Pub Date : 2022-07-21DOI: 10.1080/10826076.2023.2165096
Nianhua Jing, Junyou Shi, Jiang Hu, Zhiwei Sun
Abstract Three kinds of “Snowlotus” including Saussurea involucrate, Saussurea medusa and Saussurea laniceps had been prescribed as folk medicine interchangeably in Tibet and Uygur, China. To verify the feasibility of this phenomenon, a HPLC-DAD-ESI-MS method was developed in this study to determine the flavonoid compounds from three Saussurea species qualitatively and quantitatively. The LODs and LOQs ranged from 0.0263–0.1172 µg/mL and 0.0862–0.3867 µg/mL, respectively. The relative standard deviation (RSD × 100%) of the validation for the instrument precision was below 2.03%, while the RSD × 100% values for the method precision were below 5.73%, respectively. The recoveries ranged from 92.98–101.79%. These results further demonstrated that this method was precise and practical for determining flavonoid compounds from three Saussurea species. In this study, 14 kinds of constituents were simultaneously identified according to the ESI-MS data and previous studies. The contents of total flavonoids and eight components were determined with spectrophotometry and HPLC-DAD methods, respectively. The results demonstrated that the total flavonoids in S. involucrate had the hightest value and there were some differences in the content of eight flavonoids. For S. involucrate, a proportion of rutin, luteolin-7-O-glucoside, and hispidulin were detected. For S. laniceps, Arctiin, apigenin, and arctigenin were the major flavonoid compounds. For S. medusa, seven types of compounds were detected and arctiin presented the highest value, whereas apigenlin exhibited the lowest value. This comparative study may promote the differentiation in use of three kinds of snowlotus. Graphical abstract
{"title":"Comparative study on flavonoids from Tibetan medicinal plants Saussurea species using HPLC-DAD-ESI-MS","authors":"Nianhua Jing, Junyou Shi, Jiang Hu, Zhiwei Sun","doi":"10.1080/10826076.2023.2165096","DOIUrl":"https://doi.org/10.1080/10826076.2023.2165096","url":null,"abstract":"Abstract Three kinds of “Snowlotus” including Saussurea involucrate, Saussurea medusa and Saussurea laniceps had been prescribed as folk medicine interchangeably in Tibet and Uygur, China. To verify the feasibility of this phenomenon, a HPLC-DAD-ESI-MS method was developed in this study to determine the flavonoid compounds from three Saussurea species qualitatively and quantitatively. The LODs and LOQs ranged from 0.0263–0.1172 µg/mL and 0.0862–0.3867 µg/mL, respectively. The relative standard deviation (RSD × 100%) of the validation for the instrument precision was below 2.03%, while the RSD × 100% values for the method precision were below 5.73%, respectively. The recoveries ranged from 92.98–101.79%. These results further demonstrated that this method was precise and practical for determining flavonoid compounds from three Saussurea species. In this study, 14 kinds of constituents were simultaneously identified according to the ESI-MS data and previous studies. The contents of total flavonoids and eight components were determined with spectrophotometry and HPLC-DAD methods, respectively. The results demonstrated that the total flavonoids in S. involucrate had the hightest value and there were some differences in the content of eight flavonoids. For S. involucrate, a proportion of rutin, luteolin-7-O-glucoside, and hispidulin were detected. For S. laniceps, Arctiin, apigenin, and arctigenin were the major flavonoid compounds. For S. medusa, seven types of compounds were detected and arctiin presented the highest value, whereas apigenlin exhibited the lowest value. This comparative study may promote the differentiation in use of three kinds of snowlotus. Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45050185","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 : 2022-05-09DOI: 10.1080/10826076.2022.2134146
Mohammed AlSaeedy, Ahmed Hasan, Arwa Al-Adhreai, Ali Alrabie, Hafsah Qaba, Abdulrahman Mashrah, Elif Mine Öncü-Kaya
Abstract Pregabalin, Lacosamide, Rufinamide, Perampanel, Eslicarbazepine acetate, Brivaracetam, Cannabidiol, Stiripentol, Everolimus, Cenobamate, and Fenfluramine are drugs of the third generation of antiepileptic drugs registered by International Coalition of Medicine Regulatory Authorities between 2000 and 2021. There are 213 peer-reviewed papers on antiepileptic drug analysis in the literature over the last three decades (1990–2022) which were reviewed in this article to provide an extensive overview of liquid chromatography techniques used to determine antiepileptic drugs. These details were discussed on the basis of a matrix: additives that are used to prepare a dosage form, sample preparation technique, column, limits of detection and quantification, types of elution in chromatography (isocratic or gradient), and detector. This review article will provide vital information to the scientific community in order to identify the most appropriate approach for antiepileptic drug analysis and determination. Graphical Abstract
