Liang Zhang, Weiwei Xu, Hongxia Jiang, Jianqun Liu
There has been a lively interest on macrocyclic polyamine alkaloids due to their remarkable pharmacological activities such as anti-tumor, anti-inflammatory, anti-Alzheimer's disease and anti-parasitic. Tripterygium wilfordii is a widely used traditional Chinese medicine, which is abundant in alkaloids including macrocyclic polyamine alkaloids. However, there are rarely studies on macrocyclic spermidine alkaloids of T. wilfordii so far. In this article, we use three known macrocyclic spermidine alkaloids celafurine, celabenzine and celacinnine, and successfully develop a simple and sensitive HPLC method for simultaneous quantification of macrocyclic spermidine alkaloids in root, stem and leaf of T. wilfordii.
{"title":"A simple and sensitive HPLC method for simultaneous quantification of macrocyclic spermidine alkaloids in root, stem and leaf of Tripterygium wilfordii","authors":"Liang Zhang, Weiwei Xu, Hongxia Jiang, Jianqun Liu","doi":"10.1556/1326.2022.01014","DOIUrl":"https://doi.org/10.1556/1326.2022.01014","url":null,"abstract":"\u0000 There has been a lively interest on macrocyclic polyamine alkaloids due to their remarkable pharmacological activities such as anti-tumor, anti-inflammatory, anti-Alzheimer's disease and anti-parasitic. Tripterygium wilfordii is a widely used traditional Chinese medicine, which is abundant in alkaloids including macrocyclic polyamine alkaloids. However, there are rarely studies on macrocyclic spermidine alkaloids of T. wilfordii so far. In this article, we use three known macrocyclic spermidine alkaloids celafurine, celabenzine and celacinnine, and successfully develop a simple and sensitive HPLC method for simultaneous quantification of macrocyclic spermidine alkaloids in root, stem and leaf of T. wilfordii.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49122011","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 sensitive and validated method for determining quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) was established in aquatic products using ultra-high-performance liquid chromatography-tandem spectrometry (UHPLC-MS/MS). Samples were extracted with 2.0 mol L−1 hydrochloric acid, then purified on MAX columns. After extraction and purification, the supernatant was evaporated to dry nearly under a gentle stream of nitrogen at 40 °C. Formic acid-acetonitrile-water (0.1/30/70, v/v/v) was adjusted to 1.00 mL final volume. An aliquot (10 μL) was injected into the C18 column for separation with the mobile phase of acetonitrile and 0.5% formic acid in water at 0.25 mL min−1. Calibration curves were linear ranged from 10.00 ng mL−1 to 200.0 ng mL−1 for quinocetone and 3-methylquinoxaline-2-carboxylic acid, and 20.00 ng mL−1 to 400.0 ng mL−1 for dedioxoquinenone. Mean recoveries were 70%–89%, 73%–83% and 72%–84%, respectively. The limit of detection (LOD) was 1.00 μg kg−1, 1.00 μg kg−1 and 2.00 μg kg−1, and quantification (LOQ) were 2.00 μg kg−1, 2.00 μg kg−1 and 4.00 μg kg−1 for quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone. Based on the method above, the analytes were determined in Apostichopus japonicus, three fishes (including Ctenopharyngodon idellus, Crucian carp and Oreochromis mossambicus), Penaeus vannamei, Penaeus chinensis, and Chlamys farreri. The method shows good sensitivity, linearity, precision, and accuracy. In short, the proposed method was reliable for the determination of quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone in aquatic products.
