D. Qi, Yingying Sun, Bingying Hu, Hai An, Haiyang Lin, Jinjun Fang, Yang Wei
SZJ-1207 is an antidepressant natural product with a steroidal structure extracted from Stephanotis mucronata. It is a novel antidepressant candidate molecule and all its pharmacokinetic properties have not been reported. In this pharmacokinetic study in mice following oral administration, an accurate and sensitive UPLC-MS/MS method was established and evaluated to measure SZJ-1207 concentrations in mouse plasma and brain samples. The results provide information regarding the pharmacokinetics of SZJ-1207 as a potential antidepressant.
{"title":"UPLC-MS/MS analysis of SZJ-1207 in mouse plasma and brain and application in pharmacokinetic studies","authors":"D. Qi, Yingying Sun, Bingying Hu, Hai An, Haiyang Lin, Jinjun Fang, Yang Wei","doi":"10.1556/1326.2022.01102","DOIUrl":"https://doi.org/10.1556/1326.2022.01102","url":null,"abstract":"SZJ-1207 is an antidepressant natural product with a steroidal structure extracted from Stephanotis mucronata. It is a novel antidepressant candidate molecule and all its pharmacokinetic properties have not been reported. In this pharmacokinetic study in mice following oral administration, an accurate and sensitive UPLC-MS/MS method was established and evaluated to measure SZJ-1207 concentrations in mouse plasma and brain samples. The results provide information regarding the pharmacokinetics of SZJ-1207 as a potential antidepressant.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45255314","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}
D. Obradović, Ivana Pešić, Marija Čarapić, S. Lazović, D. Agbaba
The retention behaviour of scopolamine (hyoscine) and its related compounds (norhyoscine, atropine, homatropine, and noratropine) was investigated on the silica-based HPLC stationary phase. The retention of investigated tropane alkaloids was interpreted by using the Soczewiński-Wachtmeister equation. A high correlation between the retention parameter (log k) and lipophilicity (log P) (R = 0.9923) confirms the significant influence of hydrophobic interactions on the retention behaviour of the aforementioned compounds. It was found that by increasing the acetonitrile fraction, a decrease in retention of the more polar epoxide derivatives (scopolamine, norhyoscine) and an increase in retention of the more lipophilic derivatives (atropine, noratropine, homatropine) is obtained. The best separation of the tropane alkaloids was achieved by a simple procedure that involved a mobile phase composed of acetonitrile and 40 mM ammonium acetate/0.05% TEA, pH 6.5; 50:50 v/v. Selected conditions were assumed for the determination of scopolamine hydrochloride in the eye drops (Scopolamini hydrobromidum 0.25%). The method was validated and it was found as selective, sensitive, precise, accurate, and robust for the further qualitative analysis of the scopolamine-related compounds.
{"title":"Analysis of scopolamine and its related substances by means of high-performance liquid chromatography","authors":"D. Obradović, Ivana Pešić, Marija Čarapić, S. Lazović, D. Agbaba","doi":"10.1556/1326.2022.01107","DOIUrl":"https://doi.org/10.1556/1326.2022.01107","url":null,"abstract":"The retention behaviour of scopolamine (hyoscine) and its related compounds (norhyoscine, atropine, homatropine, and noratropine) was investigated on the silica-based HPLC stationary phase. The retention of investigated tropane alkaloids was interpreted by using the Soczewiński-Wachtmeister equation. A high correlation between the retention parameter (log k) and lipophilicity (log P) (R = 0.9923) confirms the significant influence of hydrophobic interactions on the retention behaviour of the aforementioned compounds. It was found that by increasing the acetonitrile fraction, a decrease in retention of the more polar epoxide derivatives (scopolamine, norhyoscine) and an increase in retention of the more lipophilic derivatives (atropine, noratropine, homatropine) is obtained. The best separation of the tropane alkaloids was achieved by a simple procedure that involved a mobile phase composed of acetonitrile and 40 mM ammonium acetate/0.05% TEA, pH 6.5; 50:50 v/v. Selected conditions were assumed for the determination of scopolamine hydrochloride in the eye drops (Scopolamini hydrobromidum 0.25%). The method was validated and it was found as selective, sensitive, precise, accurate, and robust for the further qualitative analysis of the scopolamine-related compounds.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-12-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46500174","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}
In this study, we report the systematic approach for characterization of two major degradant impurities, which are not listed in any compendia and were formed during the stability studies of Dihydroergotamine mesylate injection (DHE). An ion-pair UPLC chromatographic method was developed to quantify the related substances present in the DHE injection drug product. The same was used to monitor the impurity profiling during its stability. The two unknown impurities were observed at RRT about 0.08 (Impurity-1) and RRT about 0.80 (Impurity-5) and found to be significantly increasing on stability. Forced degradation studies revealed the nature of the impurity and conditions required for enriching them. A Mass compatible HPLC method was developed to quantify only these two impurities using 25% ammonia and formic acid in water. Their mass numbers were identified using LC MS/MS with triple quadruple mass spectrometer coupled with a HPLC. These two impurities were then isolated from enriched products using preparative HPLC. These impurities were then characterized using Mass and NMR analysis along with Q-TOF elemental analysis.