{"title":"An overview of liquid chromatographic methods for analyzing new generation anti-epileptic drugs","authors":"Mohammed AlSaeedy, Ahmed Hasan, Arwa Al-Adhreai, Ali Alrabie, Hafsah Qaba, Abdulrahman Mashrah, Elif Mine Öncü-Kaya","doi":"10.1080/10826076.2022.2134146","DOIUrl":"https://doi.org/10.1080/10826076.2022.2134146","url":null,"abstract":"Abstract Pregabalin, Lacosamide, Rufinamide, Perampanel, Eslicarbazepine acetate, Brivaracetam, Cannabidiol, Stiripentol, Everolimus, Cenobamate, and Fenfluramine are drugs of the third generation of antiepileptic drugs registered by International Coalition of Medicine Regulatory Authorities between 2000 and 2021. There are 213 peer-reviewed papers on antiepileptic drug analysis in the literature over the last three decades (1990–2022) which were reviewed in this article to provide an extensive overview of liquid chromatography techniques used to determine antiepileptic drugs. These details were discussed on the basis of a matrix: additives that are used to prepare a dosage form, sample preparation technique, column, limits of detection and quantification, types of elution in chromatography (isocratic or gradient), and detector. This review article will provide vital information to the scientific community in order to identify the most appropriate approach for antiepileptic drug analysis and determination. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47489979","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}
Abstract The main product of acetylation of ferrocene was successfully separated and purified with high purity from synthetic mixtures by countercurrent chromatography using a selected biphasic solvent system. According to distribution performance of main product and reactant, a two-phase solvent system was selected by thin layer chromatography, in which the partition coefficient for each component was determined by HPLC. Then a two-phase solvent system consisting of petroleum ether/ethyl acetate/methanol/water (6:4:6:4, v/v) was selected. After acetylation reaction, 20 mg of synthetic mixture was subjected to countercurrent chromatography, yielding 2.1 mg of ferrocene and 8.7 mg of acetyl ferrocene with 96.6% and 97.4% purity. Results indicated that countercurrent chromatography is a very efficient method for separation and purification of target product from synthetic mixtures. GRAPHICAL ABSTRACT
{"title":"Separation of acetylferrocene from synthetic mixtures by countercurrent chromatography","authors":"Xiao‐yong Lv, Haibo You, Huiyun Qiu, Mengyi Wen, Chuncui Zheng, Shengqiang Tong","doi":"10.1080/10826076.2022.2143798","DOIUrl":"https://doi.org/10.1080/10826076.2022.2143798","url":null,"abstract":"Abstract The main product of acetylation of ferrocene was successfully separated and purified with high purity from synthetic mixtures by countercurrent chromatography using a selected biphasic solvent system. According to distribution performance of main product and reactant, a two-phase solvent system was selected by thin layer chromatography, in which the partition coefficient for each component was determined by HPLC. Then a two-phase solvent system consisting of petroleum ether/ethyl acetate/methanol/water (6:4:6:4, v/v) was selected. After acetylation reaction, 20 mg of synthetic mixture was subjected to countercurrent chromatography, yielding 2.1 mg of ferrocene and 8.7 mg of acetyl ferrocene with 96.6% and 97.4% purity. Results indicated that countercurrent chromatography is a very efficient method for separation and purification of target product from synthetic mixtures. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47783617","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 : 2022-05-09DOI: 10.1080/10826076.2022.2117190
Zhicong Liu, Yongjie Zhao, Huihui Peng, Tiexuan Luo, Yang Liu
