Journal of chromatographic science最新文献_第9页

Determination of Volatile Halogenated Hydrocarbons in Drinking and Environmental Waters by Headspace Gas Chromatography. 利用顶空气相色谱法测定饮用水和环境水体中的挥发性卤代烃。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-12-11 DOI: 10.1093/chromsci/bmae047

Weifei Mo, Hongmei Hu, Jiangmei Yu, Tongtong Zhang, Qin Liu, Mengyan Li, Xiaoning Zhang, Tiejun Li, Yuanming Guo

{"title":"Determination of Volatile Halogenated Hydrocarbons in Drinking and Environmental Waters by Headspace Gas Chromatography.","authors":"Weifei Mo, Hongmei Hu, Jiangmei Yu, Tongtong Zhang, Qin Liu, Mengyan Li, Xiaoning Zhang, Tiejun Li, Yuanming Guo","doi":"10.1093/chromsci/bmae047","DOIUrl":"10.1093/chromsci/bmae047","url":null,"abstract":"Volatile halogenated hydrocarbons (VHHs) are annually produced and released into the environment, posing a threat to public health. In this study, a simple, rapid, sensitive and automated method based on headspace and gas chromatography (GC) with electron-capture detection was described for the determination of VHHs in different concentration levels in water samples. The proposed headspace GC method was initially optimized, and the optimum experimental conditions found were 10-mL water sample containing 20% w/v sodium chloride placed in a 20-mL vial and stirred at 60°C for 35 min, and then 14 VHHs were well separated on DB-35 MS capillary column with a split ratio of 12.5: 1. The limits of detection were in the low μg/L level, ranging between 0.01 and 0.6 μg/L. Finally optimized method was applied for determination 14 VHHs in drinking and environmental waters. The total mean concentrations of VHHs were 34.962, 26.183, 3.228 and 647.344 μg/L in tap water, purified water with 1-year-old filter element, seawater and effluents, respectively. However, no VHHs was detected in purified water with a new filter element. The main composition is different among different water matrix, which may be attributed to their different sources.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"912-921"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141906759","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

Ultra-High Performance Liquid Chromatography Method for Bioanalysis of Fampridine Using Dried Blood Spot (DBS) Methodology: Application to Pharmacokinetic Study in Albino Rats. 干血点（DBS）超高效液相色谱法分析福必定在白化大鼠体内的药代动力学研究。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-12-11 DOI: 10.1093/chromsci/bmad062

Sheba M K Chalil, Indukala P Chandrasekharan, Singaram Kathirvel, Raja R Katta

{"title":"Ultra-High Performance Liquid Chromatography Method for Bioanalysis of Fampridine Using Dried Blood Spot (DBS) Methodology: Application to Pharmacokinetic Study in Albino Rats.","authors":"Sheba M K Chalil, Indukala P Chandrasekharan, Singaram Kathirvel, Raja R Katta","doi":"10.1093/chromsci/bmad062","DOIUrl":"10.1093/chromsci/bmad062","url":null,"abstract":"Fampridine (dalfampridine) is used to improve walking in people who have multiple sclerosis (a disease in which the nerves do not function properly and may cause weakness, numbness, loss of muscle coordination and problems with vision, speech and bladder control). Measurement of fampridine plasma concentrations is not practical at sites lacking the facilities to prepare and process blood samples. A dried blood spot (DBS) sampling method, in which a few drops of blood, drawn by lancet from the finger, are applied onto specially manufactured absorbent filter paper, can be used as an alternative to plasma monitoring and would allow for simplified sample storage and transport. Using blood samples from pharmacokinetic studies, an ultra-high performance liquid chromatography assay method for quantification of fampridine in DBS is developed and validated for specificity, selectivity, accuracy, precision, reproducibility and stability. Method was specific and selective relative to endogenous compounds, with required process efficiency, and no matrix effect. Inaccuracy and precision for intra-day and inter-day analyses were tested at all concentrations. Quantification of fampridine in DBS assay was not affected by blood deposit volume and punch position within spot, and hematocrit level had a limited but acceptable effect on measurement accuracy. Fampridine was stable for at least 2 months at room temperature. The correlation between DBS and plasma concentrations with an average blood-to-plasma ratio is determined. DBS sampling is a simple and practical method for monitoring fampridine concentrations. The method is completely validated as per ICH guidelines and extended to the in vivo determination of fampridine in male albino rats.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"929-937"},"PeriodicalIF":1.5,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10332261","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