{"title":"Isolation and characterization of major degradants in dihydroergotamine injection","authors":"Praveen Basappa, U. Ms, V. Dama","doi":"10.1556/1326.2022.01095","DOIUrl":"https://doi.org/10.1556/1326.2022.01095","url":null,"abstract":"In this study, we report the systematic approach for characterization of two major degradant impurities, which are not listed in any compendia and were formed during the stability studies of Dihydroergotamine mesylate injection (DHE). An ion-pair UPLC chromatographic method was developed to quantify the related substances present in the DHE injection drug product. The same was used to monitor the impurity profiling during its stability. The two unknown impurities were observed at RRT about 0.08 (Impurity-1) and RRT about 0.80 (Impurity-5) and found to be significantly increasing on stability. Forced degradation studies revealed the nature of the impurity and conditions required for enriching them. A Mass compatible HPLC method was developed to quantify only these two impurities using 25% ammonia and formic acid in water. Their mass numbers were identified using LC MS/MS with triple quadruple mass spectrometer coupled with a HPLC. These two impurities were then isolated from enriched products using preparative HPLC. These impurities were then characterized using Mass and NMR analysis along with Q-TOF elemental analysis.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-12-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42010689","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}
V. Dobričić, J. Savić, T. Tomašič, Martina Durcik, Nace Zidar, L. P. Mašič, J. Ilaš, D. Kikelj, O. Čudina
Bacterial DNA gyrase and topoisomerase IV control the topological state of DNA during replication and represent important antibacterial drug targets. To be successful as drug candidates, newly synthesized compounds must possess optimal lipophilicity, which enables efficient delivery to the site of action. In this study, retention behavior of twenty-three previously synthesized dual DNA gyrase and topoisomerase IV inhibitors was tested in RP-HPLC system, consisting of C8 column and acetonitrile/phosphate buffer (pH 5.5 and pH 7.4) mobile phase. logD was calculated at both pH values and the best correlation with logD was obtained for retention parameter φ0, indicating that this RP-HPLC system could be used as an alternative to the shake-flask determination of lipophilicity. Subsequent QSRR analysis revealed that intrinsic lipophilicity (logP) and molecular weight (bcutm13) have a positive, while solubility (bcutp3) has a negative influence on this retention parameter.