Abstract Countercurrent chromatography (CCC) is the separation technique based on the different partition coefficients of the sample between two immiscible solvents, which is a liquid-liquid partition without solid support in the column. In this paper, Firstly, the mechanic’s equilibrium principle of CCC is described, which includes hydrostatic equilibrium system (HSES), hydrodynamic equilibrium system (HDES), unidirectional hydrodynamic equilibrium phenomenon, etc. The separation principle of the CCC is also explained. Secondly, the mechanical structure and design of parallel-axis CCC, cross-axis CCC, oblique-axis CCC, as well as some CCC derived from the three are illustrated respectively. Finally, the existing problems for the development of CCC have been exposed, and the trend of the future development direction and applications of CCC are discussed. Graphical Abstract
{"title":"Countercurrent chromatography: separation principle, mechanical design, development trends, and applications","authors":"Zhicong Liu, Yongjie Zhao, Huihui Peng, Tiexuan Luo, Yang Liu","doi":"10.1080/10826076.2022.2117190","DOIUrl":"https://doi.org/10.1080/10826076.2022.2117190","url":null,"abstract":"Abstract Countercurrent chromatography (CCC) is the separation technique based on the different partition coefficients of the sample between two immiscible solvents, which is a liquid-liquid partition without solid support in the column. In this paper, Firstly, the mechanic’s equilibrium principle of CCC is described, which includes hydrostatic equilibrium system (HSES), hydrodynamic equilibrium system (HDES), unidirectional hydrodynamic equilibrium phenomenon, etc. The separation principle of the CCC is also explained. Secondly, the mechanical structure and design of parallel-axis CCC, cross-axis CCC, oblique-axis CCC, as well as some CCC derived from the three are illustrated respectively. Finally, the existing problems for the development of CCC have been exposed, and the trend of the future development direction and applications of CCC are discussed. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46058462","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 : 2022-05-09DOI: 10.1080/10826076.2023.2173608
Diva C. Purohit, Jigna Vadalia, H. Joshi, Udaykumar G. Vegad
Abstract Adulterating herbal and dietary supplements with synthetic hypoglycemics is widely practiced, especially in developing and undeveloped countries. A simple, precise, and novel method was developed to simultaneously determine synthetic antidiabetics belonging to different classes, namely biguanide, sulfonylurea, and thiazolidinedione, in counterfeit herbal products as adulterants using HPTLC-MS. The method can simultaneously identify and quantify undeclared synthetic drugs metformin, pioglitazone, glipizide, and glimepiride in herbal as well as dietary supplements. The optimized mobile phase for the TLC system consists of cyclohexane:dichloromethane:1-propanol:saturated solution of ammonium acetate in acetic acid in the ratio of (7:5:2:2, v/v/v/v). The method is highly selective and sensitive for detecting chemicals in complex herbal molecules. Identification and quantification of drugs were performed using the densitometric method. The drugs were confirmed using triple quadrupole mass spectrometry through the MS interface. The screening of market preparations revealed the presence of metformin in two of eight products. This study shows that the method for simultaneous determination of these four drugs can be applied successfully to screen synthetic antidiabetics in the herbal complex matrix as adulterants. Graphical abstract
{"title":"Rapid screening of undeclared hypoglycemics in counterfeit herbal antidiabetic products using HPTLC-MS","authors":"Diva C. Purohit, Jigna Vadalia, H. Joshi, Udaykumar G. Vegad","doi":"10.1080/10826076.2023.2173608","DOIUrl":"https://doi.org/10.1080/10826076.2023.2173608","url":null,"abstract":"Abstract Adulterating herbal and dietary supplements with synthetic hypoglycemics is widely practiced, especially in developing and undeveloped countries. A simple, precise, and novel method was developed to simultaneously determine synthetic antidiabetics belonging to different classes, namely biguanide, sulfonylurea, and thiazolidinedione, in counterfeit herbal products as adulterants using HPTLC-MS. The method can simultaneously identify and quantify undeclared synthetic drugs metformin, pioglitazone, glipizide, and glimepiride in herbal as well as dietary supplements. The optimized mobile phase for the TLC system consists of cyclohexane:dichloromethane:1-propanol:saturated solution of ammonium acetate in acetic acid in the ratio of (7:5:2:2, v/v/v/v). The method is highly selective and sensitive for detecting chemicals in complex herbal molecules. Identification and quantification of drugs were performed using the densitometric method. The drugs were confirmed using triple quadrupole mass spectrometry through the MS interface. The screening of market preparations revealed the presence of metformin in two of eight products. This study shows that the method for simultaneous determination of these four drugs can be applied successfully to screen synthetic antidiabetics in the herbal complex matrix as adulterants. Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47709995","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 : 2022-05-09DOI: 10.1080/10826076.2022.2126856
