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":" ","pages":""},"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":" ","pages":""},"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}
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":" ","pages":""},"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}
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":" ","pages":""},"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}
Joanna Wróbel-Szkolak, A. Cwener, R. Pietraś, Ł. Komsta
70 species of grasses family (Poaceae), coming from genera: Agrostis, Alopecurus, Anthoxanthum, Apera, Arrhenatherum, Avena, Brachypodium, Briza, Bromus, Calamagrostis, Corynephorus, Cynosurus, Dactylis, Danthonia, Deschampsia, Digitaria, Echinochloa, Elymus, Eragrostis, Festuca, Glyceria, Helictotrichon, Hierochloe, Holcus, Hordeum, Koeleria, Leymus, Lolium, Milium, Molinia, Nardus, Panicum, Phalaris, Phleum, Phragmites, Poa, Saccharum and Setaria, collected mostly from natural stands in Poland during 2020 season, were subjected to GC-MS fingerprinting of headspace volatile fraction above dried material. Obtained mass spectrometry data were analyzed by means of principal component analysis (PCA) and hierarchical cluster analysis (HCA). Five species: Glyceria maxima (Hartm.) Holmb., Lolium multiflorum Lam., Hordeum jubatum L., Bromus tectorum L. and Bromus secalinus L. were identified as outliers, which is consistent with our earlier analysis by thin layer chromatography. These species deserve further look and their outliance is orthogonal to coumarin content, which was independently observed for odorant species of grasses.
{"title":"Simultaneous component analysis as an interesting preliminary data analysis method in GC-MS – An example of headspace screening of Polish grasses","authors":"Joanna Wróbel-Szkolak, A. Cwener, R. Pietraś, Ł. Komsta","doi":"10.1556/1326.2022.01099","DOIUrl":"https://doi.org/10.1556/1326.2022.01099","url":null,"abstract":"70 species of grasses family (Poaceae), coming from genera: Agrostis, Alopecurus, Anthoxanthum, Apera, Arrhenatherum, Avena, Brachypodium, Briza, Bromus, Calamagrostis, Corynephorus, Cynosurus, Dactylis, Danthonia, Deschampsia, Digitaria, Echinochloa, Elymus, Eragrostis, Festuca, Glyceria, Helictotrichon, Hierochloe, Holcus, Hordeum, Koeleria, Leymus, Lolium, Milium, Molinia, Nardus, Panicum, Phalaris, Phleum, Phragmites, Poa, Saccharum and Setaria, collected mostly from natural stands in Poland during 2020 season, were subjected to GC-MS fingerprinting of headspace volatile fraction above dried material. Obtained mass spectrometry data were analyzed by means of principal component analysis (PCA) and hierarchical cluster analysis (HCA). Five species: Glyceria maxima (Hartm.) Holmb., Lolium multiflorum Lam., Hordeum jubatum L., Bromus tectorum L. and Bromus secalinus L. were identified as outliers, which is consistent with our earlier analysis by thin layer chromatography. These species deserve further look and their outliance is orthogonal to coumarin content, which was independently observed for odorant species of grasses.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46200322","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}
An easy, quick, and sensitive approach adopting ultra-performance liquid chromatography (UPLC) equipped with diode array detector was used to analyze and systematically evaluate the quality of Pudilan tablets manufactured by 12 distinct pharmaceutical companies. In this research, 15 peaks were chosen as the common peaks to assess the similarities for different batches (S1–S43) of Pudilan tablet samples. In comparison with the control fingerprint, similarity values for 43 batches of samples exceeded 0.922. In addition, by analyzing the reference substances of epigoitrin, caffeic acid, chlorogenic acid, acetylcorynoline, baicalin and baicanshialein, the chromatogram of the 6 reference substances was established. The recoveries for the reference substances which demonstrated good regression in the linear range (r 2 > 0.999) were in the range of 98.3–101.1%. The results demonstrated that the established method was highly accurate, efficient and reliable. This study provides a valid, dependable and pragmatic method to evaluate the quality of Pudilan tablet.
