Pub Date : 2024-05-17DOI: 10.1093/chromsci/bmae029
Shu-Tong Yang, Yi-Wen Cao, Zi-Ying Zeng, Zheng Gang, Min Chen, Bing-Yan Du, Miao-Miao Su, Zhong-Hua Yang, Zhu-Hua Tang, Yun-Liu Zeng
In this work, a magnetic adsorption material based on metal-organic framework (Fe3O4@ZnAl-LDH@MIL-53(Al)) was synthesized and used as an adsorbent in the process of magnetic solid phase extraction. Then, a high-performance liquid chromatograph was used to quantitatively detect triazole fungicides in samples. In order to verify the successful preparation of the material, a series of characterization analyses were carried out. Besides, the key parameters that may affect the extraction efficiency have been optimized, and under optimal conditions the three triazole fungicides showed good linearity in the range of 10-1000 μg/L (R2 ≥ 0.9796); Limit of detections were ranged from 0.013 to 0.030 μg/mL. Finally, the established method was applied to the detection of triazole fungicides in four fresh juice samples. The results showed that the target analyte was not detected in all the test samples. By detecting the recoveries (73.3-104.3%) and coefficient variation (RSD ≤ 6.8%) of triazole fungicides in fortified samples, it proved that this established method meets the requirements of pesticide residue analysis and showed excellent application potential.
{"title":"Determination of Azole Fungicide Residues in Fresh Juice by Magnetic Solid Phase Extraction Based on Fe3O4@ZnAl-LDH@MIL-53(Al) Sorbent in Combination with High-Performance Liquid Chromatograph.","authors":"Shu-Tong Yang, Yi-Wen Cao, Zi-Ying Zeng, Zheng Gang, Min Chen, Bing-Yan Du, Miao-Miao Su, Zhong-Hua Yang, Zhu-Hua Tang, Yun-Liu Zeng","doi":"10.1093/chromsci/bmae029","DOIUrl":"https://doi.org/10.1093/chromsci/bmae029","url":null,"abstract":"<p><p>In this work, a magnetic adsorption material based on metal-organic framework (Fe3O4@ZnAl-LDH@MIL-53(Al)) was synthesized and used as an adsorbent in the process of magnetic solid phase extraction. Then, a high-performance liquid chromatograph was used to quantitatively detect triazole fungicides in samples. In order to verify the successful preparation of the material, a series of characterization analyses were carried out. Besides, the key parameters that may affect the extraction efficiency have been optimized, and under optimal conditions the three triazole fungicides showed good linearity in the range of 10-1000 μg/L (R2 ≥ 0.9796); Limit of detections were ranged from 0.013 to 0.030 μg/mL. Finally, the established method was applied to the detection of triazole fungicides in four fresh juice samples. The results showed that the target analyte was not detected in all the test samples. By detecting the recoveries (73.3-104.3%) and coefficient variation (RSD ≤ 6.8%) of triazole fungicides in fortified samples, it proved that this established method meets the requirements of pesticide residue analysis and showed excellent application potential.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140957570","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 : 2024-05-14DOI: 10.1093/chromsci/bmae028
Shereen A Boltia, Manal Ibrahim, Magda M Ibrahim, Nesrin K Ramadan
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.
{"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":"https://doi.org/10.1093/chromsci/bmae028","url":null,"abstract":"<p><p>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.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-14","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}
A new stability-indicating high-performance liquid chromatographic method for the quantitative determination of ibuprofen and famotidine degradation products in combined pharmaceutical products was developed and validated. The current aim of this study is to develop a rapid, accurate and robust analytical stability indicating impurity method that can separate ibuprofen, famotidine and their related impurities by using a reversed-phase high-performance liquid chromatography. A Zorbax SB-Phenyl column (4.6 × 150 mm2, 5-μm particle size) with mobile phase containing phosphate buffer solution with a pH value of 3.0 and acetonitrile was used. The flow rate was 0.8 mL/min and the analytes were detected by UV detector at 265 nm. The retention times of ibuprofen and famotidine were 18.43 and 5.14 min, respectively. This method was validated to confirm specificity, linearity, sensitivity (limit of detection and limit of quantitation), precision, accuracy, robustness and sample stability according to the International Conference on Harmonization guidelines. Studies have been completed and reported with two active substances in the combined dosage form and seven impurities in total. There is no method in the literature that simultaneously distinguishes and quantitatively analyzes both active substances and degradation products.