Pharmacokinetic Analysis of Two N-Substituted Rosmarinic Acid Analogs in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry. 利用液相色谱-串联质谱法分析大鼠血浆中两种 N-取代香豆酸类似物的药代动力学特征

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmae009

Shujie Fu, Qinglang Zhang, Shiyu Zhang, Weizhe Jiang, Minjie Jiang

{"title":"Pharmacokinetic Analysis of Two N-Substituted Rosmarinic Acid Analogs in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Shujie Fu, Qinglang Zhang, Shiyu Zhang, Weizhe Jiang, Minjie Jiang","doi":"10.1093/chromsci/bmae009","DOIUrl":"10.1093/chromsci/bmae009","url":null,"abstract":"This study reports the development of an effective high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the quantification of two analogs of rosmarinic acid (RA) in rat plasma, namely methyl (E)-2-(3-(3,4-difluorophenyl)acrylamido)-3-(3,4-dihydroxyphenyl)propanoate (A11) and methyl (E)-3-(3,4-dihydroxyphenyl)-2-(3-(3,4-dihydroxyphenyl)acrylamido)propanoate (A2). These analogs, featuring N atoms instead of O atoms, exhibit enhanced bioavailability and distinct pharmacological activities compared with RA. The HPLC separation was carried out on a C18 column (1.9 μm, 2.1 mm × 100 mm) coupled with a security guard C18 column (5 μm, 2.1 mm × 10 mm). A triple-quadrupole mass spectrometer equipped with an electrospray ionization ion source was utilized for ion generation. Pseudoephedrine hydrochloride was utilized as a standard, and a single-step protein precipitation method using isopropanol:ethyl acetate (v/v, 20:80) was employed for sample pretreatment. The developed method demonstrated excellent linearity over the concentration range of 5-750 ng/ml for both A11 and A2, with relative standard deviations of <15% and relative errors within 15% during daily course analysis. The method allowed for the unambiguous quantification and identification of A11 and A2 in vivo. The results of this study provide a meaningful foundation for evaluating the clinical applications of these analogs.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"815-820"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140193922","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 RP-HPLC Method for the Simultaneous Determination of Silver Sulfadiazine and Sodium Hyaluronate in the Presence of Methyl and Propyl Paraben in a Pharmaceutical Cream for Burns. 用于同时测定烧伤用药膏中存在对羟基苯甲酸甲酯和对羟基苯甲酸丙酯的磺胺嘧啶银和透明质酸钠的 RP-HPLC 方法的开发与验证。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmae028

Shereen A Boltia, Manal Ibrahim, Magda M Ibrahim, Nesrin K Ramadan

{"title":"Development and Validation of a RP-HPLC Method for the Simultaneous Determination of Silver Sulfadiazine and Sodium Hyaluronate in the Presence of Methyl and Propyl Paraben in a Pharmaceutical Cream for Burns.","authors":"Shereen A Boltia, Manal Ibrahim, Magda M Ibrahim, Nesrin K Ramadan","doi":"10.1093/chromsci/bmae028","DOIUrl":"10.1093/chromsci/bmae028","url":null,"abstract":"A direct and precise isocratic RP-HPLC method for simultaneous determination of silver sulfadiazine (SSD) and sodium hyaluronate (SH) in the presence of methyl (MP) and propyl parabens (PP) was developed and validated. Agilent chromatograph with X-Select C18 column (250 × 4.6 mm2, 5 μm) was used. Chromatographic separation was achieved using a mobile phase consisting of acetonitrile and 0.05 M phosphate buffer (pH 5.0 to which added triethyl amine 0.5 ml/L), at a ratio 35: 65 v/v. Elution was used at flow rate of 1.0 mL/min at ambient temperature with UV detection at 205 nm. The retention times for SH, SSD, MP and PP were 1.49, 3.3, 6.7 and 19.5 min, respectively. The presented chromatographic method was fully validated in accordance with ICH requirements, it was valid over linearity ranges of (0.80-100.00 μg/mL) and (3.20-100.00 μg/mL) for SSD and SH, respectively. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges and the sensitivity of the method, as the limits of detection and quantification for each active ingredient was also determined. The validated method was successfully applied for the quantification of SSD and SH in pharmaceutical cream formulation and the mean recovery % ± SD were 100.93 ± 0.985 and 100.05 ± 0.668 for SSD and SH; respectively, indicating satisfactory accuracy of the method.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"878-885"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140922240","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

