Journal of chromatographic science最新文献_第7页

Separation of Three Polar Compounds with Similar Polarities from Swertia mussotii by a Combination of Two Counter-Current Chromatography Modes. 两种逆流色谱法联合分离獐牙菜中极性相近的3种极性化合物。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-14 DOI: 10.1093/chromsci/bmaf006

Hongmei Li, Tao Chen, Cheng Shen, Shuo Wang, Juyuan Luo, Zhibo Song, Yumei Ma, Aijing Li, Weihang Lu, Hailun Feng, Yulin Li

{"title":"Separation of Three Polar Compounds with Similar Polarities from Swertia mussotii by a Combination of Two Counter-Current Chromatography Modes.","authors":"Hongmei Li, Tao Chen, Cheng Shen, Shuo Wang, Juyuan Luo, Zhibo Song, Yumei Ma, Aijing Li, Weihang Lu, Hailun Feng, Yulin Li","doi":"10.1093/chromsci/bmaf006","DOIUrl":"10.1093/chromsci/bmaf006","url":null,"abstract":"Separation of polar compounds especially with similar polarities is challenging. In the present study, three polar compounds with similar polarities, including gentiopicroside, sweroside and mangiferin, have been successfully separated from Swertia mussotii by a combination of two counter-current chromatography modes. With the selected solvent system of ethyl acetate/n-butanol/water (8/2/10, v/v), a continuous injection mode was firstly employed. As a result, 10.4 g of mangiferin with purity higher than 98% and 8 g of Peak I mainly composed of gentiopicroside and sweroside could be easily obtained from 24 g of the sample by counter-current chromatography through eight injections. Then, a recycling counter-current chromatography mode was introduced for the separation of gentiopicroside and sweroside. Through six cycles, 5.3 g of gentiopicroside and 0.8 g of sweroside with purity higher than 98% were obtained from 8 g of Peak I. The research provides a reference for the large-scale separation of polar compounds with similar polarities.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143006231","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

Method Validation for Estimation of Imidacloprid and its Metabolites in Maize and Soil by LCMS-MS. 方法用液相色谱-质谱法测定玉米和土壤中吡虫啉及其代谢物的方法验证。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-14 DOI: 10.1093/chromsci/bmaf005

Sandeep Kaur, Smriti Sharma, Balpreet K Kang

{"title":"Method Validation for Estimation of Imidacloprid and its Metabolites in Maize and Soil by LCMS-MS.","authors":"Sandeep Kaur, Smriti Sharma, Balpreet K Kang","doi":"10.1093/chromsci/bmaf005","DOIUrl":"10.1093/chromsci/bmaf005","url":null,"abstract":"Validation of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was performed for estimation of imidacloprid (IM) and its metabolites in maize leaves, immature kernels, mature kernels, stalk, and soil using liquid chromatograph tandem mass spectrometry, coupled with electrospray ionization. The extraction in different matrices of maize and soil was performed using acetonitrile +0.1% formic acid followed by clean-up with primary secondary amine sorbent and anhydrous magnesium sulfate. The method was validated in terms of selectivity, linearity, limit of detection, limit of quantification, matrix effect, ion ratios, quality control, robustness, accuracy, and precision. The validation of all parameters was done in accordance with European Commission's Directorate-General for Health and Food Safety (DG SANTE) guidelines. A linear relationship with high correlation coefficients R2 > 0.99 was obtained for solvents and different matrices viz., maize leaves, immature kernels, mature kernels, stalk, and soil. The recovery and relative standard deviations were ˃78% and ˂5.4%, respectively. This method permits a simple, sensitive, accurate, cost-effective, precise, and rapid extraction of IM and its metabolites from maize leaves, immature kernels, mature kernels, stalks, and soil. This can help the residue analysts to address effective residue estimation, regular monitoring of residues and can also aid in the regulatory and food safety concerns about the usage of IM in maize.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143006213","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

A New Headspace Gas Chromatography Method for Determination of Ethylene Oxide and Dioxane in Polyethylene Glycols. 顶空气相色谱法测定聚乙二醇中环氧乙烷和二恶烷的新方法。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-14 DOI: 10.1093/chromsci/bmaf011