{"title":"Stability-Indicating HPLC Method for Determination of Ibuprofen and Famotidine Degradation Products.","authors":"Nurdan Atilgan, Gizem Tabansiz, Ezgi Turkes, Nagehan Sarracoglu, Asuman Aybey Doganay, Onur Pinarbasli","doi":"10.1093/chromsci/bmae027","DOIUrl":"https://doi.org/10.1093/chromsci/bmae027","url":null,"abstract":"<p><p>A new stability-indicating high-performance liquid chromatographic method for the quantitative determination of ibuprofen and famotidine degradation products in combined pharmaceutical products was developed and validated. The current aim of this study is to develop a rapid, accurate and robust analytical stability indicating impurity method that can separate ibuprofen, famotidine and their related impurities by using a reversed-phase high-performance liquid chromatography. A Zorbax SB-Phenyl column (4.6 × 150 mm2, 5-μm particle size) with mobile phase containing phosphate buffer solution with a pH value of 3.0 and acetonitrile was used. The flow rate was 0.8 mL/min and the analytes were detected by UV detector at 265 nm. The retention times of ibuprofen and famotidine were 18.43 and 5.14 min, respectively. This method was validated to confirm specificity, linearity, sensitivity (limit of detection and limit of quantitation), precision, accuracy, robustness and sample stability according to the International Conference on Harmonization guidelines. Studies have been completed and reported with two active substances in the combined dosage form and seven impurities in total. There is no method in the literature that simultaneously distinguishes and quantitatively analyzes both active substances and degradation products.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140898513","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}
The current treatment protocol for drug-sensitive tuberculosis involves all four first-line anti-tuberculosis drugs: rifampicin, isoniazid, pyrazinamide and ethambutol hydrochloride in a single tablet, known as fixed-dose combination tablets. However, the analytical methods are scanty to test all these drugs simultaneously in a single run without any pre-sample process or using a simple method suitable for resource-limited settings. In this method, 50 mM potassium phosphate buffer containing 0.2% triethylamine (without pH adjustment) added with acetonitrile (98:2, v/v) was served as mobile phase A, while mobile phase B was 100% acetonitrile. All four drugs were separated within 10.3 min using a gradient mobile phase program in a C18 column (150 mm × 4.6 mm; 5 μm) and detected at two ultraviolet wavelengths (238 nm for rifampicin, isoniazid and pyrazinamide, and 210 nm for ethambutol hydrochloride). The method was selective, sensitive and linear with a correlation coefficient >0.999 with the acceptable precision and accuracy (<2% relative standard deviation) for all four drugs. In conclusion, the method is simple and it does not require any pH adjustment of the buffer/mobile phase, and within 11 min, the separation of all four drugs can be achieved. Overall, the method is suitable for quality testing of fixed-dose combination tablets in limited-resource settings.