Ravi Solanki, C. Patel, Ravi Patel, Anujkumar Maradiya, Shalin Parikh, Bhavinkumar Gayakvad
Abstract As per the ICH M7 guideline nitrosamine impurities are referred to as cohort of concern which are having a potential significant carcinogenic risk and for the safe human consumption of drug products, the levels of nitrosamine impurities need to be controlled as per respective permissible daily exposures (PDE). An accurate, precise, sensitive, and robust UPLC-APCI-TQ-MS/MS method has been developed for the quantification of eight nitrosamine impurities in the marketed formulation of metformin and glipizide Tablets. Chromatographic separation was achieved using Kinetex® 150 × 3.0 mm Biphenyl 100 Å, 2.6 µm column with mobile phase A (0.1% w/v formic acid dissolved in water) and mobile phase B (0.1% w/v formic acid dissolved in methanol) with a flow rate of 0.4 mL per minute having run time of 20 min with gradient mode of elution. As per ICH Q2(R1) guideline the method had been validated which demonstrates the sensitivity of the developed method with a good linearity range of 1–5 ng/mL for all eight nitrosamine impurities. The validation parameters suggest that the developed method for the simultaneous quantification of eight nitrosamine impurities in the marketed formulation of metformin hydrochloride and glipizide can be routinely applied in the quality control laboratory. Graphical Abstract
{"title":"UHPLC-APCI-TQ-MS analytical method to quantify nitrosamine impurities in the commercial formulation of metformin and glipizide","authors":"Ravi Solanki, C. Patel, Ravi Patel, Anujkumar Maradiya, Shalin Parikh, Bhavinkumar Gayakvad","doi":"10.1080/10826076.2022.2126856","DOIUrl":"https://doi.org/10.1080/10826076.2022.2126856","url":null,"abstract":"Abstract As per the ICH M7 guideline nitrosamine impurities are referred to as cohort of concern which are having a potential significant carcinogenic risk and for the safe human consumption of drug products, the levels of nitrosamine impurities need to be controlled as per respective permissible daily exposures (PDE). An accurate, precise, sensitive, and robust UPLC-APCI-TQ-MS/MS method has been developed for the quantification of eight nitrosamine impurities in the marketed formulation of metformin and glipizide Tablets. Chromatographic separation was achieved using Kinetex® 150 × 3.0 mm Biphenyl 100 Å, 2.6 µm column with mobile phase A (0.1% w/v formic acid dissolved in water) and mobile phase B (0.1% w/v formic acid dissolved in methanol) with a flow rate of 0.4 mL per minute having run time of 20 min with gradient mode of elution. As per ICH Q2(R1) guideline the method had been validated which demonstrates the sensitivity of the developed method with a good linearity range of 1–5 ng/mL for all eight nitrosamine impurities. The validation parameters suggest that the developed method for the simultaneous quantification of eight nitrosamine impurities in the marketed formulation of metformin hydrochloride and glipizide can be routinely applied in the quality control laboratory. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48563205","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 : 2022-02-25DOI: 10.1080/10826076.2022.2098760
Ala A. Alhusban, Lama A. Hamadneh, Aliaa I. Shallan, O. Tarawneh
Abstract Breast cancer is among the most common cancer types worldwide. The first and second line treatment protocols for various stages of breast cancer in females rely on tamoxifen. Until now, the development of tamoxifen resistance is not entirely understood. In this study, an automated sequential injection capillary electrophoresis with capacitively coupled contactless conductivity detector was developed for online levels monitoring of both lactate and pyruvate from the supernatant media of MCF-7 cells developing tamoxifen resistance. Changes in concentration of the two metabolites were simultaneously monitored from three model cell cultures and two control untreated cells. The electrophoretic separation was performed under reversed electroosmotic flow conditions. The system delivers high sample throughput at low sample consumption of 20 µL per analysis. The method is robust and achieved high sensitivity and resolution. Limits of detection were 8.0 and 17.0 nM and linear ranges were 0.15–5 and 