Gayan Premaratne, Andrew McAdoo, Jingzhi Tian, Abu Rustum

{"title":"A New Headspace Gas Chromatography Method for Determination of Ethylene Oxide and Dioxane in Polyethylene Glycols.","authors":"Gayan Premaratne, Andrew McAdoo, Jingzhi Tian, Abu Rustum","doi":"10.1093/chromsci/bmaf011","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf011","url":null,"abstract":"In this paper, a new headspace gas chromatography (HSGC) method has been developed for the determination of ethylene oxide (EO) and 1,4-Dioxane (Dioxane) in bulk lots of polyethylene glycols (PEG). PEG samples are dissolved in dimethyl sulfoxide, heated in a headspace oven maintained at 90°C for 10 min and then injected into the GC system for analysis. Analytes are separated through a thermal gradient elution from 36 to 240°C on an Agilent DB-624 column (60 m × 0.53 mm diameter, film thickness 3.00 μm). The carrier gas is helium and detector is flame ionization detector. Total run time of the new HSGC method is about 18 min. In the new HSGC method, other common residual solvents present in PEGs such as methanol (MeOH), methyl formate (MF) and acetyl aldehyde (Acetal) are also sufficiently separated from EO and Dioxane peaks. In the HSGC methods prescribed in USP monograph <228> and EP monograph <2.4.25>, EO co-elutes with MF. The new HSGC method was successfully validated according to current ICH/VICH guidelines and was found to be specific, linear, accurate, precise, robust and sensitive. This HSGC method is fast and quality control (QC) friendly and suitable for routine analysis for the determination of EO and Dioxane in bulk batches of PEGs in QC laboratories.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143364960","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

Development and Validation of a New High-Performance Liquid Chromatography-Ultraviolet Assay for Quantification of Mitoxantrone in Plasma of BALB/c-nu Mice. 开发并验证用于 BALB/c-nu 小鼠血浆中米托蒽醌定量的新型高效液相色谱-紫外检测法

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmae007

Yanru Tao, Hua Zhao, Yujie Xiang, Jin Li, Yanting Li, Jiangling Hu, Hongmei Wang, Xinhui Jiang

{"title":"Development and Validation of a New High-Performance Liquid Chromatography-Ultraviolet Assay for Quantification of Mitoxantrone in Plasma of BALB/c-nu Mice.","authors":"Yanru Tao, Hua Zhao, Yujie Xiang, Jin Li, Yanting Li, Jiangling Hu, Hongmei Wang, Xinhui Jiang","doi":"10.1093/chromsci/bmae007","DOIUrl":"10.1093/chromsci/bmae007","url":null,"abstract":"The concentration of mitoxantrone in the blood of mice was determined by a high-performance liquid chromatography-ultraviolet method with aloe-emodin as the internal standard. The separation was performed on a Hypersil BDS2 column (4.6 × 250 mm, 5 μm) as the analytical column, the mobile Phase A was acetonitrile, and B was 20-mM potassium dihydrogen phosphate (adding 1% triethylamine and adjusting the pH to 2.8 with phosphoric acid) and 4.6-mM sodium octyl sulfonate. The flow rate was 1.0 mL·min-1, the detection wavelength was 243 nm, the column temperature is 25 ± 5°C and the injection amount was 20 μL. Finally, the linear range of mitoxantrone was 5-200 μg·mL-1, and the correlation coefficient was r = 0.9999. The recovery rate of the method was 91.93-105.5%, and the extraction recovery rate was 91.45-105.5%. The intraday precision and interday precision were <3.29% (limit of detection = 0.3 μg·mL-1). The HPLC method established in this paper was simple, rapid, sensitive and accurate, and can be used to determine the content of mitoxantrone in mouse plasma after tail vein injection.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140140323","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

Stability-Indicating Liquid Chromatographic Method Development for the Simultaneous Determination of Amitriptyline Hydrochloride and Propranolol Hydrochloride in Tablet Dosage Form. 稳定性指示液相色谱法同时测定片剂中盐酸阿米替林和盐酸心得洛尔的含量。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmae060