{"title":"High-performance liquid chromatography evaluation of lipophilicity and QSRR modeling of a series of dual DNA gyrase and topoisomerase IV inhibitors","authors":"V. Dobričić, J. Savić, T. Tomašič, Martina Durcik, Nace Zidar, L. P. Mašič, J. Ilaš, D. Kikelj, O. Čudina","doi":"10.1556/1326.2022.01096","DOIUrl":"https://doi.org/10.1556/1326.2022.01096","url":null,"abstract":"Bacterial DNA gyrase and topoisomerase IV control the topological state of DNA during replication and represent important antibacterial drug targets. To be successful as drug candidates, newly synthesized compounds must possess optimal lipophilicity, which enables efficient delivery to the site of action. In this study, retention behavior of twenty-three previously synthesized dual DNA gyrase and topoisomerase IV inhibitors was tested in RP-HPLC system, consisting of C8 column and acetonitrile/phosphate buffer (pH 5.5 and pH 7.4) mobile phase. logD was calculated at both pH values and the best correlation with logD was obtained for retention parameter φ0, indicating that this RP-HPLC system could be used as an alternative to the shake-flask determination of lipophilicity. Subsequent QSRR analysis revealed that intrinsic lipophilicity (logP) and molecular weight (bcutm13) have a positive, while solubility (bcutp3) has a negative influence on this retention parameter.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-12-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44524197","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}
Chun Chen, L. Lv, Yueying Huang, Mingzhu Gao, Xue Jiang, Xiaoying Ge, D. Zheng, L. Bao
The bark of Eucommia ulmoides and the roots of Achyranthes bidentata are commonly used in traditional Chinese medicine, and their pairing appears in many traditional Chinese medicine formulas as a recognized compatible unit. However, the changes and interactions of the main components of these two formulas when paired remain unclear, and there is currently no standard or method for their quality control and assessment of pharmacological effects.An optimized ultra-high-performance liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS/MS) method was established for the simultaneous identification of 10 components in E. ulmoides and A. bidentata using in vitro and in vivo models. Tributyltin methacrylate was the internal standard solution, and the blood samples were treated by an organic solvent precipitation method. Gradient elution was conducted on a C18 column at 25 °C with 0.1% formic acid water:acetonitrile as the mobile phase at a flow rate of 0.5 mL min−1. Dynamic multiple response monitoring was performed in negative-ion mode using an Agilent Jet Stream electrospray ionization ion source.In negative-ion detection mode, eucommiol exhibited a good response, and the isomers ginsenoside Ro and achyranthoside C could also be well separated. The developed method accurately detected the five components with a low blood content. Compared to controls, the levels of ginsenoside Ro, chikusetsusaponin Ⅳa, and achyranthoside C increased; the contents of geniposidic acid and pinoresinol diglucoside were unchanged; and the levels of eucommiol, geniposide, β-ecdysterone, genipin, and achyranthoside D decreased in vitro. In vivo, the contents of geniposidic acid, geniposide, pinoresinol diglucoside, and β-ecdysterone were reduced; the contents of eucommiol and ginsenoside Ro were unchanged; and those of achyranthoside D, chikusetsusaponin Ⅳa, and achyranthoside C increased compared to the corresponding levels in the internal control.A method for the quality control of the E. ulmoides-A. bidentata drug pair was established for the first time and the main components in 10 drug pairs could be determined simultaneously in vitro and in vivo. These findings show that the E. ulmoides and A. bidentata drug pair cause a compositional change, providing new ideas for the development of this combination to improve clinical efficacy.
杜仲的树皮和牛膝的根是常用的中药，它们的配对作为公认的相容单位出现在许多中药配方中。然而，这两种配方配对时主要成分的变化和相互作用尚不清楚，目前尚无质量控制和药理作用评估的标准或方法。建立了一种超高效液相色谱-四极杆质谱(UHPLC-MS/MS)优化方法，用于杜仲和刺草中10种成分的体外和体内同时鉴定。内标液为甲基丙烯酸三丁锡，血液样品采用有机溶剂沉淀法处理。在C18柱上梯度洗脱，25℃，0.1%甲酸水:乙腈为流动相，流速0.5 mL min - 1。使用Agilent Jet Stream电喷雾离子源在负离子模式下进行动态多响应监测。在负离子检测模式下，杜仲醇表现出良好的响应，人参皂苷Ro和牛蹄草苷C的异构体也能很好地分离。该方法能准确地检测出低血含量的五种成分。与对照组相比，人参皂苷Ro、七苦参皂苷Ⅳa和牛膝花苷C的含量增加;京尼平苷酸和松脂醇二葡萄糖苷含量不变;杜仲酚、京尼平苷、β-蜕皮酮、京尼平、牛膝花苷D含量降低。在体内，京尼平苷酸、京尼平苷、松脂醇二葡糖苷、β-蜕皮酮含量降低;杜仲酚和人参皂苷Ro含量不变;牛膝花苷D、菊糖皂苷Ⅳa、牛膝花苷C的含量较内控组相应水平升高。杜仲药材质量控制方法的研究。首次建立了Bidentata药物对，10个药物对的主要成分在体内外均可同时测定。上述结果表明杜仲与双叶杜仲药物对引起了药物组成的变化，为该组合的开发提供了新的思路，以提高临床疗效。
