Journal of Liquid Chromatography & Related Technologies最新文献_第10页

Rapid screening of undeclared hypoglycemics in counterfeit herbal antidiabetic products using HPTLC-MS 利用HPTLC-MS快速筛选假冒中药降糖药中未申报的降糖药

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-05-09 DOI: 10.1080/10826076.2023.2173608

Diva C. Purohit, Jigna Vadalia, H. Joshi, Udaykumar G. Vegad

{"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":"45 1","pages":"100 - 106"},"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}

引用次数: 1

UHPLC-APCI-TQ-MS analytical method to quantify nitrosamine impurities in the commercial formulation of metformin and glipizide UHPLC-APCI-TQ-MS分析方法定量二甲双胍和格列吡嗪市售制剂中亚硝胺类杂质

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-05-09 DOI: 10.1080/10826076.2022.2126856

Ravi Solanki, C. Patel, Ravi Patel, Anujkumar Maradiya, Shalin Parikh, Bhavinkumar Gayakvad

{"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":"45 1","pages":"84 - 93"},"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}

引用次数: 1

Non-pharmacological interventions for tobacco cessation: A systematic review of existing practices and their effectiveness. 非药物戒烟干预：对现有做法及其有效性的系统回顾。

IF 1 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-03-25 DOI: 10.4081/monaldi.2022.2229

Shyam Kanhaiya Saroj, Tushti Bhardwaj

{"title":"Non-pharmacological interventions for tobacco cessation: A systematic review of existing practices and their effectiveness.","authors":"Shyam Kanhaiya Saroj, Tushti Bhardwaj","doi":"10.4081/monaldi.2022.2229","DOIUrl":"10.4081/monaldi.2022.2229","url":null,"abstract":"<p><p>Smoking tobacco is associated with lung cancer and other life-threatening diseases which requires serious action to curb it. Tobacco cessation interventions are available as pharmacological and non-pharmacological methods or a combination of both. The present review examines the effectiveness of the existing non-pharmacological tobacco cessation interventions and synthesizes the result for the future development of drug-free treatment in the community for tobacco cessation. The literature search was conducted in August 2020, using two electronic databases (PubMed and JSTOR), with search terms: ['tobacco cessation' OR 'smoking cessation'] AND ['intervention'] which included studies published during 2010 and 2020 (till 31st July 2020). All studies were limited to English language, human participants and excluded patients with comorbidities. A total of 2,114 publications were retrieved out of which 11 articles were reviewed. On the basis of intervention used in reviewed studies, we categorized them into seven categories: i. incentive-based intervention, ii. exercise based, iii. telephone-based proactive counselling, iv. mobile phone SMS (Short Message Service) based, v. smartphone app (application) based, vi. web-based intervention, vii. self-help material. Incentives were provided in most of the studies to maintain the retention rate and motivate the participants for completing follow-up. Non-pharmacological interventions for tobacco cessation include a combination of various elements. Our findings suggest that behavioural counselling is one of the most important elements of any non-pharmacological intervention. In addition to behaviour counselling, yoga and exercises along with self-help material, video and phone counselling may have higher efficacy. Thus, practicing non-pharmacological interventions may also increase the cessation rate and reduce the tobacco use burden.</p>","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"6 1","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-03-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81171658","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}

引用次数: 0

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 使用顺序注射毛细管电泳非接触式电导检测（SI-CE-C4D）自动在线监测三苯氧胺耐药MCF-7细胞中的乳酸和丙酮酸盐及其与MCT1和MCT4基因表达的相关性

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2098760

Ala A. Alhusban, Lama A. Hamadneh, Aliaa I. Shallan, O. Tarawneh

{"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":"45 1","pages":"18 - 27"},"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}

引用次数: 0

Simultaneous determination of plasma indoles by HPLC with fluorescence detection: Application in polycystic ovary syndrome patients with/without depression 荧光高效液相色谱法同时测定血浆吲哚:在多囊卵巢综合征伴/不伴抑郁患者中的应用

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2124267

Ke Yang, Ying Chen, Zhang Xiaoqing, Q. Zhen, Wenwu Gui, Yanna Ban, Yifan He, Shengnan Pan, Min Ding

{"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":"45 1","pages":"44 - 50"},"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}

引用次数: 0

Validation and application of a simple and rapid stability-indicating liquid chromatographic assay for the quantification of caffeine from human saliva 快速稳定指示液相色谱法定量人唾液中咖啡因的验证与应用

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2095402

E. Oliphant, Trusha J. Purohit, J. Alsweiler, C. McKinlay, S. Hanning

{"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":"45 1","pages":"10 - 17"},"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}

引用次数: 2

Simultaneous determination of nine flavonoids in Farfarae Flos by UHPLC-MS/MS and its application in quality evaluation UHPLC-MS/MS法同时测定法拉中9种黄酮类化合物及其在质量评价中的应用

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2109669

An-Ping Li, Yan-Ping Shi

{"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":"45 1","pages":"28 - 43"},"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}

引用次数: 0

Identification and characterization of novel hydrolytic degradation products of netarsudil by LC-Q-TOF-MS/MS: In silico toxicity prediction 用LC-Q-TOF-MS/MS鉴定奈沙地尔新型水解降解产物及其在硅毒性预测中的应用