Single Method for Determination of Biocides Benzalkonium Chloride, Chloroxylenol and Chlorhexidine Gluconate in Cosmetics, Hygiene and Health Care Products by Using High Performance Liquid Chromatography. 利用高效液相色谱法测定化妆品、卫生和保健产品中杀菌剂苯扎氯铵、氯甲酚和葡萄糖酸氯己定的单一方法。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmae039

Kumar Thangarathinam, Meenakshi Narayanan, Ashwin Kumar Ks, Banupriya Arjunan, Divya Bhavani Raja

{"title":"Single Method for Determination of Biocides Benzalkonium Chloride, Chloroxylenol and Chlorhexidine Gluconate in Cosmetics, Hygiene and Health Care Products by Using High Performance Liquid Chromatography.","authors":"Kumar Thangarathinam, Meenakshi Narayanan, Ashwin Kumar Ks, Banupriya Arjunan, Divya Bhavani Raja","doi":"10.1093/chromsci/bmae039","DOIUrl":"10.1093/chromsci/bmae039","url":null,"abstract":"Benzalkonium chloride (BKC), chloroxylenol (PCMX) and chlorhexidine gluconate (CHG) are widely recognized biocidal compounds that require precise control and monitoring in various applications, including cosmetics, hygiene, health and ophthalmic products. In this study, we present a straightforward and highly sensitive high-performance liquid chromatographic (HPLC) method for the detection of these substances. The HPLC method we developed allows for the detection of BKC at concentrations as low as 1.0 ppm, PCMX at 1.0 ppm and CHG at 2.0 ppm, all with a signal-to-noise (S/N) ratio exceeding 3.0. Additionally, the method enables quantification up to 2.0 ppm for BKC, 2.0 ppm for PCMX and 5 ppm for CHG, with an S/N ratio surpassing 10.0. This validated method serves as a versatile tool for the accurate quantification of BKC, PCMX and CHG in cosmetics, hygiene products, health products and ophthalmic products. Its applicability extends across a wide range of industries, ensuring the reliable assessment of these critical biocides.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"837-844"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141293419","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

Simultaneously Selective Separation of Zearalenone and Four Aflatoxins From Rice Samples Using Co-Pseudo-Template Imprinted Polymers With MIL-101(Cr)-NH2 as Core. 使用以 MIL-101(Cr)-NH2 为核心的共假模板印迹聚合物同时选择性分离大米样品中的玉米赤霉烯酮和四种黄曲霉毒素

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmae041

Lixin Song, Jian Zhang, Mingyu Wang, Zhipeng Huang, Yunxia Zhang, Xing Zhang, Yutao Liang, Juan He

{"title":"Simultaneously Selective Separation of Zearalenone and Four Aflatoxins From Rice Samples Using Co-Pseudo-Template Imprinted Polymers With MIL-101(Cr)-NH2 as Core.","authors":"Lixin Song, Jian Zhang, Mingyu Wang, Zhipeng Huang, Yunxia Zhang, Xing Zhang, Yutao Liang, Juan He","doi":"10.1093/chromsci/bmae041","DOIUrl":"10.1093/chromsci/bmae041","url":null,"abstract":"A novel approach for the simultaneous separation of zearalenone (ZEN) and four types of aflatoxins (AFB1, AFB2, AFG1 and AFG2) from rice samples was presented. This approach utilized modified MIL-101(Cr)-NH2 as core, with molecularly imprinted polymers (MIPs) serving as the shell. The MIL-101(Cr)-NH2 was prepared via ring-opening reaction, while the imprinted polymers were synthesized using warfarin and 4-methylumbelliferyl acetate as co-pseudo template, ethylene glycol dimethacrylate as the cross-linker and azobisisobutyronitrile as initiator. The resulting co-pseudo-template-MIPs (CPT-MIPs) were thoroughly characterized and evaluated. Adsorption studies demonstrate that the adsorption process of CPT-MIPs follows a chemical monolayer adsorption mechanism, with imprinted factors ranging from 1.24 to 1.52 and selective factors ranging from 1.29 to 1.52. Self-made columns were prepared, and the method for separation was developed and validated. The limit of detections ranged from 0.12 to 2.09 μg/kg, and the limit of qualifications ranged from 1.2 to 6.25 μg/kg. To assess the reliability of the method, ZEN and AFs were spiked at three different levels, and the recoveries ranged from 79.53 to 94.58%, with relative standard deviations of 2.90-5.78%.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"892-903"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141306047","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