{"title":"Optimized ultra-high-performance liquid chromatography tandem mass spectrometry method for detecting compositional changes in Eucommia ulmoides and Achyranthes bidentata paired decoctions in vitro and in vivo","authors":"Chun Chen, L. Lv, Yueying Huang, Mingzhu Gao, Xue Jiang, Xiaoying Ge, D. Zheng, L. Bao","doi":"10.1556/1326.2022.01090","DOIUrl":"https://doi.org/10.1556/1326.2022.01090","url":null,"abstract":"The bark of Eucommia ulmoides and the roots of Achyranthes bidentata are commonly used in traditional Chinese medicine, and their pairing appears in many traditional Chinese medicine formulas as a recognized compatible unit. However, the changes and interactions of the main components of these two formulas when paired remain unclear, and there is currently no standard or method for their quality control and assessment of pharmacological effects.An optimized ultra-high-performance liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS/MS) method was established for the simultaneous identification of 10 components in E. ulmoides and A. bidentata using in vitro and in vivo models. Tributyltin methacrylate was the internal standard solution, and the blood samples were treated by an organic solvent precipitation method. Gradient elution was conducted on a C18 column at 25 °C with 0.1% formic acid water:acetonitrile as the mobile phase at a flow rate of 0.5 mL min−1. Dynamic multiple response monitoring was performed in negative-ion mode using an Agilent Jet Stream electrospray ionization ion source.In negative-ion detection mode, eucommiol exhibited a good response, and the isomers ginsenoside Ro and achyranthoside C could also be well separated. The developed method accurately detected the five components with a low blood content. Compared to controls, the levels of ginsenoside Ro, chikusetsusaponin Ⅳa, and achyranthoside C increased; the contents of geniposidic acid and pinoresinol diglucoside were unchanged; and the levels of eucommiol, geniposide, β-ecdysterone, genipin, and achyranthoside D decreased in vitro. In vivo, the contents of geniposidic acid, geniposide, pinoresinol diglucoside, and β-ecdysterone were reduced; the contents of eucommiol and ginsenoside Ro were unchanged; and those of achyranthoside D, chikusetsusaponin Ⅳa, and achyranthoside C increased compared to the corresponding levels in the internal control.A method for the quality control of the E. ulmoides-A. bidentata drug pair was established for the first time and the main components in 10 drug pairs could be determined simultaneously in vitro and in vivo. These findings show that the E. ulmoides and A. bidentata drug pair cause a compositional change, providing new ideas for the development of this combination to improve clinical efficacy.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44905685","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}
We developed and validated a sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry (2D-LC‒MS/MS) method to determine the concentration of mometasone furoate in human plasma after nasal spray administration. Isotopically labeled mometasone furoate-13C,d6 was used as an internal standard (IS). Plasma samples were prepared using a solid-phase extraction (SPE) method. With this 2D-LC strategy, the analytes were trapped in the first dimension (1D) column, and only judiciously selected portions of the 1D effluent were transferred to the second dimension (2D) column for further separation to obtain high-resolution information. MS/MS quantification was performed in positive ionization mode via multiple-reaction monitoring (MRM). This analytical method was fully validated according to related regulatory guidance, and the results showed that the method is robust and sensitive enough for pharmacokinetic investigation of mometasone furoate with satisfactory linearity from 0.25 to 30 pg mL−1. This method was successfully applied to a bioequivalence (BE) study of mometasone furoate aqueous nasal sprays in healthy volunteers.