0.01–1 mM with a correlation coefficient of 0.9951 and 0.9963 for lactate and pyruvate, respectively. Inter-run and intra-run accuracy were in the range of 95.37–107.02% with precision (RSD, %) of ≤9.84%. The method was completely validated and the data obtained were in agreement with results achieved using the lactate and pyruvate assay kits. The highly informative generated data revealed a significant increase in lactate and pyruvate production in the three tamoxifen resistant MCF-7 cells models compared to the two control cells starting from 5.8 hours and 6.8 hours culturing times, respectively. The increase in concentrations of both lactate and pyruvate were correlated with an increase in MCT1 and MCT4 genes expression. Graphical abstract
{"title":"Automated online monitoring of lactate and pyruvate in tamoxifen resistant MCF-7 cells using sequential-injection capillary electrophoresis with contactless conductivity detection (SI-CE-C4D) and correlation with MCT1 and MCT4 genes expression","authors":"Ala A. Alhusban, Lama A. Hamadneh, Aliaa I. Shallan, O. Tarawneh","doi":"10.1080/10826076.2022.2098760","DOIUrl":"https://doi.org/10.1080/10826076.2022.2098760","url":null,"abstract":"Abstract Breast cancer is among the most common cancer types worldwide. The first and second line treatment protocols for various stages of breast cancer in females rely on tamoxifen. Until now, the development of tamoxifen resistance is not entirely understood. In this study, an automated sequential injection capillary electrophoresis with capacitively coupled contactless conductivity detector was developed for online levels monitoring of both lactate and pyruvate from the supernatant media of MCF-7 cells developing tamoxifen resistance. Changes in concentration of the two metabolites were simultaneously monitored from three model cell cultures and two control untreated cells. The electrophoretic separation was performed under reversed electroosmotic flow conditions. The system delivers high sample throughput at low sample consumption of 20 µL per analysis. The method is robust and achieved high sensitivity and resolution. Limits of detection were 8.0 and 17.0 nM and linear ranges were 0.15–5 and 0.01–1 mM with a correlation coefficient of 0.9951 and 0.9963 for lactate and pyruvate, respectively. Inter-run and intra-run accuracy were in the range of 95.37–107.02% with precision (RSD, %) of ≤9.84%. The method was completely validated and the data obtained were in agreement with results achieved using the lactate and pyruvate assay kits. The highly informative generated data revealed a significant increase in lactate and pyruvate production in the three tamoxifen resistant MCF-7 cells models compared to the two control cells starting from 5.8 hours and 6.8 hours culturing times, respectively. The increase in concentrations of both lactate and pyruvate were correlated with an increase in MCT1 and MCT4 genes expression. Graphical abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42423120","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 : 2022-02-25DOI: 10.1080/10826076.2022.2124267
Ke Yang, Ying Chen, Zhang Xiaoqing, Q. Zhen, Wenwu Gui, Yanna Ban, Yifan He, Shengnan Pan, Min Ding
Abstract Microbiota-derived indoles were closely associated with psychological disorders like depression. We aimed to develop an HPLC method with fluorescence detection (FLD) for simultaneous determination of plasma indoles, including indoxyl sulfate (3-INDS), indole-3-acetic acid (IAA), indole-3-propionate (IPA), indole (IND) and 3-methylindole (3-MI). Diethyl ether and ethyl acetate were selected as the mixed extractant for the sample preparation. The separation was carried out on a Shim-Pack VP-ODS column (150 × 4.6 mm, 4.6 µm) with the mobile phase composed of 10 mmol/L sodium dihydrogen phosphate/methanol (40:60, v/v). The excitation and emission wavelengths were set at 280 and 355 nm, respectively. The linearities in plasma were obtained in the range of 1.56–400.0 μmol/L for 3-INDS, 0.312–10.0 μmol/L for IAA, 0.125–6.00 μmol/L for IPA, 6.25–400.0 nmol/L for IND, and 1.56–400.0 nmol/L for 3-MI, respectively. The coefficients of variation (CVs) for each analyte of the intra-day and inter-day precisions were within 4.0 and 5.2%, respectively. The recoveries were in the range of 90.1–109.3%. This sensitive and accurate method was applied to analyze plasma indoles for the diagnostic of depression in the patients with polycystic ovary syndrome (PCOS). Graphical Abstract