建立了一种高效液相色谱-串联光谱(UHPLC-MS/MS)测定水产品中喹诺酮及其主要代谢物(3-甲基喹诺啉-2-羧酸和去二氧喹诺酮)的方法。样品用2.0 mol L−1盐酸提取，MAX柱纯化。提取和纯化后，上清液在40°C的温和氮气流下蒸发至几乎干燥。甲酸-乙腈-水(0.1/30/70,v/v/v)调节至终体积1.00 mL。在C18色谱柱中注入10 μL的等分物，流动相为乙腈和0.5%甲酸，流速为0.25 mL min - 1。喹诺酮和3-甲基喹诺啉-2-羧酸的校准曲线在10.00 ~ 200.0 ng mL−1范围内呈线性，二氧喹诺酮的校准曲线在20.00 ~ 400.0 ng mL−1范围内呈线性。平均加样回收率分别为70% ~ 89%、73% ~ 83%和72% ~ 84%。喹诺酮、3-甲基喹诺啉-2-羧酸和去二氧醌的检出限分别为1.00、1.00和2.00 μ kg - 1，定量限分别为2.00、2.00和4.00 μ kg - 1。根据上述方法，对日本刺参、三种鱼类(带鱼、鲫鱼和莫桑鱼)、凡纳对虾、中国对虾和法氏对虾进行了分析。该方法具有良好的灵敏度、线性度、精密度和准确度。总之，该方法可用于水产品中喹诺酮、3-甲基喹诺啉-2-羧酸和去二氧喹诺酮的测定。
{"title":"Validation and quantification of a UPLC-MS/MS method for the simultaneous determination of quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) in aquatic products","authors":"Xiuhui Tian, Dianfeng Han, Yanmei Cui, L. Ren, Fang Jiang, Hui Huang, Xianghong Gong, Jingling Xue, Jiawei Li, Huihui Liu, Yingjiang Xu, Xiaojun Luo, Xiaojing Liu, Xiuzhen Zhang","doi":"10.1556/1326.2022.01001","DOIUrl":"https://doi.org/10.1556/1326.2022.01001","url":null,"abstract":"\u0000 A sensitive and validated method for determining quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) was established in aquatic products using ultra-high-performance liquid chromatography-tandem spectrometry (UHPLC-MS/MS). Samples were extracted with 2.0 mol L−1 hydrochloric acid, then purified on MAX columns. After extraction and purification, the supernatant was evaporated to dry nearly under a gentle stream of nitrogen at 40 °C. Formic acid-acetonitrile-water (0.1/30/70, v/v/v) was adjusted to 1.00 mL final volume. An aliquot (10 μL) was injected into the C18 column for separation with the mobile phase of acetonitrile and 0.5% formic acid in water at 0.25 mL min−1. Calibration curves were linear ranged from 10.00 ng mL−1 to 200.0 ng mL−1 for quinocetone and 3-methylquinoxaline-2-carboxylic acid, and 20.00 ng mL−1 to 400.0 ng mL−1 for dedioxoquinenone. Mean recoveries were 70%–89%, 73%–83% and 72%–84%, respectively. The limit of detection (LOD) was 1.00 μg kg−1, 1.00 μg kg−1 and 2.00 μg kg−1, and quantification (LOQ) were 2.00 μg kg−1, 2.00 μg kg−1 and 4.00 μg kg−1 for quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone. Based on the method above, the analytes were determined in Apostichopus japonicus, three fishes (including Ctenopharyngodon idellus, Crucian carp and Oreochromis mossambicus), Penaeus vannamei, Penaeus chinensis, and Chlamys farreri. The method shows good sensitivity, linearity, precision, and accuracy. In short, the proposed method was reliable for the determination of quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone in aquatic products.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42809893","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}
Qianchun Zhang, Yan Chen, Yanqun Yang, Yulan Liu, Ming Wen, Xingyi Wang
A novel method was established for analysing trace four acidic phytohormones, namely, indole-3-acetic acid, 3-indolebutyric acid, abscisic acid, and 1-naphthylacetic acid, using magnetic ordered mesoporous carbon (MOMC). MOMC was facilely synthesised via self-assembly strategy with a direct carbonisation process. The properties of MOMC were characterised using various instruments. MOMC exhibited excellent adsorption capacity towards the analytes. Various critical parameters which may influence the enrichment efficiency were evaluated, including amount of MOMC, extraction conditions, and desorption conditions. An efficient method based on MOMC magnetic solid-phase extraction coupled with ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) was developed to analyse the trace four acidic phytohormones, with good correlation coefficients (R 2 = 0.9965–0.9998) and low limits of detection (0.13–9.7 ng L−1, S/N = 3). Trace acidic phytohormones in Agaricus bisporus and Hypsizygus marmoreus samples were determined with satisfactory recoveries (91.8–108%) and reproducibility (2.6–6.3%). The features indicated that MOMC provides an efficient platform for mushroom sampling; the developed method is convenient, promising, and sensitive for the detection of trace phytohormones in complicated mushroom samples.
