bio-Techne Brand).Consent for publicationNot applicable.Declaration of interestUdo Burger and Susanne Doerks are employees of Bio-Techne.Ethics approval and consent to participateNot applicable.Additional informationFundingThis work was supported by Protein Simple (a Brand of Bio-Techne) with materials.
{"title":"Efficient and reliable CE-SDS separations by the high-speed turbo CE-SDS <sup>®</sup> cartridge","authors":"Robert Minkner, Udo Burger, Louis Malz, Susanne Doerks, Hermann Wätzig","doi":"10.1080/10826076.2023.2269233","DOIUrl":"https://doi.org/10.1080/10826076.2023.2269233","url":null,"abstract":"AbstractCapillary electrophoresis-sodium dodecyl sulfate (CE-SDS) is a modern form of SDS-PAGE that uses capillary electrophoresis to separate proteins by size. The technique is based on the sieving effect of net-like structures in the capillary. In this study, we compared the Maurice Turbo CE-SDS Cartridge™ with the established Maurice CE-SDS PLUS Cartridge, both developed for the Maurice CE system. The Turbo cartridge was found to be up to 4–5 times faster than the PLUS cartridge, while maintaining similar separation efficiency. The limit of quantitation (LOQ) for the Turbo cartridge was estimated to be 0.1 mg/mL with a signal-to-noise ratio (S/N) of 18.55. The linearity of the cartridge was verified in the range of 0.1–4 mg/mL, with correlation coefficient (R2) values of at least 0.99. The separation efficiency remained constant over long series of measurements, and the relative migration time of proteins in a mixture remained stable over 1,000 injections. These results demonstrate that the Turbo CE-SDS Cartridge is a very useful tool for fast and efficient analysis of protein (mixtures). The shorter analysis time can save significant resources by reducing the time and consumables required for analysis, while the high LOQ and linearity ensure that the method is sensitive and accurate.Keywords: CECE-SDScomparisongel electrophoresisvalidation Disclosure StatementThe authors declare there is no Complete of Interest at this study.AcknowledgmentsNot applicableAuthors’ contributionsRM performed the experiments, wrote the manuscript, and designed the study. UB participated in study design and partly supervised the project. LM carried out repetitive experiments as instructed. SD partly supervised the project. HW supervised the entire project and revised the manuscript. All authors read and approved the final manuscript.Availability of data and materialsAll relevant data generated or analyzed during this study are included in this published article and its additional file. The missing datasets used and/or analyzed during the current study are available from the corresponding author upon reasonable request.Competing interestsUdo Burger and Susanne Doerks are employes of ProteinSimple (a Bio-Techne Brand).Consent for publicationNot applicable.Declaration of interestUdo Burger and Susanne Doerks are employees of Bio-Techne.Ethics approval and consent to participateNot applicable.Additional informationFundingThis work was supported by Protein Simple (a Brand of Bio-Techne) with materials.","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135888610","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}
Pub Date : 2023-09-29DOI: 10.1080/10826076.2023.2262002
Mohd Shafie Zabidi, Ruzilawati Abu Bakar, Nurfadhlina Musa, Suzana Mustafa, Wan Nasrudin Wan Ismail, Siti Nur Aziela Ab Manap, Nur Aishah Che Mohd Zaid, Wan Nazirah Wan Yusuf