{"title":"Simultaneous determination of plasma indoles by HPLC with fluorescence detection: Application in polycystic ovary syndrome patients with/without depression","authors":"Ke Yang, Ying Chen, Zhang Xiaoqing, Q. Zhen, Wenwu Gui, Yanna Ban, Yifan He, Shengnan Pan, Min Ding","doi":"10.1080/10826076.2022.2124267","DOIUrl":"https://doi.org/10.1080/10826076.2022.2124267","url":null,"abstract":"Abstract Microbiota-derived indoles were closely associated with psychological disorders like depression. We aimed to develop an HPLC method with fluorescence detection (FLD) for simultaneous determination of plasma indoles, including indoxyl sulfate (3-INDS), indole-3-acetic acid (IAA), indole-3-propionate (IPA), indole (IND) and 3-methylindole (3-MI). Diethyl ether and ethyl acetate were selected as the mixed extractant for the sample preparation. The separation was carried out on a Shim-Pack VP-ODS column (150 × 4.6 mm, 4.6 µm) with the mobile phase composed of 10 mmol/L sodium dihydrogen phosphate/methanol (40:60, v/v). The excitation and emission wavelengths were set at 280 and 355 nm, respectively. The linearities in plasma were obtained in the range of 1.56–400.0 μmol/L for 3-INDS, 0.312–10.0 μmol/L for IAA, 0.125–6.00 μmol/L for IPA, 6.25–400.0 nmol/L for IND, and 1.56–400.0 nmol/L for 3-MI, respectively. The coefficients of variation (CVs) for each analyte of the intra-day and inter-day precisions were within 4.0 and 5.2%, respectively. The recoveries were in the range of 90.1–109.3%. This sensitive and accurate method was applied to analyze plasma indoles for the diagnostic of depression in the patients with polycystic ovary syndrome (PCOS). Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"59682535","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 : 2022-02-25DOI: 10.1080/10826076.2022.2095402
E. Oliphant, Trusha J. Purohit, J. Alsweiler, C. McKinlay, S. Hanning
Abstract A clinical trial is currently underway to examine the efficacy of using caffeine citrate to prevent intermittent hypoxemia in late preterm neonates. Determining caffeine concentration using saliva in this population would be preferable as it is less invasive than plasma sampling, but a suitable method of analysis is required. This paper presents the development and validation of a rapid, efficient and reproducible stability-indicating high-performance liquid chromatography (HPLC) method and extraction protocol for the quantification of caffeine present in saliva. The stability of extemporaneously prepared caffeine citrate solutions (at 20–25 °C) was determined, along with the stability of caffeine spiked saliva samples (at 20–25 and 2–8 °C), to ensure the suitability of the developed method in the analysis of clinical trial samples. Protein precipitation using acetonitrile ensured the complete removal of salivary proteins and resulted in extraction recovery of ≥95% for all samples. The HPLC assay following extraction was linear (R 2>0.99) over the range 0.3–50 µg/mL (lower limit of quantification 0.3 µg/mL). The accuracy of the quality control samples was 94–100% and the relative standard deviation (RSD) was <7% for all samples. Caffeine-spiked saliva samples were stable for three freeze-and-thaw cycles pre-extraction and up to 72 hr post-extraction. The extraction and HPLC methods described were thus suitable for the analysis of clinical trial samples from the Latte Dosage Trial. All caffeine solutions were physically and chemically stable, with concentrations at the end of the three-month test period being within 4% of the baseline concentrations, indicating appropriateness for use as clinical trial medications. Graphical Abstract
{"title":"Validation and application of a simple and rapid stability-indicating liquid chromatographic assay for the quantification of caffeine from human saliva","authors":"E. Oliphant, Trusha J. Purohit, J. Alsweiler, C. McKinlay, S. Hanning","doi":"10.1080/10826076.2022.2095402","DOIUrl":"https://doi.org/10.1080/10826076.2022.2095402","url":null,"abstract":"Abstract A clinical trial is currently underway to examine the efficacy of using caffeine citrate to prevent intermittent hypoxemia in late preterm neonates. Determining caffeine concentration using saliva in this population would be preferable as it is less invasive than plasma sampling, but a suitable method of analysis is required. This paper presents the development and validation of a rapid, efficient and reproducible stability-indicating high-performance liquid chromatography (HPLC) method and extraction protocol for the quantification of caffeine present in saliva. The stability of extemporaneously prepared caffeine citrate solutions (at 20–25 °C) was determined, along with the stability of caffeine spiked saliva samples (at 20–25 and 2–8 °C), to ensure the suitability of the