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2089999

Surapuraju Pavan Kumar Raju, Juturu Ravindra Reddy

{"title":"Identification and characterization of novel hydrolytic degradation products of netarsudil by LC-Q-TOF-MS/MS: In silico toxicity prediction","authors":"Surapuraju Pavan Kumar Raju, Juturu Ravindra Reddy","doi":"10.1080/10826076.2022.2089999","DOIUrl":"https://doi.org/10.1080/10826076.2022.2089999","url":null,"abstract":"Abstract A forced degradation study on novel glaucoma drug netarsudil was performed as per ICH and WHO guidelines. All the degradation products were separated from the drug on a C-18 column utilizing ammonium acetate buffer (10 mM, pH 4.90) as a mobile phase-A and acetonitrile: methanol (70:30) v/v as mobile phase-B, by employing gradient elution mode. The injection volume was 10 µL with a 0.8 mL/min flow rate. The detection wavelength was 245 nm and the study was executed at a constant column temperature of 40 °C. Initially, the mass fragmentation pathway of the drug was postulated followed by characterization of degradation products from LC-MS-TOF/MS data. This was followed by LC-MS/TOF studies on the degradation products. Significant degradation was witnessed in alkaline and acidic conditions whereas no signification decline in the drug was observed in other decomposition environments. A total of four degradation products were formed and characterized with the aid of high-resolution mass spectrometry. The mechanistic pathway of formation of all DPs from netarsudil is established. In addition, comparative toxicity properties of the drug and degradation products were established using the online web server Pro Tox II. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"45 1","pages":"1 - 9"},"PeriodicalIF":1.3,"publicationDate":"2022-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44965313","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}

引用次数: 1

Indexation of mixed mode adsorbents using low temperature nitrogen adsorption and Silica-C18 surface energy scale 低温氮吸附和Silica-C18表面能标度对混合模式吸附剂的指数化

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2021-12-14 DOI: 10.1080/10826076.2022.2110117

Dinah Lee, Y. Kazakevich

{"title":"Indexation of mixed mode adsorbents using low temperature nitrogen adsorption and Silica-C18 surface energy scale","authors":"Dinah Lee, Y. Kazakevich","doi":"10.1080/10826076.2022.2110117","DOIUrl":"https://doi.org/10.1080/10826076.2022.2110117","url":null,"abstract":"Abstract Mixed-mode chromatography is becoming increasingly popular in pharmaceutical and biopharmaceutical applications due to its unique selectivity and retention of a variety of compounds. Mixed-mode chromatography is a chromatographic method in which solutes interact with stationary phase through more than one interaction mode or mechanism. It is because of these complex interactions, however, that it is difficult to predict chromatographic behavior of analytes on mixed-mode columns. Characterization of different mixed-mode columns on the basis of surface energy characteristics has not been explored. In this study, different ratios of porous silica (Axia Luna 5 µm Silica – Phenomenex), and C18 (Axia Luna 5 µm C18 – Phenomenex), single mode adsorbents were blended in various ratios and analyzed by Low Temperature Nitrogen Adsorption (LTNA). A variety of commercially available mixed mode columns were also unpacked and the materials were analyzed by LTNA. Adsorption isotherms, surface area, and BET constants were obtained for all the blended materials in various ratios and the mixed-mode materials. A linear relationship between the BET C-constant and the blend ratio of silica has been observed. The results from the commercial mixed mode packing material showed similar surface energy characteristics to single mode C18 materials. This data suggests that the BET C-constant maybe a viable parameter that can be used to characterize mixed-mode columns on the basis of surface energy. Utilizing this surface energy scale in conjunction with the study of retention behaviors on mixed-mode material could lead to improvements in the understanding of method development on mixed-mode columns, allow the comparison of commercialized mixed-mode columns, and even predict retention behavior of an analyte in mixed-mode columns. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"44 1","pages":"880 - 887"},"PeriodicalIF":1.3,"publicationDate":"2021-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49431578","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}

引用次数: 0

Separation optimization and quantitative analysis of phytoestrogens employing reverse-phase high-performance liquid chromatography with UV-VIS detection 紫外可见反相高效液相色谱法优化植物雌激素分离及定量分析

IF 1.3 4区化学

Journal of Liquid Chromatography & Related Technologies Pub Date : 2021-12-14 DOI: 10.1080/10826076.2022.2110118

Michael Payette, Marta R. M. Lima, W. M. Coleman, M. Ashraf-Khorassani

{"title":"Separation optimization and quantitative analysis of phytoestrogens employing reverse-phase high-performance liquid chromatography with UV-VIS detection","authors":"Michael Payette, Marta R. M. Lima, W. M. Coleman, M. Ashraf-Khorassani","doi":"10.1080/10826076.2022.2110118","DOIUrl":"https://doi.org/10.1080/10826076.2022.2110118","url":null,"abstract":"Abstract The effect of different acidic modifiers on the separation of seven selected phytoestrogens by reverse-phase high-performance liquid chromatography has been described. Variation in the hydrocarbon chain length of organic acids as represented by acetic acid, propanoic acid, iso-butyric acid, and n-butyric acid as additives to the mobile phase had minimal effect on the separation of phytoestrogens but notably reduced sample turnaround times relative to the turnaround time linked with formic acid. Two different C18 columns were evaluated in attempts of optimize the phytoestrogen separations. Formic acid as a modifier in the mobile phase and an Atlantis C18 column provided the best overall separation at optimum gradient conditions. A higher acid concentration in the mobile phase did not improve the phytoestrogen separation. Higher column temperature (40 °C) provided an improved separation. Finally, the optimized method was used to quantify different phytoestrogens in selected different botanical samples. For this purpose, both internal and external standard methods were compared to obtain the quantitative results. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"44 1","pages":"888 - 896"},"PeriodicalIF":1.3,"publicationDate":"2021-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46869503","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}

引用次数: 1