目前对药物敏感的结核病的治疗方案包括将所有四种一线抗结核药物(利福平、异烟肼、吡嗪酰胺和盐酸乙胺丁醇)制成一片,即固定剂量复方片剂。然而,能在一次运行中同时检测所有这些药物而无需任何预抽样过程或使用适合资源有限环境的简单方法的分析方法却很少。在该方法中,流动相 A 为含 0.2% 三乙胺的 50 mM 磷酸二氢钾缓冲液(无需调节 pH 值),流动相 B 为 100% 乙腈(98:2, v/v)。采用 C18 色谱柱(150 mm × 4.6 mm; 5 μm),以梯度流动相程序在 10.3 min 内分离了所有四种药物,并在两个紫外波长(利福平、异烟肼和吡嗪酰胺为 238 nm,盐酸乙胺丁醇为 210 nm)下进行检测。该方法选择性好、灵敏度高、线性关系良好,相关系数大于 0.999,精密度和准确度均可接受 (
{"title":"Development and Validation of a Simple High-Pressure Liquid Chromatography-Ultraviolet Detection Method for Simultaneous Quantitation of First-Line Anti-Tuberculosis Drugs in Formulations of Fixed-Dose Combination.","authors":"Sudha Vilvamani, Santhanamahalingam Mahalingam, Sruthi Nhavilthodi, Dharman Murugesan, Shanmugam Murugaiha Jeyakumar","doi":"10.1093/chromsci/bmae023","DOIUrl":"https://doi.org/10.1093/chromsci/bmae023","url":null,"abstract":"<p><p>The current treatment protocol for drug-sensitive tuberculosis involves all four first-line anti-tuberculosis drugs: rifampicin, isoniazid, pyrazinamide and ethambutol hydrochloride in a single tablet, known as fixed-dose combination tablets. However, the analytical methods are scanty to test all these drugs simultaneously in a single run without any pre-sample process or using a simple method suitable for resource-limited settings. In this method, 50 mM potassium phosphate buffer containing 0.2% triethylamine (without pH adjustment) added with acetonitrile (98:2, v/v) was served as mobile phase A, while mobile phase B was 100% acetonitrile. All four drugs were separated within 10.3 min using a gradient mobile phase program in a C18 column (150 mm × 4.6 mm; 5 μm) and detected at two ultraviolet wavelengths (238 nm for rifampicin, isoniazid and pyrazinamide, and 210 nm for ethambutol hydrochloride). The method was selective, sensitive and linear with a correlation coefficient >0.999 with the acceptable precision and accuracy (<2% relative standard deviation) for all four drugs. In conclusion, the method is simple and it does not require any pH adjustment of the buffer/mobile phase, and within 11 min, the separation of all four drugs can be achieved. Overall, the method is suitable for quality testing of fixed-dose combination tablets in limited-resource settings.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140876568","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 : 2024-05-05DOI: 10.1093/chromsci/bmae024
Aya A Mouhamed, Basma M Eltanany, Nadia M Mostafa, Ahmed H Nadim
Design of experiment is an efficient and cost-effective tool to optimize the chromatographic separation of a multicomponent mixture. The central composite design was conducted to develop and optimize a green high performance liquid chromatography (HPLC) method for simultaneous quantitation of a quaternary mixture of paracetamol, chlorpheniramine maleate, caffeine and ascorbic acid in their pharmaceutical dosage form as well as the determination of their dissolution profile. A five-level three-factor model was performed to investigate the effect of mobile phase composition, pH and flow rate on enhanced resolution and short run time. Analysis was performed using a Kinitex EVO C18 column and a mobile phase composed of methanol: 0.02 M phosphate buffer pH 3.3 (34:66, v/v) at 1.0 mL/min using photodiode array detection. Optimum chromatographic separation was achieved in <6 min with a desirability of 0.999. Linearity was achieved over a range of 1.00–300.00, 1.00–50.00, 2.00–50.00 and 2.00–100.00 μg/mL for paracetamol, chlorpheniramine maleate, caffeine and ascorbic acid, respectively, with a limit of detection (<0.1 μg/mL). The greenness profile was evaluated using the analytical eco-scale and Analytical GREEnness Metric Approach with values of 81 and 0.77, respectively.