利用磁性有序介孔碳（MOMC）建立了一种分析痕量四种酸性植物激素，即吲哚-3-乙酸、3-吲哚丁酸、脱落酸和1-萘乙酸的新方法。MOMC是通过自组装策略和直接碳化过程容易合成的。使用各种仪器对MOMC的性质进行了表征。MOMC对分析物具有良好的吸附性能。评估了可能影响富集效率的各种关键参数，包括MOMC的量、提取条件和解吸条件。开发了一种基于MOMC磁性固相萃取结合超高效液相色谱-串联质谱（UHPLC–MS/MS）的有效方法来分析痕量四种酸性植物激素，其相关系数良好（R2=0.965–0.9998），检测限较低（0.13–9.7 ng L−1，S/N=3）。测定了双孢蘑菇和蘑菇样品中的微量酸性植物激素，回收率为91.8-108%，重现性为2.6-6.3%；该方法简便、快速、灵敏，可用于复杂蘑菇样品中微量植物激素的检测。
{"title":"Fabrication of magnetic ordered mesoporous carbon for quantitative analysis of acidic phytohormones in mushroom samples prior to their determination by ultra-high-performance liquid chromatography–tandem mass spectrometry","authors":"Qianchun Zhang, Yan Chen, Yanqun Yang, Yulan Liu, Ming Wen, Xingyi Wang","doi":"10.1556/1326.2022.01022","DOIUrl":"https://doi.org/10.1556/1326.2022.01022","url":null,"abstract":"\u0000 A novel method was established for analysing trace four acidic phytohormones, namely, indole-3-acetic acid, 3-indolebutyric acid, abscisic acid, and 1-naphthylacetic acid, using magnetic ordered mesoporous carbon (MOMC). MOMC was facilely synthesised via self-assembly strategy with a direct carbonisation process. The properties of MOMC were characterised using various instruments. MOMC exhibited excellent adsorption capacity towards the analytes. Various critical parameters which may influence the enrichment efficiency were evaluated, including amount of MOMC, extraction conditions, and desorption conditions. An efficient method based on MOMC magnetic solid-phase extraction coupled with ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) was developed to analyse the trace four acidic phytohormones, with good correlation coefficients (R\u0000 2 = 0.9965–0.9998) and low limits of detection (0.13–9.7 ng L−1, S/N = 3). Trace acidic phytohormones in Agaricus bisporus and Hypsizygus marmoreus samples were determined with satisfactory recoveries (91.8–108%) and reproducibility (2.6–6.3%). The features indicated that MOMC provides an efficient platform for mushroom sampling; the developed method is convenient, promising, and sensitive for the detection of trace phytohormones in complicated mushroom samples.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-02-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44860876","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}
B. Ivković, Ivana Milutinović, O. Čudina, B. Marković
Gentamicin sulfate is a potent broad spectrum aminoglycoside antibiotic which is used against Gram-positive and Gram-negative bacteria. A simple, isocratic HPLC method for separation, identification and determination of gentamicin and parabens (methylparaben and propylparaben) was developed and validated. To our knowledge there is no report about simultaneous determination of those three analytes in pharmaceutical products. The optimum chromatographic conditions were achieved on CN column with a mobile phase consisting of 0.15% triethylamine in 10 mM KH2PO4 aqueous solution (final pH 3.0 adjusted with H3PO4) and methanol in the ratio 70:30 (v/v), providing selective quantification of analytes within 5 min. The method was successfully validated according to ICH guidelines acceptance criteria in terms of selectivity, linearity, accuracy, precision and robustness. The linearity of the method was proved in defined concentrations ranges for gentamicin (0.32–1.04 mg mL−1), methylparaben (0.0072–0.0234 mg mL−1) and propylparaben (0.0008–0.0026 mg mL−1). Relative standard deviations calculated for all analytes in precision testing were <2% (analysis repeatability) and <3% (intermediate precision). Recovery values were between 98.87% and 101.67%. Chromatographic parameters are not significantly influenced by small variations of column temperature, pH and molarity of KH2PO4. Finally, the method was successfully applied for quantitative determination of gentamicin and parabens in commercially available solution for injection. Proposed HPLC method is found to be promising in terms of simplicity, analysis times and non-use of derivatization and ion-pair agents.