HPTLC Method Development and Validation for the Simultaneous Estimation of Nortriptyline HCl and Pregabalin in their Combined Dosage Form. 同时测定盐酸去甲替林和普瑞巴林联合剂型的高效薄层色谱法的建立和验证。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmad081

Hinal Harkhani, Kashyap Thummar, Sanjay Chauhan, Jigna Vadalia

{"title":"HPTLC Method Development and Validation for the Simultaneous Estimation of Nortriptyline HCl and Pregabalin in their Combined Dosage Form.","authors":"Hinal Harkhani, Kashyap Thummar, Sanjay Chauhan, Jigna Vadalia","doi":"10.1093/chromsci/bmad081","DOIUrl":"10.1093/chromsci/bmad081","url":null,"abstract":"Nortriptyline HCl and pregabalin Tablet is used to treat neuropathic pain as well as mental or mood issues such as sadness, mood, feelings, anxiety and tensions. Very few analytical methods are available for the simultaneous estimation of nortriptyline HCl and pregabalin and no reports has been found for HPTLC method. In the current study, a reliable HPTLC method for the simultaneous measurement of nortriptyline HCl and pregabalin in pure forms and pharmaceutical formulations has been developed with ninhydrine post derivatization of pregabalin. The HPTLC method development was carried using silica gel G60 F254 as stationary phase and acetonitrile: methanol: triethylamine: water: formic acid (7:3:0.3:0.8:0.02 v/v/v/v/v) was used as mobile phase with saturation time of 20 min. The system was found to give a compact band for nortriptyline HCl (Rf = 0.523 ± 0.008) pregabalin (Rf = 0.279 ± 0.005). The developed method was found to be validated as per ICH Q2 (R1) guideline. The peak of nortriptyline HCl and pregabalin showed good linearity over the concentration range of 50-300 ng/band and 350-2250 ng/band, respectively, with a correlation coefficient of ˃0.995. The % recoveries of both drugs were found to be in the range of 98.84-101.87%. Statistical analysis proved that the method is selective, precise, robust and accurate for the estimation of nortriptyline HCl and pregabalin.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"886-891"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49677964","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

Ecofriendly HPLC Method for Simultaneous Determination of the Co-Prescribed Drugs in Chemotherapy Omeprazole, Ondansetron and Deflazacort in Spiked Human Plasma. 环境友好高效液相色谱法同时测定人血浆中加标药物奥美拉唑、昂丹司琼和地氮唑。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmad088

Fatma F Abdallah, M Fatma, Ahmed M Gouda, Eglal A Abdelaleem, Aml A Emam

{"title":"Ecofriendly HPLC Method for Simultaneous Determination of the Co-Prescribed Drugs in Chemotherapy Omeprazole, Ondansetron and Deflazacort in Spiked Human Plasma.","authors":"Fatma F Abdallah, M Fatma, Ahmed M Gouda, Eglal A Abdelaleem, Aml A Emam","doi":"10.1093/chromsci/bmad088","DOIUrl":"10.1093/chromsci/bmad088","url":null,"abstract":"Green, selective and accurate high-performance liquid chromatography (HPLC) chromatographic method is presented for simultaneous separation and quantitation of the co-prescribed drugs in chemotherapy omeprazole, ondansetron and deflazacort in spiked human plasma. An isocratic HPLC separation was performed on X Bridge C18 (4.6 × 250 mm) column with 5 μm particle size using mobile phase consisting of methanol: ammonium acetate buffer pH 4 adjusted by acetic acid (60: 40, v/v). The injection volume was 20μL with UV detection wavelength at 237 nm at room temperature. Flow rate of the mobile phase was adjusted to be 2.0 ml/min. Dexamethasone was used as internal standard to correct the variation during sample pretreatment. FDA guidelines were followed to validate the developed method. Successful application of the developed method was revealed by simultaneous determination of omeprazole, ondansetron and deflazacort in spiked human plasma in ranges of 1-20, 0.1-8 and 0.2-8 μg mL-1 for omeprazole, ondansetron and deflazacort, respectively. Four greenness assessment tools were used to evaluate the greenness of the developed method and the results were accepted. This method permitted the accurate simultaneous determination of the studied drugs, thus it can be used during therapeutic drug monitoring in daily clinical practice.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"845-853"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138299185","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