{"title":"A sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry method for the determination of mometasone furoate in human plasma: Application for a bioequivalence study in nasal spray formulations","authors":"Leting Yang, Hongyi Yang, Hui-ru Xie, Hui Liu, Gangmin He, Wenjing Zhong, Ling Wang","doi":"10.1556/1326.2022.01088","DOIUrl":"https://doi.org/10.1556/1326.2022.01088","url":null,"abstract":"We developed and validated a sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry (2D-LC‒MS/MS) method to determine the concentration of mometasone furoate in human plasma after nasal spray administration. Isotopically labeled mometasone furoate-13C,d6 was used as an internal standard (IS). Plasma samples were prepared using a solid-phase extraction (SPE) method. With this 2D-LC strategy, the analytes were trapped in the first dimension (1D) column, and only judiciously selected portions of the 1D effluent were transferred to the second dimension (2D) column for further separation to obtain high-resolution information. MS/MS quantification was performed in positive ionization mode via multiple-reaction monitoring (MRM). This analytical method was fully validated according to related regulatory guidance, and the results showed that the method is robust and sensitive enough for pharmacokinetic investigation of mometasone furoate with satisfactory linearity from 0.25 to 30 pg mL−1. This method was successfully applied to a bioequivalence (BE) study of mometasone furoate aqueous nasal sprays in healthy volunteers.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41858685","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}
Wenqing Li, Z. Qian, Yuansheng Zou, Guoying Tan, Wenjia Li, Qing-Qing Lei, Run-feng Li, Dongming Lan
A simple, rapid, sensitive and eco-friendly liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of free cordycepin (3′-deoxyadenosine) and isocordycepin (2′-deoxyadenosine) in 10 kinds of Cordyceps samples. The samples were prepared by ultrasonic extraction at 75 °C for 30 min with boiling water as the extraction solvent. The LC separation was performed on an Agilent poroshell 120 SB-Aq C18 column (3.0 × 50 mm, 2.7 μm) in isocratic mode with an eco-friendly mobile phase (2% ethanol containing 0.2% acetic acid) at a flow rate of 0.6 mL min−1, and detected by MS/MS in positive mode with multiple reaction monitoring (MRM). The developed method showed good linearity (r > 0.9990), sensitivity (LODs = 0.04 pg, LOQ = 0.1 pg), precision (RSD ≤ 3.8%) and stability (RSD ≤ 3.6%). The recoveries of developed method were 94.4–109.5% (RSD ≤ 5.5%). Compared with reported methods, the current method was rapid (less than 35% analytical time), sensitive (more than 5 folds), and eco-friendly (less than 10 μL harmful organic solvent). 10 different kinds of Cordyceps samples (40 batches) were tested by the developed method. Codycepin was only found in Cordyceps millitaris and C. millitaris fruiting body, and isocordycepin was detected in Cordyceps sinensis and other 6 Cordyceps samples. The developed method would be an improved method for the quality evaluation of Cordyceps samples.