{"title":"A new simple liquid chromatographic assay for gentamicin in presence of methylparaben and propylparaben","authors":"B. Ivković, Ivana Milutinović, O. Čudina, B. Marković","doi":"10.1556/1326.2022.00999","DOIUrl":"https://doi.org/10.1556/1326.2022.00999","url":null,"abstract":"\u0000 Gentamicin sulfate is a potent broad spectrum aminoglycoside antibiotic which is used against Gram-positive and Gram-negative bacteria. A simple, isocratic HPLC method for separation, identification and determination of gentamicin and parabens (methylparaben and propylparaben) was developed and validated. To our knowledge there is no report about simultaneous determination of those three analytes in pharmaceutical products. The optimum chromatographic conditions were achieved on CN column with a mobile phase consisting of 0.15% triethylamine in 10 mM KH2PO4 aqueous solution (final pH 3.0 adjusted with H3PO4) and methanol in the ratio 70:30 (v/v), providing selective quantification of analytes within 5 min. The method was successfully validated according to ICH guidelines acceptance criteria in terms of selectivity, linearity, accuracy, precision and robustness. The linearity of the method was proved in defined concentrations ranges for gentamicin (0.32–1.04 mg mL−1), methylparaben (0.0072–0.0234 mg mL−1) and propylparaben (0.0008–0.0026 mg mL−1). Relative standard deviations calculated for all analytes in precision testing were <2% (analysis repeatability) and <3% (intermediate precision). Recovery values were between 98.87% and 101.67%. Chromatographic parameters are not significantly influenced by small variations of column temperature, pH and molarity of KH2PO4. Finally, the method was successfully applied for quantitative determination of gentamicin and parabens in commercially available solution for injection. Proposed HPLC method is found to be promising in terms of simplicity, analysis times and non-use of derivatization and ion-pair agents.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-02-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43448797","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}
B. Ivković, Milkica Crevar, Anka Cvetanović, Katarina Ubavkić, B. Marković
Corticosteroids are anti-inflammatory and immunosuppressant drugs. Topical corticosteroids formulations (ointments, creams, gels) are used in the treatment of different types of dermatitis and urticaria. Considering their therapeutic and whitening effects, they are frequently used for counterfeiting of cosmetic products. Corticosteroids can cause different local and systemic side effects. HPLC method is often chosen for their analysis, because it is selective, sensitive, precise, simple and fast. The aim of this study was optimization and validation of RP-HPLC method with UV detection for determination of trace levels of corticosteroids in ambiphilic creams. This method is used for qualitative and quantitative analysis of evaluated corticosteroids. Mometasone furoate, hydrocortisone acetate, fluocinonide, fluocinolone acetonide, betamethasone, betamethasone dipropionate and triamcinolone acetonide were evaluated. Separation was performed on Inertsil® ODS-3V 250 × 4.6 mm, 5 μm chromatographic column. Mobile phase was mixture of acetonitrile and water 50:50 (v/v) with gradient elution and flow rate 1 mL min−1. Column temperature was held on 40 °C and UV detection was performed at 240 nm. Selectivity, linearity, accuracy, precision and limit of quantification (LOQ) were evaluated. Method is selective because ambiphilic cream base peaks and corticosteroids peaks were not overlapping. Linearity was confirmed since correlation coefficient was 1 for all compounds. Accuracy and precision were evaluated for hydrocortisone acetate and betamethasone dipropionate. Determined Recovery values were in range of 70–130%. Both RSD values (21.46% and 9.59%) were lower than 30%. Method is highly sensitive since LOQ concentrations were in ng mL−1 range. All evaluated parameters of validation were in accordance with regulatory requirements. Validated RP-HPLC method can be used for qualitative and quantitative analysis of selected corticosteroids in ambiphilic creams.