AbstractColistin, in the form of colistin methanesulfonate sodium (CMS), has a narrow therapeutic window, and colistin levels must be monitored during treatment. The aim of this study was to develop and validate a high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method for measuring colistin in human serum. Colistin was extracted from human serum using trichloroacetic acid and methanol for protein precipitation, followed by in-solid phase extraction derivatization with 9-fluorenylmethyl chloroformate. HPLC-FLD system using a reverse-phase HPLC C18 column and a mobile phase consisting of acetonitrile, tetrahydrofuran, and water (80%:4%:16%) were used for the quantification of colistin A, colistin B, and polymyxin B (internal standard) in human serum. The extraction recoveries were between 71% and 103%. Linear calibration curves were obtained for colistin in concentrations from 0.3 to 8.0 μg/mL, with good fit (r2 = 0.9993). The lower limit of quantitation was 0.3 μg/mL. The intra- and inter-day precision of the assay was 0.5–5% and 3.5–9.4%, respectively. The accuracy ranged from 98% to 100%. This validated method was successfully applied to the analysis of serum-receiving CMS in critically ill patients. This method will be useful to assist colistin dosage adjustment based on individual blood colistin levels for optimization of colistin therapy.Keywords: Colistin methanesulfonate sodiumcolistincritically ill patientsHPLC-FLDTDM AcknowledgementThe authors would like to thank the Director General of Health Malaysia for his permission to publish this article. We would also like to acknowledge the recruited patients and family, nurses, and staff members of the intensive care unit of Hospital Raja Perempuan Zainab II, Kota Bahru for their cooperation in conducting the research. The authors would also like to acknowledge staff members of Laboratory Department of Pharmacology, School of Medical Sciences, Universiti Sains Malaysia for their support and help.Disclosure statementNo potential conflict of interest was reported by the author(s).Additional informationFundingThis study was supported by USM Bridging Grant No: 304.PPSP.6316240 and GIPS-PhD Grant No: 311/PPSP/4404810. The first author was supported by Malaysia Ministry of Health, Hadiah Latihan Persekutuan (HLP). Institute of Postgraduate Studies, Universiti Sains Malaysia
摘要粘菌素以粘菌素甲磺酸钠(CMS)的形式存在,其治疗窗口期较窄,在治疗过程中必须监测粘菌素水平。本研究的目的是建立并验证一种高效液相色谱-荧光检测(HPLC-FLD)测定人血清中粘菌素的方法。采用三氯乙酸和甲醇沉淀法从人血清中提取粘菌素,然后用9-氟酰氯甲酸甲酯进行固相萃取衍生化。HPLC- fld系统采用反相高效液相色谱C18柱,流动相为乙腈、四氢呋喃和水(80%:4%:16%),定量测定人血清中粘菌素a、粘菌素B和多粘菌素B(内标)。提取回收率在71% ~ 103%之间。在0.3 ~ 8.0 μg/mL范围内建立了线性校准曲线,拟合良好(r2 = 0.9993)。定量下限为0.3 μg/mL。日内精密度为0.5 ~ 5%,日内精密度为3.5 ~ 9.4%。准确率从98%到100%不等。该方法已成功应用于危重患者接受血清CMS的分析。该方法将有助于根据个体血液粘菌素水平调整粘菌素剂量,以优化粘菌素治疗。关键词:粘菌素甲磺酸钠粘菌危重病人shplc - fldtdm作者感谢马来西亚卫生部局长允许发表这篇文章。我们还要感谢哥打巴鲁Raja Perempuan Zainab II医院特护病房的受聘病人和家属、护士和工作人员在开展研究方面的合作。作者还要感谢马来西亚理科大学医学院药理学实验室工作人员的支持和帮助。披露声明作者未报告潜在的利益冲突。本研究由USM桥接基金No . 304.PPSP资助。GIPS-PhD资助号:311/PPSP/4404810。第一作者得到了马来西亚卫生部Hadiah Latihan Persekutuan (HLP)的支持。马来西亚理科大学研究生院
{"title":"High-performance liquid chromatography with fluorescence detection method for measuring colistin in human serum and its application in critically ill patients treated with colistin methanesulfonate sodium","authors":"Mohd Shafie Zabidi, Ruzilawati Abu Bakar, Nurfadhlina Musa, Suzana Mustafa, Wan Nasrudin Wan Ismail, Siti Nur Aziela Ab Manap, Nur Aishah Che Mohd Zaid, Wan Nazirah Wan Yusuf","doi":"10.1080/10826076.2023.2262002","DOIUrl":"https://doi.org/10.1080/10826076.2023.2262002","url":null,"abstract":"AbstractColistin, in the form of colistin methanesulfonate sodium (CMS), has a narrow therapeutic window, and colistin levels must be monitored during treatment. The aim of this study was to develop and validate a high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method for measuring colistin in human serum. Colistin was extracted from human serum using trichloroacetic acid and methanol for protein precipitation, followed by in-solid phase extraction derivatization with 9-fluorenylmethyl chloroformate. HPLC-FLD system using a reverse-phase HPLC C18 column and a mobile phase consisting of acetonitrile, tetrahydrofuran, and water (80%:4%:16%) were used for the quantification of colistin A, colistin B, and polymyxin B (internal standard) in human serum. The extraction recoveries were between 71% and 103%. Linear calibration curves