建立了一种简便、快速、灵敏、环保的液相色谱-串联质谱法（LC-MS/MS）同时测定10种虫草样品中游离虫草素（3′-脱氧腺苷）和异虫草素（2′-脱氧腺苷酸）的方法。样品通过75℃的超声波提取制备 °C持续30 min，用沸水作为提取溶剂。LC分离在Agilent poroshell 120 SB Aq C18柱（3.0 × 50 毫米，2.7 μm）与环保型流动相（含0.2%乙酸的2%乙醇）以0.6 mL min−1的流速在等度模式下进行检测，并通过MS/MS在阳性模式下进行多重反应监测（MRM）检测。该方法具有良好的线性（r＞0.9990）、灵敏度（LOD＝0.04） pg，LOQ=0.1 pg）、精密度（RSD≤3.8%）和稳定性（RSD≤3.6%）。该方法的回收率为94.4–109.5%（RSD≤5.5%）。与已报道的方法相比，该方法快速（分析时间小于35%）、灵敏（5倍以上）、环保（小于10 μL有害有机溶剂）。采用该方法对10个不同品种（40批次）的冬虫夏草样品进行了检测。虫草素仅在冬虫夏草和C.millitaris子实体中发现，在冬虫虫夏草等6个虫草样品中检测到异虫草素。所开发的方法将是一种改进的虫草样品质量评价方法。
{"title":"A simple, rapid, sensitive and eco-friendly LC-MS/MS method for simultaneous determination of free cordycepin and isocordycepin in 10 different kinds of Cordyceps","authors":"Wenqing Li, Z. Qian, Yuansheng Zou, Guoying Tan, Wenjia Li, Qing-Qing Lei, Run-feng Li, Dongming Lan","doi":"10.1556/1326.2022.01094","DOIUrl":"https://doi.org/10.1556/1326.2022.01094","url":null,"abstract":"A simple, rapid, sensitive and eco-friendly liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of free cordycepin (3′-deoxyadenosine) and isocordycepin (2′-deoxyadenosine) in 10 kinds of Cordyceps samples. The samples were prepared by ultrasonic extraction at 75 °C for 30 min with boiling water as the extraction solvent. The LC separation was performed on an Agilent poroshell 120 SB-Aq C18 column (3.0 × 50 mm, 2.7 μm) in isocratic mode with an eco-friendly mobile phase (2% ethanol containing 0.2% acetic acid) at a flow rate of 0.6 mL min−1, and detected by MS/MS in positive mode with multiple reaction monitoring (MRM). The developed method showed good linearity (r > 0.9990), sensitivity (LODs = 0.04 pg, LOQ = 0.1 pg), precision (RSD ≤ 3.8%) and stability (RSD ≤ 3.6%). The recoveries of developed method were 94.4–109.5% (RSD ≤ 5.5%). Compared with reported methods, the current method was rapid (less than 35% analytical time), sensitive (more than 5 folds), and eco-friendly (less than 10 μL harmful organic solvent). 10 different kinds of Cordyceps samples (40 batches) were tested by the developed method. Codycepin was only found in Cordyceps millitaris and C. millitaris fruiting body, and isocordycepin was detected in Cordyceps sinensis and other 6 Cordyceps samples. The developed method would be an improved method for the quality evaluation of Cordyceps samples.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-11-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43559558","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 study was aimed to validate and optimize high performance liquid chromatographic (HPLC) method for the determination of coumarin-3-carboxylic acid (C3A) in the heart and liver issue of Sprague-Dawley (SD) rats after intragastric administration of extractive of leaves of Ficus virens var sublanceolata. And simple ADME and target prediction analyses were performed for C3A. Ethyl acetate was employed to precipitate protein with appropriate sensitivity and acceptable matrix effects. The satisfactory separation was developed on an ODS2 column (4.6 mm × 250 mm, 5 μm) by gradient elution with a methanol-acetic acid solution (pH = 3.0) as the mobile phase. The flow rate was 1.0 mL min−1, the column temperature was maintained at 30 ± 2 °C, the injection volume was 20 μL, and the detection wavelength was set as 309 nm. The method was fully validated in terms of selectivity, linearity, accuracy, precision, extraction recovery and stability. The results of the ADME analysis found that C3A has excellent characteristics of drug-likeness, consistent with good bio-absorption. And the predicted 12 target protein belongs to the amine oxidoreductase and carbonic anhydrase target class. This method is simple, rapid, sensitive, and accurate for the determination of coumarin-3-carboxylic acid in the heart and liver tissue of SD rats.