皮质类固醇是抗炎和免疫抑制药物。局部皮质类固醇制剂(软膏、乳膏、凝胶)用于治疗不同类型的皮炎和荨麻疹。考虑到它们的治疗和美白效果，它们经常被用于假冒化妆品。皮质类固醇可引起不同的局部和全身副作用。高效液相色谱法具有选择性好、灵敏度高、精密度高、简便、快速等优点。本研究的目的是优化和验证反相高效液相色谱-紫外检测法测定两亲性面霜中微量皮质激素的含量。该方法可用于评价的皮质类固醇的定性和定量分析。评价糠酸莫米松、醋酸氢化可的松、氟西尼德、醋酸氟西诺酮、倍他米松、二丙酸倍他米松和曲安奈德。色谱柱为Inertsil®ODS-3V 250 × 4.6 mm, 5 μm。流动相为乙腈与水的混合物50:50 (v/v)，梯度洗脱，流速1 mL min - 1。柱温保持在40℃，紫外检测波长240 nm。对该方法的选择性、线性、准确度、精密度和定量限进行了评价。方法是选择性的，因为两亲性乳膏底峰和皮质激素峰不重叠。所有化合物的相关系数均为1，证实了线性关系。评价醋酸氢化可的松和二丙酸倍他米松的准确度和精密度。测定的回收率范围为70-130%。RSD值分别为21.46%和9.59%，均小于30%。LOQ浓度在ng mL−1范围内，灵敏度高。所有评价的验证参数均符合法规要求。经验证的反相高效液相色谱法可用于两亲性乳膏中所选皮质激素的定性和定量分析。
{"title":"Development and validation of RP-HPLC method for quantification of trace levels of topical corticosteroids in ambiphilic cream","authors":"B. Ivković, Milkica Crevar, Anka Cvetanović, Katarina Ubavkić, B. Marković","doi":"10.1556/1326.2021.00998","DOIUrl":"https://doi.org/10.1556/1326.2021.00998","url":null,"abstract":"\u0000 Corticosteroids are anti-inflammatory and immunosuppressant drugs. Topical corticosteroids formulations (ointments, creams, gels) are used in the treatment of different types of dermatitis and urticaria. Considering their therapeutic and whitening effects, they are frequently used for counterfeiting of cosmetic products. Corticosteroids can cause different local and systemic side effects. HPLC method is often chosen for their analysis, because it is selective, sensitive, precise, simple and fast.\u0000 The aim of this study was optimization and validation of RP-HPLC method with UV detection for determination of trace levels of corticosteroids in ambiphilic creams. This method is used for qualitative and quantitative analysis of evaluated corticosteroids.\u0000 Mometasone furoate, hydrocortisone acetate, fluocinonide, fluocinolone acetonide, betamethasone, betamethasone dipropionate and triamcinolone acetonide were evaluated. Separation was performed on Inertsil® ODS-3V 250 × 4.6 mm, 5 μm chromatographic column. Mobile phase was mixture of acetonitrile and water 50:50 (v/v) with gradient elution and flow rate 1 mL min−1. Column temperature was held on 40 °C and UV detection was performed at 240 nm.\u0000 Selectivity, linearity, accuracy, precision and limit of quantification (LOQ) were evaluated. Method is selective because ambiphilic cream base peaks and corticosteroids peaks were not overlapping. Linearity was confirmed since correlation coefficient was 1 for all compounds. Accuracy and precision were evaluated for hydrocortisone acetate and betamethasone dipropionate. Determined Recovery values were in range of 70–130%. Both RSD values (21.46% and 9.59%) were lower than 30%. Method is highly sensitive since LOQ concentrations were in ng mL−1 range.\u0000 All evaluated parameters of validation were in accordance with regulatory requirements. Validated RP-HPLC method can be used for qualitative and quantitative analysis of selected corticosteroids in ambiphilic creams.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42582359","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}
Vendula Kubíčková, Z. Racova, J. Strojil, P. Šantavý, K. Urbanek
The accurate, simple, and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of an antibiotic ampicillin (AMP) in human blood plasma. The SPE extraction was used for the sample preparation. Chromatographic separation was accomplished by a mobile phase containing 15 mM monopotassium phosphate solution of pH 3.3 and methanol (75:25, v/v) in an isocratic mode at a flow rate of 1.4 mL min−1 at 30 °C. The separation was evaluated on a column with a new polar-endcapped C18 stationary phase Arion® Polar C18 or well-known phase Luna® Omega Polar C18. Excellent linearity (R 2 0.9998) was shown over range 10–300 mg L−1 with mean percentage recovery 90%. Peak shapes were symmetrical in both columns, Arion® Polar C18 and Luna® Omega Polar C18, with asymmetry factor of 1.0 and 1.4, tailing factor of 1.0 and 1.2, and retention factor of 4.6 and 5.6, respectively. The Arion® Polar C18 was almost 1.4-fold more effective than Luna® Omega Polar C18 phase. The LOQ for ampicillin was achieved 10 mg L−1 for Luna® Omega Polar C18 and 5 mg L−1 for Arion® Polar C18 using 20 µL of a solution containing 0.24 mg mL−1 of cephalexin as an internal standard. A number of articles dealing with the determination of ampicillin is limited, therefore, this study showed the HPLC method suitable for the determination of AMP in human blood plasma from patient who underwent elective cardiac surgical revascularization. In addition, the determination of AMP was also performed for the first time using an Arion® Polar C18 column, which effectively separated AMP from other compounds present in human blood plasma. This new polar-endcapped phase can help in separation of polar antibiotics or other polar compounds, which are unsuccessfully separated on conventional C18 column, and thus can help during method development.