{"title":"Quantitative evaluation and chromatographic fingerprinting for the quality assessment of Pudilan tablet","authors":"Mengya Lu, Q. Tang, Chenyu Zhou, Zhizheng Fang, Zheng Fan, Xiangyu Li, R. Han, X. Tong","doi":"10.1556/1326.2022.01084","DOIUrl":"https://doi.org/10.1556/1326.2022.01084","url":null,"abstract":"\u0000 An easy, quick, and sensitive approach adopting ultra-performance liquid chromatography (UPLC) equipped with diode array detector was used to analyze and systematically evaluate the quality of Pudilan tablets manufactured by 12 distinct pharmaceutical companies. In this research, 15 peaks were chosen as the common peaks to assess the similarities for different batches (S1–S43) of Pudilan tablet samples. In comparison with the control fingerprint, similarity values for 43 batches of samples exceeded 0.922. In addition, by analyzing the reference substances of epigoitrin, caffeic acid, chlorogenic acid, acetylcorynoline, baicalin and baicanshialein, the chromatogram of the 6 reference substances was established. The recoveries for the reference substances which demonstrated good regression in the linear range (r\u0000 2 > 0.999) were in the range of 98.3–101.1%. The results demonstrated that the established method was highly accurate, efficient and reliable. This study provides a valid, dependable and pragmatic method to evaluate the quality of Pudilan tablet.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45765767","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}
Qi An, Hong Sun, Linzhi Wu, Liangliang Liu, Sue Chen
Codonopsis Radix (CR) is recorded as the roots of Codonopsis pilosula, C. pilosula var. modesta and Codonopsis tangshen. It is difficult to evaluate the quality of CR because of the existence of many original plants. In this paper, a strategy integrating chromatographic analysis and chemometrics for the quality control of CR is proposed. Systematic analysis of the chemical composition of CR was achieved through high performance liquid chromatography (HPLC) fingerprinting. Based on the HPLC fingerprinting data, chemometrics, including unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discrimination analysis (OPLS-DA), were applied to classify all CR samples. Components with variable importance in projection values higher than 1 in the OPLS-DA model were selected as potential chemical markers for distinguishing the origins of CR. Finally, an HPLC method was validated for determining the five characteristic ingredients in the CR samples. HPLC characteristic fingerprints showed 17 common peaks for C. pilosula, 13 for C. pilosula var. modesta, and 9 for C. tangshen, and all of them showed good similarity (>0.9). Additionally, there were 9 common peaks for all CR samples with relatively poor similarity, ranging from 0.607 to 0.970. PCA could differentiate CR from the three origins, except for a partial overlap between C. pilosula and C. pilosula var. Modesta, and the OPLS-DA model achieved excellent classification results. Eight components (peaks 12, 8, lobetyolin, 10, codonopsin І, syringin, 3, and 11) were selected as potential chemical markers. There was a large discrepancy in the contents of the five characteristic ingredients in all samples, with the relative standard deviation ranging from 36.0% (lobetyolin) to 85.9% (atractylenolide Ⅲ). The average contents of the five characteristic ingredients were similar between C. pilosula and C. pilosula var. modesta samples and notably higher than those of C. tangshen samples. Consequently, a rapid, precise, and feasible strategy was established for the discrimination and quality control of CR with different origins.
党参根(Codonopsis Radix, CR)是党参、党参、党参的根。由于原植物的存在，给CR的质量评价带来了困难。本文提出了一种色谱分析与化学计量学相结合的CR质量控制策略。采用高效液相色谱(HPLC)指纹图谱对其化学成分进行了系统分析。基于HPLC指纹图谱数据，采用无监督主成分分析(PCA)和监督正交偏最小二乘判别分析(OPLS-DA)等化学计量学方法对所有CR样品进行分类。选择在OPLS-DA模型中投影值大于1的可变重要成分作为鉴别CR来源的潜在化学标记。最后，验证了HPLC法确定CR样品中5种特征成分的有效性。HPLC特征指纹图谱显示，党参有17个共同峰，酢浆草有13个共同峰，汤参有9个共同峰，具有较好的相似性(>0.9)。此外，所有CR样本有9个共同峰，相似度较差，范围为0.607 ~ 0.970。主成分分析法能够区分出三种来源的CR，除了C. pilosula和C. pilosula var. Modesta有部分重叠外，OPLS-DA模型取得了很好的分类效果。选取峰12、峰8、峰10、峰10、峰12、峰8、峰10、峰10、峰3、峰11作为潜在化学标记物。各样品中5种特征成分的含量差异较大，相对标准偏差在36.0%(枇杷膏)~ 85.9%(苍术内酯Ⅲ)之间，5种特征成分的平均含量在木犀草和木犀草样品中基本一致，显著高于汤参样品。为不同来源CR的鉴别和质量控制提供了一种快速、准确、可行的策略。