本研究旨在验证和优化Sprague-Dawley (SD)大鼠灌胃无花果叶提取物后心肝组织中香豆素-3-羧酸(C3A)的高效液相色谱测定方法。对C3A进行简单的ADME和靶标预测分析。用乙酸乙酯沉淀蛋白质，有适当的灵敏度和可接受的基质效应。在ODS2色谱柱(4.6 mm × 250 mm, 5 μm)上，以甲醇-乙酸溶液(pH = 3.0)为流动相进行梯度洗脱，得到了满意的分离效果。流速为1.0 mL min - 1，柱温为30±2℃，进样量为20 μL，检测波长为309 nm。该方法在选择性、线性度、准确度、精密度、提取回收率、稳定性等方面均得到了充分验证。ADME分析结果发现C3A具有优异的药物相似特性，具有良好的生物吸收性。预测的12靶蛋白属于胺氧化还原酶和碳酸酐酶靶类。该方法简便、快速、灵敏、准确，适用于SD大鼠心脏和肝脏组织中香豆素-3-羧酸的测定。
{"title":"Determination of coumarin-3-carboxylic acid in the liver and heart tissue of Sprague-Dawley rats after intragastric administration of extractive of leaves of F. virens var. sublanceolata by HPLC","authors":"Yujie Xiang, Bahetibieke Chuahe, Jing Zhang, Jiansha Li, Xinhui Jiang","doi":"10.1556/1326.2022.01075","DOIUrl":"https://doi.org/10.1556/1326.2022.01075","url":null,"abstract":"The study was aimed to validate and optimize high performance liquid chromatographic (HPLC) method for the determination of coumarin-3-carboxylic acid (C3A) in the heart and liver issue of Sprague-Dawley (SD) rats after intragastric administration of extractive of leaves of Ficus virens var sublanceolata. And simple ADME and target prediction analyses were performed for C3A. Ethyl acetate was employed to precipitate protein with appropriate sensitivity and acceptable matrix effects. The satisfactory separation was developed on an ODS2 column (4.6 mm × 250 mm, 5 μm) by gradient elution with a methanol-acetic acid solution (pH = 3.0) as the mobile phase. The flow rate was 1.0 mL min−1, the column temperature was maintained at 30 ± 2 °C, the injection volume was 20 μL, and the detection wavelength was set as 309 nm. The method was fully validated in terms of selectivity, linearity, accuracy, precision, extraction recovery and stability. The results of the ADME analysis found that C3A has excellent characteristics of drug-likeness, consistent with good bio-absorption. And the predicted 12 target protein belongs to the amine oxidoreductase and carbonic anhydrase target class. This method is simple, rapid, sensitive, and accurate for the determination of coumarin-3-carboxylic acid in the heart and liver tissue of SD rats.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42328953","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}
Tao Huang, Li Wang, Fang Wang, Xin Shen, Libin Wang
In the present study, an LC-MS/MS method allowing to quantify pretomanid and pyrazinamide simultaneously in rat plasma was developed. Chromatographic separation was achieved on an Agilent Eclipse plus C18 column (100 mm × 2.1 mm, 3.5 μm; Agilent, USA) and maintained at 30 °C. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 360.1 → m/z 175.1 for pretomanid, m/z 124.1 → m/z 81.0 for pyrazinamide, m/z 172.1 → m/z 128.1 for metronidazole (IS). The calibration curves showed good linear relationships over the concentration range of 50–7,500 ng mL−1 for pretomanid and 500–75,000 ng mL−1 for pyrazinamide. The precision and accuracy were below 15% and within ±15% of the nominal concentrations, respectively. The selectivity, recovery and matrix effect of this method were all within acceptable limits of bioanalytics. The method was applied to the analysis of plasma samples from pharmacokinetic studies in rats. The results show that the main pharmacokinetic parameters of pyrazinamide, namely, Tmax, t1/2, and AUC(0–t), decreased in the combined group than in the alone group.