developed method in the analysis of clinical trial samples. Protein precipitation using acetonitrile ensured the complete removal of salivary proteins and resulted in extraction recovery of ≥95% for all samples. The HPLC assay following extraction was linear (R 2>0.99) over the range 0.3–50 µg/mL (lower limit of quantification 0.3 µg/mL). The accuracy of the quality control samples was 94–100% and the relative standard deviation (RSD) was <7% for all samples. Caffeine-spiked saliva samples were stable for three freeze-and-thaw cycles pre-extraction and up to 72 hr post-extraction. The extraction and HPLC methods described were thus suitable for the analysis of clinical trial samples from the Latte Dosage Trial. All caffeine solutions were physically and chemically stable, with concentrations at the end of the three-month test period being within 4% of the baseline concentrations, indicating appropriateness for use as clinical trial medications. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47459777","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 : 2022-02-25DOI: 10.1080/10826076.2022.2109669
An-Ping Li, Yan-Ping Shi
Abstract Farfarae Flos, a frequently used traditional herbal medicine with outstanding antitussive and anti-asthmatic effects. As an herbal rich in natural flavonoids, the quantitative determination of multi-flavonoids can be helpful to comprehensively evaluate its quality. Herein, an efficient, sensitive and accurate UHPLC-MS/MS method was established to simultaneous determinate nine flavonoids (rutin, hyperin, kaempferol-3-O-rutinoside, hesperidin, luteolin, quercetin, kaempferol, apigenin, and genkwanin) in Farfarae Flos. The calibration curves of the analytes had good linearity (R2 ≥ 0.9991). Limit of detection and limit of quantitation of each analytes was in the range of 1.06 × 10−5–2.26 × 10−3 μg·mL−1 and 3.52 × 10−5–7.53 × 10−3 μg·mL−1. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.71% and 2.94%. The RSD of repeatability test and stability test was less than 2.35% and 2.56%. The recovery rates were in the range of 95.27%–103.60%. The method was further applied to determinate 40 batches of samples that derived from different plant parts and with definite habitat. The results of chemometric statistical analysis showed that, firstly, the content of flavonoids can effectively reflect the differences between traditional medicinal parts and impurities. Secondly, the geographical environment has impact on the quality. In conclusion, this study provides a valuable methodological reference for the quality evaluation and further resource utilization of Farfarae Flos. Graphical Abstract
{"title":"Simultaneous determination of nine flavonoids in Farfarae Flos by UHPLC-MS/MS and its application in quality evaluation","authors":"An-Ping Li, Yan-Ping Shi","doi":"10.1080/10826076.2022.2109669","DOIUrl":"https://doi.org/10.1080/10826076.2022.2109669","url":null,"abstract":"Abstract Farfarae Flos, a frequently used traditional herbal medicine with outstanding antitussive and anti-asthmatic effects. As an herbal rich in natural flavonoids, the quantitative determination of multi-flavonoids can be helpful to comprehensively evaluate its quality. Herein, an efficient, sensitive and accurate UHPLC-MS/MS method was established to simultaneous determinate nine flavonoids (rutin, hyperin, kaempferol-3-O-rutinoside, hesperidin, luteolin, quercetin, kaempferol, apigenin, and genkwanin) in Farfarae Flos. The calibration curves of the analytes had good linearity (R2 ≥ 0.9991). Limit of detection and limit of quantitation of each analytes was in the range of 1.06 × 10−5–2.26 × 10−3 μg·mL−1 and 3.52 × 10−5–7.53 × 10−3 μg·mL−1. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.71% and 2.94%. The RSD of repeatability test and stability test was less than 2.35% and 2.56%. The recovery rates were in the range of 95.27%–103.60%. The method was further applied to determinate 40 batches of samples that derived from different plant parts and with definite habitat. The results of chemometric statistical analysis showed that, firstly, the content of flavonoids can effectively reflect the differences between traditional medicinal parts and impurities. Secondly, the geographical environment has impact on the quality. In conclusion, this study provides a valuable methodological reference for the quality evaluation and further resource utilization of Farfarae Flos. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2022-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48775011","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}
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