{"title":"Development of Response Surface Approach for Determination of Paracetamol, Chlorpheniramine Maleate, Caffeine and Ascorbic Acid by Green HPLC Method: A Desirability-Based Optimization","authors":"Aya A Mouhamed, Basma M Eltanany, Nadia M Mostafa, Ahmed H Nadim","doi":"10.1093/chromsci/bmae024","DOIUrl":"https://doi.org/10.1093/chromsci/bmae024","url":null,"abstract":"Design of experiment is an efficient and cost-effective tool to optimize the chromatographic separation of a multicomponent mixture. The central composite design was conducted to develop and optimize a green high performance liquid chromatography (HPLC) method for simultaneous quantitation of a quaternary mixture of paracetamol, chlorpheniramine maleate, caffeine and ascorbic acid in their pharmaceutical dosage form as well as the determination of their dissolution profile. A five-level three-factor model was performed to investigate the effect of mobile phase composition, pH and flow rate on enhanced resolution and short run time. Analysis was performed using a Kinitex EVO C18 column and a mobile phase composed of methanol: 0.02 M phosphate buffer pH 3.3 (34:66, v/v) at 1.0 mL/min using photodiode array detection. Optimum chromatographic separation was achieved in &lt;6 min with a desirability of 0.999. Linearity was achieved over a range of 1.00–300.00, 1.00–50.00, 2.00–50.00 and 2.00–100.00 μg/mL for paracetamol, chlorpheniramine maleate, caffeine and ascorbic acid, respectively, with a limit of detection (&lt;0.1 μg/mL). The greenness profile was evaluated using the analytical eco-scale and Analytical GREEnness Metric Approach with values of 81 and 0.77, respectively.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140829785","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}
Ayurveda emphasizes the propagation of nature in maintaining health. In the present scenario, we have seen the faith of people in herbal drugs during the Covid 19 outbreak. The raises in the number of peoples have been using herbal drugs to boost immunity against infectious diseases shows the popularity of this ancient system of medicine. The standardization of Ayush Kvatha Churna (AKC), work set out to establish a straightforward, accurate and sensitive HPTLC method for the identification and quantification of marker compounds. The Rosmarinic acid, trans-Cinnamaldehyde and Piperine were used for the estimation of markers in Ayush Kvatha Churna by using HPTLC with a solvent system, consisting of Toluene: Ethyl acetate: Ethyl alcohol: Formic acid (5.6:2.4:2: 0.3 v/v/v/v). The Rf value 0.33 for Rosmarinic Acid, 0.69 for Piperine and 0.77 for trans-Cinnamaldehyde was observed and it is exactly complying with the corresponding bands in Ayush Kvatha Churna. The technique has been effectively verified and validated, enabling it to be used for the standardization or quantitative analysis of Rosmarinic acid, trans-Cinnamaldehyde and piperine in Ayush Kvatha Churna.
{"title":"Development of Simultaneous HPTLC Method and Validation for the Quality Assessment of Ayurvedic Formulation-Ayush Kvatha Churna by Using Marker Compound Rosmarinic Acid, Trans-Cinnamaldehyde and Piperine.","authors":"Umakant Sahu, Nagendra Singh Chauhan, Arun Kumar Singh Parihar, Kamleshwar Singh Karbhal, Shrikant R Inchulkar, Prashant Kumar Gupta, Rajesh Kumar Singh","doi":"10.1093/chromsci/bmae019","DOIUrl":"https://doi.org/10.1093/chromsci/bmae019","url":null,"abstract":"<p><p>Ayurveda emphasizes the propagation of nature in maintaining health. In the present scenario, we have seen the faith of people in herbal drugs during the Covid 19 outbreak. The raises in the number of peoples have been using herbal drugs to boost immunity against infectious diseases shows the popularity of this ancient system of medicine. The standardization of Ayush Kvatha Churna (AKC), work set out to establish a straightforward, accurate and sensitive HPTLC method for the identification and quantification of marker compounds. The Rosmarinic acid, trans-Cinnamaldehyde and Piperine were used for the estimation of markers in Ayush Kvatha Churna by using HPTLC with a solvent system, consisting of Toluene: Ethyl acetate: Ethyl alcohol: Formic acid (5.6:2.4:2: 0.3 v/v/v/v). The Rf value 0.33 for Rosmarinic Acid, 0.69 for Piperine and 0.77 for trans-Cinnamaldehyde was observed and it is exactly complying with the corresponding bands in Ayush Kvatha Churna. The technique has been effectively verified and validated, enabling it to be used for the standardization or quantitative analysis of Rosmarinic acid, trans-Cinnamaldehyde and piperine in Ayush Kvatha Churna.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140849768","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 : 2024-05-05DOI: 10.1093/chromsci/bmae021