本研究建立了同时定量大鼠血浆中pretomanid和pyrazinamide的LC-MS/MS方法。色谱分离采用Agilent Eclipse + C18色谱柱(100 mm × 2.1 mm, 3.5 μm;安捷伦，美国)，并保持在30°C。多反应监测(MRM)采用正离子ESI模式监测pretomanid的m/z 360.1→m/z 175.1，吡嗪酰胺的m/z 124.1→m/z 81.0，甲硝唑(IS)的m/z 172.1→m/z 128.1的离子跃迁。在50 ~ 7500 ng mL−1的浓度范围内，吡嗪酰胺在500 ~ 75000 ng mL−1的浓度范围内，标定曲线呈良好的线性关系。精密度和准确度分别低于标称浓度的15%和±15%。该方法的选择性、回收率和基质效应均在生物分析学可接受的范围内。该方法应用于大鼠药代动力学研究血浆样品的分析。结果表明，联合用药组吡嗪酰胺的主要药动学参数Tmax、t1/2和AUC(0-t)均低于单独用药组。
{"title":"LC-MS/MS method assay for simultaneous determination of the pretomanid and pyrazinamide in rat plasma by LC-MS/MS: Assessment of pharmacokinetic drug-drug interaction study","authors":"Tao Huang, Li Wang, Fang Wang, Xin Shen, Libin Wang","doi":"10.1556/1326.2022.01087","DOIUrl":"https://doi.org/10.1556/1326.2022.01087","url":null,"abstract":"In the present study, an LC-MS/MS method allowing to quantify pretomanid and pyrazinamide simultaneously in rat plasma was developed. Chromatographic separation was achieved on an Agilent Eclipse plus C18 column (100 mm × 2.1 mm, 3.5 μm; Agilent, USA) and maintained at 30 °C. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 360.1 → m/z 175.1 for pretomanid, m/z 124.1 → m/z 81.0 for pyrazinamide, m/z 172.1 → m/z 128.1 for metronidazole (IS). The calibration curves showed good linear relationships over the concentration range of 50–7,500 ng mL−1 for pretomanid and 500–75,000 ng mL−1 for pyrazinamide. The precision and accuracy were below 15% and within ±15% of the nominal concentrations, respectively. The selectivity, recovery and matrix effect of this method were all within acceptable limits of bioanalytics. The method was applied to the analysis of plasma samples from pharmacokinetic studies in rats. The results show that the main pharmacokinetic parameters of pyrazinamide, namely, Tmax, t1/2, and AUC(0–t), decreased in the combined group than in the alone group.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43246458","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}
Muscle relaxants and pain killers with their different types are widely used as combination approach for treatment of pain associated with several muscle spasm conditions. A sensitive and simple HPLC-UV detection method was developed in this work for simultaneous assay of Dantrolene (DNT) and co-administrated: Ibuprofen (IBU) and Diclofenac (DIC). After simple protein precipitation, separation was achieved using C18 column (150 × 4.6 mm) with a mobile phase of acidified water with orthophosphoric acid (pH = 3.5) and acetonitrile using gradient elution with a flow rate of 1 mL/min. The DAD was adjusted at 380, 219, 280 and 240 nm to measure DNT, IBU, DIC, and dexamethasone (internal standard), respectively. Linearity was demonstrated over the range from 0.1 to 3 μg/mL, 1 to 40 μg/mL, and 0.1 to 2 μg/mL for DNT, IBU, and DIC, respectively. The validated method was applied successfully to compare the effect of co-administration of IBU or DIC on the pharmacokinetic profile of DNT.
{"title":"Simultaneous determination of dantrolene with ibuprofen and diclofenac in plasma by HPLC-DAD: Application to comparative pharmacokinetic study","authors":"M. A. Abdel Moneim","doi":"10.1556/1326.2022.01089","DOIUrl":"https://doi.org/10.1556/1326.2022.01089","url":null,"abstract":"Muscle relaxants and pain killers with their different types are widely used as combination approach for treatment of pain associated with several muscle spasm conditions. A sensitive and simple HPLC-UV detection method was developed in this work for simultaneous assay of Dantrolene (DNT) and co-administrated: Ibuprofen (IBU) and Diclofenac (DIC). After simple protein precipitation, separation was achieved using C18 column (150 × 4.6 mm) with a mobile phase of acidified water with orthophosphoric acid (pH = 3.5) and acetonitrile using gradient elution with a flow rate of 1 mL/min. The DAD was adjusted at 380, 219, 280 and 240 nm to measure DNT, IBU, DIC, and dexamethasone (internal standard), respectively. Linearity was demonstrated over the range from 0.1 to 3 μg/mL, 1 to 40 μg/mL, and 0.1 to 2 μg/mL for DNT, IBU, and DIC, respectively. The validated method was applied successfully to compare the effect of co-administration of IBU or DIC on the pharmacokinetic profile of DNT.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2022-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46690979","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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