Obi Reddy Chabala, Simon Haque Md, Durai Ananda Kumar Thirumoorthy

{"title":"Stability-Indicating Liquid Chromatographic Method Development for the Simultaneous Determination of Amitriptyline Hydrochloride and Propranolol Hydrochloride in Tablet Dosage Form.","authors":"Obi Reddy Chabala, Simon Haque Md, Durai Ananda Kumar Thirumoorthy","doi":"10.1093/chromsci/bmae060","DOIUrl":"10.1093/chromsci/bmae060","url":null,"abstract":"The combination of the tricyclic antidepressant amitriptyline hydrochloride (AMH) and the non-selective beta-adrenergic blocker propranolol hydrochloride (PPH) is used for migraine prophylaxis. Higher doses of AMH trigger cardiac arrhythmias, anxiety, tachycardia, convulsions, hyperglycemia and anticholinergic side effects. The combined dosage formulation of AMH and PPH leads to drug-drug interactions; causes sedation, xerostomia, dysuria, insomnia and bradycardia; and results in patient non-compliance. The quantification of AMH and PPN becomes essential, especially for combination formulations, in addition to regular quality control to avoid clinical issues. Considering these facts into account, the reverse-phase -high-performance liquid chromatography (RP-HPLC) method was developed in accordance with International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use Q2(R1) guidelines for the simultaneous determination of AMH and PPH. The HPLC separation was performed on an HPLC system (Shimadzu, Japan, Prominence I series 2030C) using a Shimadzu Shim-Pack GIST C18 column (100 mm × 4.6 mm, 5 μ), which was equipped with an ultraviolet detector at the isosbestic point 238 nm. The mixture of acetonitrile and orthophosphoric acid (pH 3.5) in a ratio of 35:65 v/v with a flow rate of 0.75 mL/min was used as the mobile phase. The regression coefficients of AMH (r2 > 0.998) and PPH (r2 > 0.999) show good linearity between peak areas and drug concentration ranges. The limits of detection (AMH = 0.67 μg/mL, PPH = 0.67 μg/mL) and limits of quantification (AMH = 2.04 μg/mL, PPH = 2.05 μg/mL) demonstrated the higher detection sensitivity of the proposed method.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142894943","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

Bioanalytical Method Development and Validation of Doxorubicin and Lapatinib in Rat Plasma Using UHPLC-HESI-LTQ-MS. 利用 UHPLC-HESI-LTQ-MS 对大鼠血浆中多柔比星和拉帕替尼的生物分析方法进行开发和验证

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmad090

Shaik Khaja Moinuddin, Pirangi Srikanth, Parul Sharma, Sukhendu Nandi

{"title":"Bioanalytical Method Development and Validation of Doxorubicin and Lapatinib in Rat Plasma Using UHPLC-HESI-LTQ-MS.","authors":"Shaik Khaja Moinuddin, Pirangi Srikanth, Parul Sharma, Sukhendu Nandi","doi":"10.1093/chromsci/bmad090","DOIUrl":"10.1093/chromsci/bmad090","url":null,"abstract":"Cancer is considered a silent killer. The complexity of cancer makes it earn that title. So far there are only a few approaches to treat cancer. Among them, chemotherapy is considered the best approach. Many chemotherapeutical compounds are commercially available in the market. Among them, doxorubicin (DOX) and lapatinib (LAP) are considered blockbuster molecules. However, DOX suffers from poor bioavailability and exhibits cardiotoxicity. Interestingly, a fixed dose combination of DOX and LAP significantly decreases the cardiotoxic effect of DOX. To enhance the oral bioavailability of DOX and to avail the synergistic effect of LAP, many formulations have been made. To quantify both compounds in any formulation or biological matrix, an Liquid chromatography-Mass Spectrometry (LC-MS) method is required. In this present study, a simple and rapid Ultra High-Performance Liquid Chromatography - Heated Electron Spray Ionization - Mass Spectrometry (UHPLC-HESI-MS) bioanalytical method was developed. The developed method was validated as per the regulatory guidelines. The validated bioanalytical method had a lower limit of quantification of 0.75 ng. A simple protein precipitation technique was optimized to extract the compounds from the rat plasma. All the validation parameters were found to be within the limits as per the regulatory guidelines. A novel and rapid analytical method was successfully developed and validated. This developed method can be used to quantify the DOX and LAP in any formulation and biological matrix.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138804829","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