Vikas Chauhan, Parul Grover, Monika Bhardwaj, Sandeep Kumar, K Nagarajan
A simple, rapid, sensitive, and cost-effective green solvent-assisted reverse-phase high-performance liquid chromatographic technique, coupled with a photodiode array detector, was developed and validated for the estimation of piroxicam (PRXM). The chromatographic separation was achieved by using a C-18 (250 × 4.6) mm, 5-μm stationary phase and a mobile phase consisting of methanol and 0.1% ortho-phosphoric acid in water in a ratio of (80:20) v/v at a flow rate of 1 ml/min. The detection was carried out at a wavelength of 254 nm with a constant injection volume of 10 μL throughout the analysis. The calibration curve was observed to be linear over the optimum concentration range of 50–300 μg mL−1, with an R2 value of 0.9995. The developed method was validated as per the International Council for Harmonisation (ICH) Q2 (R1) guideline. Various parameters like selectivity/specificity, accuracy/recovery, linearity, precision, detection limit, quantitation limit, robustness and stability of analyte in solution were performed for the method validation. The PRXM was evaluated under stressed conditions, including acidic, basic, oxidative, thermal and photolytic, as per ICH Q1 (R2) guidelines. Significant degradation was observed in acidic and basic degradation conditions. Conversely, the drug substance showed stability when exposed to oxidative, photolytic and thermal degradation conditions.
{"title":"Development and Validation of Fast and Sensitive RP-HPLC Stability-Indicating Method for Quantification of Piroxicam in Bulk Drug","authors":"Vikas Chauhan, Parul Grover, Monika Bhardwaj, Sandeep Kumar, K Nagarajan","doi":"10.1093/chromsci/bmae021","DOIUrl":"https://doi.org/10.1093/chromsci/bmae021","url":null,"abstract":"A simple, rapid, sensitive, and cost-effective green solvent-assisted reverse-phase high-performance liquid chromatographic technique, coupled with a photodiode array detector, was developed and validated for the estimation of piroxicam (PRXM). The chromatographic separation was achieved by using a C-18 (250 × 4.6) mm, 5-μm stationary phase and a mobile phase consisting of methanol and 0.1% ortho-phosphoric acid in water in a ratio of (80:20) v/v at a flow rate of 1 ml/min. The detection was carried out at a wavelength of 254 nm with a constant injection volume of 10 μL throughout the analysis. The calibration curve was observed to be linear over the optimum concentration range of 50–300 μg mL−1, with an R2 value of 0.9995. The developed method was validated as per the International Council for Harmonisation (ICH) Q2 (R1) guideline. Various parameters like selectivity/specificity, accuracy/recovery, linearity, precision, detection limit, quantitation limit, robustness and stability of analyte in solution were performed for the method validation. The PRXM was evaluated under stressed conditions, including acidic, basic, oxidative, thermal and photolytic, as per ICH Q1 (R2) guidelines. Significant degradation was observed in acidic and basic degradation conditions. Conversely, the drug substance showed stability when exposed to oxidative, photolytic and thermal degradation conditions.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140829789","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 : 2024-05-05DOI: 10.1093/chromsci/bmae018
Saeedeh Jafari, Abdollah Hematian Sourki
A validated rapid high-performance liquid chromatography (HPLC)-refractive index (RI) method was developed for the identification and quantification of glucose and xylose in hydrolyzed bagasse extract. The separation of compounds was achieved on Eurokat® H column (300 × 8 mm, 10 μm) at 75°C, using 0.01 N sulfuric acid solution as mobile phase and 0.6 mL/min as flow rate. The method was validated based on accuracy, precision, linearity, robustness, uncertainty, limit of detection (LOD) and limit of quantification (LOQ). Total chromatographic analysis time per sample was ~11 min. Calibration plots were linear over the concentration ranges 11–100 μg/100 μL for glucose and xylose. The LOD was 0.8 ppm and LOQ was 2.5 ppm. The high recovery and low relative standard deviation confirm the suitability of the method for determination of glucose and xylose in bagasse extract. The proposed HPLC-RI method was accurate, fast and robust and required less run time due to less analytes retention times and allowed optimal energy consumption owing to lower column oven temperature.