{"title":"Separation of ampicillin on polar-endcapped phase: Development of the HPLC method to achieve its correct dosage in cardiac surgery","authors":"Vendula Kubíčková, Z. Racova, J. Strojil, P. Šantavý, K. Urbanek","doi":"10.1556/1326.2021.00957","DOIUrl":"https://doi.org/10.1556/1326.2021.00957","url":null,"abstract":"\u0000 The accurate, simple, and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of an antibiotic ampicillin (AMP) in human blood plasma. The SPE extraction was used for the sample preparation. Chromatographic separation was accomplished by a mobile phase containing 15 mM monopotassium phosphate solution of pH 3.3 and methanol (75:25, v/v) in an isocratic mode at a flow rate of 1.4 mL min−1 at 30 °C. The separation was evaluated on a column with a new polar-endcapped C18 stationary phase Arion® Polar C18 or well-known phase Luna® Omega Polar C18. Excellent linearity (R\u0000 2 0.9998) was shown over range 10–300 mg L−1 with mean percentage recovery 90%. Peak shapes were symmetrical in both columns, Arion® Polar C18 and Luna® Omega Polar C18, with asymmetry factor of 1.0 and 1.4, tailing factor of 1.0 and 1.2, and retention factor of 4.6 and 5.6, respectively. The Arion® Polar C18 was almost 1.4-fold more effective than Luna® Omega Polar C18 phase. The LOQ for ampicillin was achieved 10 mg L−1 for Luna® Omega Polar C18 and 5 mg L−1 for Arion® Polar C18 using 20 µL of a solution containing 0.24 mg mL−1 of cephalexin as an internal standard.\u0000 A number of articles dealing with the determination of ampicillin is limited, therefore, this study showed the HPLC method suitable for the determination of AMP in human blood plasma from patient who underwent elective cardiac surgical revascularization. In addition, the determination of AMP was also performed for the first time using an Arion® Polar C18 column, which effectively separated AMP from other compounds present in human blood plasma. This new polar-endcapped phase can help in separation of polar antibiotics or other polar compounds, which are unsuccessfully separated on conventional C18 column, and thus can help during method development.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-01-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41970064","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}
Gas chromatography-ion mobility spectrometry (GC-IMS) is an emerging analytical technique that has the advantages of fast response, high sensitivity, simple operation, and low cost. The combination of the fast speed and resolution of GC with the high sensitivity of IMS makes GC-IMS play an important role in the detection of food volatile substances. This paper focuses on the basic principles and future development trend, and the comparative analysis of the functions, similarities and differences of GC-IMS, GC-MS and electronic nose in the detection of common volatile compounds. A comprehensive introduction to the main application of GC-IMS in food volatile components: fingerprint identification of sample differences and detection of characteristic compounds. On the basis of perfecting the spectral library, GC-IMS will have broad development prospects in food authentication, origin identification, process optimization and product classification, especially in the analysis and identification of trace volatile food flavor substances.
{"title":"Application of gas chromatography-ion mobility spectrometry in the analysis of food volatile components","authors":"Xuelian Yang, Tianxin Zhang, Dongdong Yang, Jianchun Xie","doi":"10.1556/1326.2022.01005","DOIUrl":"https://doi.org/10.1556/1326.2022.01005","url":null,"abstract":"\u0000 Gas chromatography-ion mobility spectrometry (GC-IMS) is an emerging analytical technique that has the advantages of fast response, high sensitivity, simple operation, and low cost. The combination of the fast speed and resolution of GC with the high sensitivity of IMS makes GC-IMS play an important role in the detection of food volatile substances. This paper focuses on the basic principles and future development trend, and the comparative analysis of the functions, similarities and differences of GC-IMS, GC-MS and electronic nose in the detection of common volatile compounds. A comprehensive introduction to the main application of GC-IMS in food volatile components: fingerprint identification of sample differences and detection of characteristic compounds. On the basis of perfecting the spectral library, GC-IMS will have broad development prospects in food authentication, origin identification, process optimization and product classification, especially in the analysis and identification of trace volatile food flavor substances.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-01-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42402684","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 simple, rapid, and environmentally friendly sample preparation method for pyrethroids determination in cereals using cyclodextrin-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplets coupled with high-performance liquid chromatography was established. The cereal samples were extracted with acetonitrile, cleaned up, and concentrated by green extractant menthol via γ-cyclodextrin assisted extraction process. The extractant menthol dispersed as fine droplets in the cyclodextrin solution and then solidified at room temperature for efficient extraction and convenient collection. The optimized method provided good linearity in the range of 0.01–10 mg kg−1 with limits of detection of 3.5–9.5 μg kg−1. The fortified recoveries of three pyrethroids (i.e., lambda-cyhalothrin, deltamethrin, and bifenthrin) in four cereals (i.e., rice, wheat, maize, and millet) at three levels were in the range of 77.6–101.6% with relative standard deviations of 0.6–6.6%. Overall, the proposed method can be successfully applied for the determination of pyrethroids in cereals.