Structural Elucidation of Novel Degradation Impurities of Ibrutinib in Ibrutinib Tablets Using Preparative Chromatography, LCMS, HRMS and 2D NMR Techniques. 利用制备色谱、LCMS、HRMS 和 2D NMR 技术阐明伊布替尼片中伊布替尼新型降解杂质的结构。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmae002

Rajender Reddy Yerla, Surendrababu Manubolusurya, Saravanakumar Meganathan, Veerababu Madalapu, Gopal Vaidyanathan

{"title":"Structural Elucidation of Novel Degradation Impurities of Ibrutinib in Ibrutinib Tablets Using Preparative Chromatography, LCMS, HRMS and 2D NMR Techniques.","authors":"Rajender Reddy Yerla, Surendrababu Manubolusurya, Saravanakumar Meganathan, Veerababu Madalapu, Gopal Vaidyanathan","doi":"10.1093/chromsci/bmae002","DOIUrl":"10.1093/chromsci/bmae002","url":null,"abstract":"Ibrutinib is an orally administered compound that functions as an irreversible covalent inhibitor of the Bruton tyrosine kinase, an essential element in multiple cellular processes including B-cell differentiation, proliferation, migration, survival and apoptosis. The compound has been found to demonstrate efficacy against a range of B-cell malignancies. The drug product is available in oral tablet and capsule formulations. The drug degradation profiles of tablets dosage form were assessed in accordance with regulatory guidelines. The results indicate that the drug substance is susceptible to alkaline and oxidative stress. The oxidation degradation led to the identification of three significant unknown degradation impurities. The three compounds were isolated through the application of preparative liquid chromatography, and their structures were determined using analytical techniques such as liquid chromatography-mass spectrometry, high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy. Utilizing structural elucidation data, predictions were made regarding the composition of impurities, revealing them to be novel degradation impurities that bear structural resemblance to ibrutinib. Additionally, potential pathways for the formation of the impurities were proposed.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139712296","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 D and L Enantiomers of 2-Hydroxyglutarate by UHPLC-MS/MS Method in Human Biological Fluids and its Clinical Application. 超高效液相色谱-质谱/质谱法同时测定人体生物液体中2-羟基戊二酸D和L对映体及其临床应用

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmae013

Xiaoqing Li, Yunhai Bo, Le Le, Fen Yang

{"title":"Simultaneous Determination of D and L Enantiomers of 2-Hydroxyglutarate by UHPLC-MS/MS Method in Human Biological Fluids and its Clinical Application.","authors":"Xiaoqing Li, Yunhai Bo, Le Le, Fen Yang","doi":"10.1093/chromsci/bmae013","DOIUrl":"10.1093/chromsci/bmae013","url":null,"abstract":"2-hydroxyglutarate has limited abundance in normal tissues but a high level under certain pathologic conditions. To clarify the diagnostic value of two chiral isomers of 2-hydroxyglutarate in plasma and urine of Chinese cancer patients, an ultra-high performance liquid chromatography-tandem mass spectrometric method was developed for simultaneous quantification of D-/L-2-hydroxyglutarate. The selected D-/L-2-hydroxyglutarate-d5 as internal standards were added to samples before the SPE on Waters Oasis® MAX 96-Well plate (30 μm, 60 mg). A derivatization step with (+)-O,O'-diacetyl-L-tartaric anhydride permitted the chromatography separation of D-/L-2-hydroxyglutarate on an ACQUITY UPLC-HSS T3 column (50 × 2.1 mm, i.d. 1.8 μm) with acetonitrile and water (containing 0.1% formic acid and 10 mmol ammonium acetate) as the mobile phase. The calibration curves showed good linearity (R ≥ 0.99) over the concentration ranges of 200-5,000 ng/mL and 500-20,000 ng/mL for analysis of D-/L-2-hydroxyglutarate in plasma and urine samples, respectively. Intra- and inter-run precision were ≤ 12.33%, and the accuracy was within the range of -10.44 to 13.90%. This method was further successfully applied to clinical sample analysis in isocitrate dehydrogenase 1/2 mutated Chinese cancer patients.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140326637","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