为鉴定和定量水解甘蔗渣提取物中的葡萄糖和木糖,开发了一种有效的快速高效液相色谱-折光率(RI)分析方法。采用 Eurokat® H 色谱柱(300 × 8 mm, 10 μm),以 0.01 N 硫酸溶液为流动相,流速为 0.6 mL/min,检测温度为 75°C。该方法的准确度、精密度、线性、稳健性、不确定性、检出限(LOD)和定量限(LOQ)均得到了验证。每个样品的色谱分析总时间约为 11 分钟。葡萄糖和木糖在 11-100 μg/100 μL 的浓度范围内线性关系良好。LOD 为 0.8 ppm,LOQ 为 2.5 ppm。高回收率和低相对标准偏差证实了该方法适用于蔗渣提取物中葡萄糖和木糖的测定。所提出的 HPLC-RI 方法准确、快速、稳健,由于分析物的保留时间较短,所需的运行时间也较短,而且由于柱温较低,能耗也较低。
{"title":"Development and Validation of the HPLC Method for Simultaneous Quantification of Glucose and Xylose in Sugar Cane Bagasse Extract","authors":"Saeedeh Jafari, Abdollah Hematian Sourki","doi":"10.1093/chromsci/bmae018","DOIUrl":"https://doi.org/10.1093/chromsci/bmae018","url":null,"abstract":"A validated rapid high-performance liquid chromatography (HPLC)-refractive index (RI) method was developed for the identification and quantification of glucose and xylose in hydrolyzed bagasse extract. The separation of compounds was achieved on Eurokat® H column (300 × 8 mm, 10 μm) at 75°C, using 0.01 N sulfuric acid solution as mobile phase and 0.6 mL/min as flow rate. The method was validated based on accuracy, precision, linearity, robustness, uncertainty, limit of detection (LOD) and limit of quantification (LOQ). Total chromatographic analysis time per sample was ~11 min. Calibration plots were linear over the concentration ranges 11–100 μg/100 μL for glucose and xylose. The LOD was 0.8 ppm and LOQ was 2.5 ppm. The high recovery and low relative standard deviation confirm the suitability of the method for determination of glucose and xylose in bagasse extract. The proposed HPLC-RI method was accurate, fast and robust and required less run time due to less analytes retention times and allowed optimal energy consumption owing to lower column oven temperature.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140829962","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 : 2024-05-05DOI: 10.1093/chromsci/bmae022
Waibiangki Lyngdoh, Sandeep Jat, Pramod Kumar
Glycyrrhiza glabra is commonly known as licorice. Licorice is the major source of glycyrrhizin. There is no reported stability indicating method for glycyrrhizin in the literature so far. Therefore, it was proposed to develop a stability indicating method and validate the method for glycyrrhizin and its application in G. glabra root extract. Method validation parameters were performed as per the International Council for Harmonization guidelines. The chromatographic separation was achieved on a Zorbax Extended C-18 (250 × 4.6 mm, 5 μm) column. The separation achieved using the mobile phase consisted of 0.1% formic acid in water and acetonitrile in gradient elution. The flow rate was kept at 1 mL/min, and ultraviolet-visible spectroscopy detection was at 250 nm. The average retention time of glycyrrhizin was found to be 7.30 min. Stress degradation studies were performed and confirmed that only acidic degradation has shown a degradation profile of glycyrrhizin up to 40%. The percentage of glycyrrhizin was found to be 0.40% in the G. glabra extract. This may be further explored for commercial applications.