{"title":"Cyclodextrin-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplets coupled with HPLC for the determination of pyrethroid residues in cereals","authors":"Haijuan Jiang, Xinyuan Bi, Xin Huang, Xingle Guo, Ziyu Zou, Ying Li, Xu Jing, Junxue Wu","doi":"10.1556/1326.2021.00991","DOIUrl":"https://doi.org/10.1556/1326.2021.00991","url":null,"abstract":"\u0000 A simple, rapid, and environmentally friendly sample preparation method for pyrethroids determination in cereals using cyclodextrin-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplets coupled with high-performance liquid chromatography was established. The cereal samples were extracted with acetonitrile, cleaned up, and concentrated by green extractant menthol via γ-cyclodextrin assisted extraction process. The extractant menthol dispersed as fine droplets in the cyclodextrin solution and then solidified at room temperature for efficient extraction and convenient collection. The optimized method provided good linearity in the range of 0.01–10 mg kg−1 with limits of detection of 3.5–9.5 μg kg−1. The fortified recoveries of three pyrethroids (i.e., lambda-cyhalothrin, deltamethrin, and bifenthrin) in four cereals (i.e., rice, wheat, maize, and millet) at three levels were in the range of 77.6–101.6% with relative standard deviations of 0.6–6.6%. Overall, the proposed method can be successfully applied for the determination of pyrethroids in cereals.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42783028","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}
K. Palandurkar, Richie Bhandre, S. H. Boddu, Minal T. Harde, Sameer S Lakade, Ujjwala Y. Kandekar, Prashant Waghmare
A systematic DoE and Analytical Quality by Design (AQbD) approach was utilized for the development and validation of a novel stability indicating high-performance thin–layer chromatographic (HPTLC) method for Rivaroxaban (RBN) estimation in bulk and marketed formulation. A D-optimal design was used to screen the effect of solvents, volume of solvents, time from spotting to development and time for development to scanning. ANOVA results and Pareto chart revealed that toluene, methanol, water and saturation time had an impact on retention time. The critical method and material attributes were further screened by Box-Behnken design (BBD) to achieve optimal chromatographic condition. A stress degradation study was carried out and structure of major alkaline degradant was elaborated. According to the design space, a control strategy was used with toluene: methanol: water (6:2:2) and the saturation time was 15 min. A retention factor (RF) of 0.59 ± 0.05 was achieved for RBN using chromatographic plate precoated with silica gel at detection wavelength 282 nm with optimized conditions. The linear calibration curve was achieved in the concentration range of 200–1,200 ng/band with r 2 > 0.998 suggesting good coordination between analyte concentration and peak areas. The quadratic model was demonstrated as the best fit model and no interaction was noted between CMAs. The optimized HPTLC method was validated critically as stated in International Conference on Harmonization (ICH) Q2 (R1) guideline and implemented successfully for stress degradation study of RBN. The developed HPTLC method obtained through AQbD application was potentially able to resolve all degradants of RBN achieved through forced degradation study. The obtained results demonstrate that a scientific AQbD approach implementation in HPTLC method development and stress degradation study drastically minimizes the number of trials in experiments, ultimately time and cost of analysis could be minimized.