were obtained for colistin in concentrations from 0.3 to 8.0 μg/mL, with good fit (r2 = 0.9993). The lower limit of quantitation was 0.3 μg/mL. The intra- and inter-day precision of the assay was 0.5–5% and 3.5–9.4%, respectively. The accuracy ranged from 98% to 100%. This validated method was successfully applied to the analysis of serum-receiving CMS in critically ill patients. This method will be useful to assist colistin dosage adjustment based on individual blood colistin levels for optimization of colistin therapy.Keywords: Colistin methanesulfonate sodiumcolistincritically ill patientsHPLC-FLDTDM AcknowledgementThe authors would like to thank the Director General of Health Malaysia for his permission to publish this article. We would also like to acknowledge the recruited patients and family, nurses, and staff members of the intensive care unit of Hospital Raja Perempuan Zainab II, Kota Bahru for their cooperation in conducting the research. The authors would also like to acknowledge staff members of Laboratory Department of Pharmacology, School of Medical Sciences, Universiti Sains Malaysia for their support and help.Disclosure statementNo potential conflict of interest was reported by the author(s).Additional informationFundingThis study was supported by USM Bridging Grant No: 304.PPSP.6316240 and GIPS-PhD Grant No: 311/PPSP/4404810. The first author was supported by Malaysia Ministry of Health, Hadiah Latihan Persekutuan (HLP). Institute of Postgraduate Studies, Universiti Sains Malaysia","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135246229","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}
Pub Date : 2023-07-06DOI: 10.1080/10826076.2023.2230594
S. Apostolov, D. Brkić, G. Vastag
Abstract The first phase of the evaluation of the biological profile of novel isatin derivatives included the theoretical verification of their drug-likeness and lead-likeness properties. In the second phase, chromatographic parameters (R M 0, m and C 0) were determined using RPTLC in the presence of four different organic modifiers. Linear regression and multivariate analysis were used to examine the correlation between chromatographic parameters, as assumed measures of lipophilicity of the investigated isatine derivatives, computer-derived logP values, drug-likeness and lead-likeness descriptors, as well as ecotoxicity parameters. The obtained relationships indicated that the agreement of studied bioactivity parameters of isatin derivatives is conditioned by the polarity of the substituent present in the molecule, and to a lesser extent by its electronic effects. Graphical Abstract
{"title":"Chemometrically assisted evaluation of isatine derivatives’ chromatographic and computational descriptors","authors":"S. Apostolov, D. Brkić, G. Vastag","doi":"10.1080/10826076.2023.2230594","DOIUrl":"https://doi.org/10.1080/10826076.2023.2230594","url":null,"abstract":"Abstract The first phase of the evaluation of the biological profile of novel isatin derivatives included the theoretical verification of their drug-likeness and lead-likeness properties. In the second phase, chromatographic parameters (R M 0, m and C 0) were determined using RPTLC in the presence of four different organic modifiers. Linear regression and multivariate analysis were used to examine the correlation between chromatographic parameters, as assumed measures of lipophilicity of the investigated isatine derivatives, computer-derived logP values, drug-likeness and lead-likeness descriptors, as well as ecotoxicity parameters. The obtained relationships indicated that the agreement of studied bioactivity parameters of isatin derivatives is conditioned by the polarity of the substituent present in the molecule, and to a lesser extent by its electronic effects. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-07-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"59682588","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}