{"title":"Stability Indicating Method Development and Validation of Glycyrrhizin Using RP-HPLC-DAD: Application to Glycyrrhiza glabra Extract.","authors":"Waibiangki Lyngdoh, Sandeep Jat, Pramod Kumar","doi":"10.1093/chromsci/bmae022","DOIUrl":"https://doi.org/10.1093/chromsci/bmae022","url":null,"abstract":"<p><p>Glycyrrhiza glabra is commonly known as licorice. Licorice is the major source of glycyrrhizin. There is no reported stability indicating method for glycyrrhizin in the literature so far. Therefore, it was proposed to develop a stability indicating method and validate the method for glycyrrhizin and its application in G. glabra root extract. Method validation parameters were performed as per the International Council for Harmonization guidelines. The chromatographic separation was achieved on a Zorbax Extended C-18 (250 × 4.6 mm, 5 μm) column. The separation achieved using the mobile phase consisted of 0.1% formic acid in water and acetonitrile in gradient elution. The flow rate was kept at 1 mL/min, and ultraviolet-visible spectroscopy detection was at 250 nm. The average retention time of glycyrrhizin was found to be 7.30 min. Stress degradation studies were performed and confirmed that only acidic degradation has shown a degradation profile of glycyrrhizin up to 40%. The percentage of glycyrrhizin was found to be 0.40% in the G. glabra extract. This may be further explored for commercial applications.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140849307","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 : 2024-05-04DOI: 10.1093/chromsci/bmae020
Shuaibin Wu, Xuejuan Peng
In this study, the attapulgite nanoparticle was immobilized on the surface of magnetic nanoparticle Fe3O4 via a novel surface covalent reaction method for the magnetic solid phase extraction (MSPE) for the first time. The surface covalent reaction method has the advantages of controllable steps, and can make the magnetic attapulgite nanoparticle (MANP) have good homogeneity and high stability. Field emission scanning electron microscopy, equipped with an energy dispersive spectrometer, Nitrogen adsorption BET, X-ray diffraction and Fourier transform infrared spectroscopy were applied to characterize the prepared MANP, confirming that the attapulgite nanoparticle could be effectively immobilized on the surface of magnetic nanoparticle Fe3O4 via covalent reactions. Under optimal conditions of the MSPE experiment based on the MANP, the limits of detection were found to be 10 ng/mL for melamine and 3 ng/mL for cyromazine with a relative standard deviation < 10% by a high-performance liquid chromatography system. Meanwhile, 0.1 mg/mL melamine in milk and 0.1 mg/mL cyromazine in cucumber can also be detected according to our MSPE procedure. More importantly, the MANP still has good magnetism and enrichment efficiency after several decades of use. These results showed that the MANP prepared by our method is a kind of promising material for the MSPE.
{"title":"Synthesis of Magnetic Attapulgite Nanoparticles Via a Novel Surface Covalent Reaction Method and its Application in the Magnetic Solid Phase Extraction","authors":"Shuaibin Wu, Xuejuan Peng","doi":"10.1093/chromsci/bmae020","DOIUrl":"https://doi.org/10.1093/chromsci/bmae020","url":null,"abstract":"In this study, the attapulgite nanoparticle was immobilized on the surface of magnetic nanoparticle Fe3O4 via a novel surface covalent reaction method for the magnetic solid phase extraction (MSPE) for the first time. The surface covalent reaction method has the advantages of controllable steps, and can make the magnetic attapulgite nanoparticle (MANP) have good homogeneity and high stability. Field emission scanning electron microscopy, equipped with an energy dispersive spectrometer, Nitrogen adsorption BET, X-ray diffraction and Fourier transform infrared spectroscopy were applied to characterize the prepared MANP, confirming that the attapulgite nanoparticle could be effectively immobilized on the surface of magnetic nanoparticle Fe3O4 via covalent reactions. Under optimal conditions of the MSPE experiment based on the MANP, the limits of detection were found to be 10 ng/mL for melamine and 3 ng/mL for cyromazine with a relative standard deviation &lt; 10% by a high-performance liquid chromatography system. Meanwhile, 0.1 mg/mL melamine in milk and 0.1 mg/mL cyromazine in cucumber can also be detected according to our MSPE procedure. More importantly, the MANP still has good magnetism and enrichment efficiency after several decades of use. These results showed that the MANP prepared by our method is a kind of promising material for the MSPE.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140829782","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}