{"title":"Quality risk assessment and DoE – Practiced validated stability-indicating chromatographic method for quantification of Rivaroxaban in bulk and tablet dosage form","authors":"K. Palandurkar, Richie Bhandre, S. H. Boddu, Minal T. Harde, Sameer S Lakade, Ujjwala Y. Kandekar, Prashant Waghmare","doi":"10.1556/1326.2021.00978","DOIUrl":"https://doi.org/10.1556/1326.2021.00978","url":null,"abstract":"\u0000 A systematic DoE and Analytical Quality by Design (AQbD) approach was utilized for the development and validation of a novel stability indicating high-performance thin–layer chromatographic (HPTLC) method for Rivaroxaban (RBN) estimation in bulk and marketed formulation. A D-optimal design was used to screen the effect of solvents, volume of solvents, time from spotting to development and time for development to scanning. ANOVA results and Pareto chart revealed that toluene, methanol, water and saturation time had an impact on retention time. The critical method and material attributes were further screened by Box-Behnken design (BBD) to achieve optimal chromatographic condition. A stress degradation study was carried out and structure of major alkaline degradant was elaborated. According to the design space, a control strategy was used with toluene: methanol: water (6:2:2) and the saturation time was 15 min. A retention factor (RF) of 0.59 ± 0.05 was achieved for RBN using chromatographic plate precoated with silica gel at detection wavelength 282 nm with optimized conditions. The linear calibration curve was achieved in the concentration range of 200–1,200 ng/band with r\u0000 2 > 0.998 suggesting good coordination between analyte concentration and peak areas. The quadratic model was demonstrated as the best fit model and no interaction was noted between CMAs. The optimized HPTLC method was validated critically as stated in International Conference on Harmonization (ICH) Q2 (R1) guideline and implemented successfully for stress degradation study of RBN. The developed HPTLC method obtained through AQbD application was potentially able to resolve all degradants of RBN achieved through forced degradation study. The obtained results demonstrate that a scientific AQbD approach implementation in HPTLC method development and stress degradation study drastically minimizes the number of trials in experiments, ultimately time and cost of analysis could be minimized.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42402893","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}
Libin Wang, Kun Shang, Xiaorui Zhang, Xin-Yuan Zhang, Tian Feng, Xu Xiaohui, Fang Wang
A sensitive and accurate LC-MS/MS method was developed and validated for the simultaneous quantification of rivaroxaban (RIV) and sitagliptin (SIT) in rat plasma using apixaban as internal standard (IS). An Agilent Eclipse plus C18 column (2.1 × 100 mm, 3.5 µm, Agilent) was used for chromatographic separation with isocratic elution. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 436.8→144.9 for RIV, m/z 407.7→173.8 for SIT, m/z 459.8→442.8 for IS. The procedure of method validation included selectivity, linearity, precision, accuracy, matrix effect, extraction recovery and stability were conducted according to the guidelines of EMA and FDA. The results indicated that no obvious drug-drug interactions occurred might be owing to their differences in metabolic pathways.
建立了以阿哌沙班为内标(IS)同时定量大鼠血浆中利伐沙班(RIV)和西格列汀(SIT)的灵敏、准确的LC-MS/MS方法。采用Agilent Eclipse加C18色谱柱(2.1 × 100 mm, 3.5µm, Agilent)，等密度洗脱进行色谱分离。多反应监测(MRM)采用正离子ESI模式监测RIV的m/z 436.8→144.9、SIT的m/z 407.7→173.8、IS的m/z 459.8→442.8的离子跃迁。方法验证包括选择性、线性度、精密度、准确度、基质效应、提取回收率和稳定性，验证过程按照EMA和FDA的指导原则进行。结果表明，两种药物之间没有发生明显的相互作用，这可能是由于它们的代谢途径不同所致。
{"title":"Simultaneous determination of rivaroxaban and sitagliptin in rat plasma by LC–MS/MS and its application to pharmacokinetic drug-drug interaction study","authors":"Libin Wang, Kun Shang, Xiaorui Zhang, Xin-Yuan Zhang, Tian Feng, Xu Xiaohui, Fang Wang","doi":"10.1556/1326.2021.00988","DOIUrl":"https://doi.org/10.1556/1326.2021.00988","url":null,"abstract":"\u0000 A sensitive and accurate LC-MS/MS method was developed and validated for the simultaneous quantification of rivaroxaban (RIV) and sitagliptin (SIT) in rat plasma using apixaban as internal standard (IS). An Agilent Eclipse plus C18 column (2.1 × 100 mm, 3.5 µm, Agilent) was used for chromatographic separation with isocratic elution. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 436.8→144.9 for RIV, m/z 407.7→173.8 for SIT, m/z 459.8→442.8 for IS. The procedure of method validation included selectivity, linearity, precision, accuracy, matrix effect, extraction recovery and stability were conducted according to the guidelines of EMA and FDA. The results indicated that no obvious drug-drug interactions occurred might be owing to their differences in metabolic pathways.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2021-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44260605","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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