UPLC-MS/MS Combined with Microdialysis for Determination of Two Active Components of Chuanxiong Rhizoma Extracts in Rat Brain: Application in Pharmacokinetic Study. 超高效液相色谱-质谱联用微透析法测定川芎提取物中两种有效成分在大鼠脑中的药动学研究

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmae059

Yu Wang, Liang Jin, Xinhua Liu, Bing Shu, Jia Xu, Lingyun Pan

{"title":"UPLC-MS/MS Combined with Microdialysis for Determination of Two Active Components of Chuanxiong Rhizoma Extracts in Rat Brain: Application in Pharmacokinetic Study.","authors":"Yu Wang, Liang Jin, Xinhua Liu, Bing Shu, Jia Xu, Lingyun Pan","doi":"10.1093/chromsci/bmae059","DOIUrl":"10.1093/chromsci/bmae059","url":null,"abstract":"Chuanxiong Rhizoma (Chuanxiong), a traditional Chinese medicine, has been widely used to treat various nervous and cardiovascular system-related conditions. Its active components, senkyunolide A (SA) and 3-n-butylphthalide (NBP), have been proven effective in treating nervous system diseases. A new method was established based on microdialysis coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to estimate the concentrations of these components in brain extracellular fluid. Chromatographic separation was achieved using an Acquity UPLC BEH C8 column (2.1 × 100 mm, 1.7 μm) with acetonitrile and 0.1% formic acid as mobile phase. The calibration curves of SA and NBP were linear in the concentration ranges of 0.25-100.00 and 0.12-48.00 ng/mL, respectively, with a correlation coefficient above 0.9992. All validation parameters, including intra- and inter-day precision, accuracy, matrix effect and stability, were within the acceptance limits of bioanalytical guidelines. The validated method was successfully applied to study the pharmacokinetics of SA and NBP in rat brain microdialysis after oral administration of Chuanxiong extracts. The results showed that both components penetrated the brain and reached maximum concentrations in the microdialysates of 72.31 and 9.93 ng/mL at 1.50 and 1.58 h, respectively.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142854094","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

Green Chromatographic Assay of Toxic Impurities of Cyproheptadine: In Silico Toxicity Profiling. 绿色色谱法检测赛庚啶的有毒杂质：In Silico 毒性分析。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-01-09 DOI: 10.1093/chromsci/bmae004

Raghda A Emam, Aml A Emam

{"title":"Green Chromatographic Assay of Toxic Impurities of Cyproheptadine: In Silico Toxicity Profiling.","authors":"Raghda A Emam, Aml A Emam","doi":"10.1093/chromsci/bmae004","DOIUrl":"10.1093/chromsci/bmae004","url":null,"abstract":"Cyproheptadine (CYP) is an antihistaminic and anti-serotonin drug used to improve the clinical course of hospitalized patients severely affected by COVID-19 and requiring supplemental oxygen. Thin layer chromatography (TLC)-densitometry method was developed and validated for the estimation of CYP and its impurity, dibenzosuberone and its degradation product: 10, 11-dihydroxy-dibenzosuberone. The toxicity profiles of CYP impurity and degradation product were studied and the in silico data, using pre-ADMET software, proved their toxicity. A developing system of hexane: methanol: ethyl acetate: formic acid: triethylamine (8:1:1:0.05:0.1, by volume) was used with densitometric scanning at 245 nm. International Conference of Harmonization guidelines were obeyed for method validation. The proposed method was applied on CYP pharmaceutical formulation whose results showed no significant difference from results of the reported chromatographic method regarding accuracy and precision. Method's greenness was evaluated by analytical Eco scale, Green Analytical Procedure Index, and Analytical greenness approach tools. The developed method can be applied for safety check analysis of CYP containing formulations and detection and even quantification of its related toxic components in quality control laboratories at high sensitivity up to 20-fold than the reported chromatographic method.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139972015","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