Reverse Phase HPLC Methodology for the Determination of Bay K8644. 反相高效液相色谱法测定 Bay K8644。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmae011

Pablo Miranda, Analía Castro, Luisina Rodríguez Grassi, Danilo Davyt, Marcelo Hill, Mercedes Segovia, Alvaro W Mombrú, Helena Pardo

{"title":"Reverse Phase HPLC Methodology for the Determination of Bay K8644.","authors":"Pablo Miranda, Analía Castro, Luisina Rodríguez Grassi, Danilo Davyt, Marcelo Hill, Mercedes Segovia, Alvaro W Mombrú, Helena Pardo","doi":"10.1093/chromsci/bmae011","DOIUrl":"10.1093/chromsci/bmae011","url":null,"abstract":"Following ICH guidelines for analytical validation, we report a common C18 column stability indicating isocratic reverse phase high performance liquid chromatography method for the determination of the ion channel modulator Bay K8644. Two main forced degradation products and a minor impurity were also tentatively identified by Mass Spectrometry. The mobile phase consisted of a 50/50 acetonitrile/buffer mixture at a flow rate of 2 mL/min. Mean retention time for Bay K8644 was 3.030 minutes. Excellent linearity (r = 0.9998) was achieved in the range 0.10-1.40 μg/mL at 274 nm wavelength. Analytical limits were 16.56 ± 1.04 ng/mL for detection and 55.21 ± 3.48 ng/mL for quantitation respectively. Accuracy and precision studies showed good results (95-105%). Robustness was assessed by varying ±3%, both temperature and flow rate. Five different stress conditions were applied to assess Bay K8644's stability. Only basic and photolytic treatments yielded degradation products, both correctly resolved in a total runtime of 4 minutes. In conclusion, we developed a fast, simple, sensitive, accurate, precise, reliable and stability indicating method for detecting/quantifying Bay K8644, and tentatively characterized its main impurities/forced degradation products.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"829-836"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140326636","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 TLC-Densitometric Method for Simultaneous Determination of Antazoline and Tetryzoline: Application to Pharmaceutical Formulation and Rabbit Aqueous Humor. 同时测定安他唑啉和泰特唑啉的绿色 TLC 密度测定法：在药物制剂和家兔水体中的应用

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2024-11-01 DOI: 10.1093/chromsci/bmad042

Ola G Hussein, Yasmin Rostom, Mohamed Abdelkawy, Mamdouh R Rezk, Dina A Ahmed

{"title":"Green TLC-Densitometric Method for Simultaneous Determination of Antazoline and Tetryzoline: Application to Pharmaceutical Formulation and Rabbit Aqueous Humor.","authors":"Ola G Hussein, Yasmin Rostom, Mohamed Abdelkawy, Mamdouh R Rezk, Dina A Ahmed","doi":"10.1093/chromsci/bmad042","DOIUrl":"10.1093/chromsci/bmad042","url":null,"abstract":"Ophthalmic pharmaceutical preparation containing antazoline (ANT) and tetryzoline (TET) is prescribed widely as an over the counter medication for allergic conjunctivitis treatment. Development of a selective, simple and environmentally friendly thin-layer chromatographic method established to determine both ANT and TET in their pure forms, pharmaceutical formulation and spiked aqueous humor samples. By using silica gel plates and means of a developing system consists of ethyl acetate:ethanol (5:5, by volume), the studied drugs separation was achieved, and scanning was carried out at 220.0 nm for the separated bands with a 0.2-18.0 μg/band concentration range for each of ANT and TET. Standard addition technique application was carried out to determine the proposed method validity. Statistical comparison was made between the proposed method and the official methods ANT and TET showing no significant difference concerning accuracy and precision. Furthermore, greenness profile assessment was accomplished by means of four metric tools, namely, analytical greenness, green analytical procedure index, analytical eco-scale and national environmental method index.Highlights.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"807-814"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9988749","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