{"title":"Quality evaluation of Codonopsis Radix through high performance liquid chromatography fingerprint combined with chemometrics and simultaneous determination of five characteristic ingredients","authors":"Qi An, Hong Sun, Linzhi Wu, Liangliang Liu, Sue Chen","doi":"10.1556/1326.2022.01059","DOIUrl":"https://doi.org/10.1556/1326.2022.01059","url":null,"abstract":"\u0000 \u0000 Codonopsis Radix (CR) is recorded as the roots of Codonopsis pilosula, C. pilosula var. modesta and Codonopsis tangshen. It is difficult to evaluate the quality of CR because of the existence of many original plants. In this paper, a strategy integrating chromatographic analysis and chemometrics for the quality control of CR is proposed. Systematic analysis of the chemical composition of CR was achieved through high performance liquid chromatography (HPLC) fingerprinting. Based on the HPLC fingerprinting data, chemometrics, including unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discrimination analysis (OPLS-DA), were applied to classify all CR samples. Components with variable importance in projection values higher than 1 in the OPLS-DA model were selected as potential chemical markers for distinguishing the origins of CR. Finally, an HPLC method was validated for determining the five characteristic ingredients in the CR samples. HPLC characteristic fingerprints showed 17 common peaks for C. pilosula, 13 for C. pilosula var. modesta, and 9 for C. tangshen, and all of them showed good similarity (>0.9). Additionally, there were 9 common peaks for all CR samples with relatively poor similarity, ranging from 0.607 to 0.970. PCA could differentiate CR from the three origins, except for a partial overlap between C. pilosula and C. pilosula var. Modesta, and the OPLS-DA model achieved excellent classification results. Eight components (peaks 12, 8, lobetyolin, 10, codonopsin І, syringin, 3, and 11) were selected as potential chemical markers. There was a large discrepancy in the contents of the five characteristic ingredients in all samples, with the relative standard deviation ranging from 36.0% (lobetyolin) to 85.9% (atractylenolide Ⅲ). The average contents of the five characteristic ingredients were similar between C. pilosula and C. pilosula var. modesta samples and notably higher than those of C. tangshen samples. Consequently, a rapid, precise, and feasible strategy was established for the discrimination and quality control of CR with different origins.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-10-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48855341","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}
Bai-Hu-Jia-Ren-Shen-Tang Decoction (BHJRSTD) is one of the oldest classic Chinese medicine prescriptions which used in the field of treatment of diabetes. However, to the best of our knowledge, the ingredients of this prescription have not been identified, and there are very few studies on the anti-diabetic mechanism of this prescription. Therefore, BHJRSTD was detected and identified by ultra-high-performance liquid chromatography coupled with Quadrupole-Exactive Focus Orbitrap MS (UHPLC–Q/Orbitrap/MS/MS). We identified 74 compounds, including flavonoids, alkaloids, chalcones, xanthones, phenols, phenylpropanoids, terpenes, triterpenes, amino acid derivatives, etc. Then, Sprague Dawley rats were fed with a high-fat and high-sugar diet for two months and injected with streptozotocin (STZ) to induce type 2 diabetes (T2DM). The diabetic rats were randomized to given metformin (200 mg kg−1·d−1, n = 15), BHJRSTD extracts (40 g kg−1·d−1) and BHJRSTD extracts (10 g kg−1·d−1) by gavage for 8 weeks. The results confirmed that BHJRSTD significantly decreased the level of MDA and increased levels of catalase (CAT), superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px), it shows that the prescription has significant antioxidant activity in the treatment of T2DM.
白虎夹肾汤是治疗糖尿病最古老的经典中药方剂之一。然而，据我们所知，该处方的成分尚未确定，关于该处方抗糖尿病机制的研究也很少。因此，BHJRSTD是通过超高效液相色谱联用四极杆Exactive Focus Orbitrap MS（UHPLC–Q/Orbitrap/MS/MS）进行检测和鉴定的。我们鉴定了74种化合物，包括黄酮类、生物碱、查尔酮、黄酮、酚类、苯丙烷类、萜类、三萜类、氨基酸衍生物等。然后，Sprague-Dawley大鼠喂食高脂高糖饮食两个月，并注射链脲佐菌素（STZ）诱导2型糖尿病（T2DM）。糖尿病大鼠随机接受二甲双胍（200 mg kg−1·d−1，n=15），BHJRSTD提取物（40 g kg−1·d−1）和BHJRSTD提取物（10 g kg−1·d−1） 灌胃8周。结果证实，BHJRSTD能显著降低MDA水平，提高过氧化氢酶（CAT）、超氧化物歧化酶（SOD）和谷胱甘肽过氧化物酶（GSH-Px）水平，表明该方对治疗T2DM具有显著的抗氧化活性。
{"title":"UHPLC–Q/Orbitrap/MS/MS fingerprinting of Bai-Hu-Jia-Ren-Shen-Tang Decoction and evaluation of its antioxidant activity in streptozotocin-induced diabetic rats","authors":"Libin Wang, Xin Shen, Fang Wang, Xiaohui Xu","doi":"10.1556/1326.2022.01068","DOIUrl":"https://doi.org/10.1556/1326.2022.01068","url":null,"abstract":"\u0000 Bai-Hu-Jia-Ren-Shen-Tang Decoction (BHJRSTD) is one of the oldest classic Chinese medicine prescriptions which used in the field of treatment of diabetes. However, to the best of our knowledge, the ingredients of this prescription have not been identified, and there are very few studies on the anti-diabetic mechanism of this prescription. Therefore, BHJRSTD was detected and identified by ultra-high-performance liquid chromatography coupled with Quadrupole-Exactive Focus Orbitrap MS (UHPLC–Q/Orbitrap/MS/MS). We identified 74 compounds, including flavonoids, alkaloids, chalcones, xanthones, phenols, phenylpropanoids, terpenes, triterpenes, amino acid derivatives, etc. Then, Sprague Dawley rats were fed with a high-fat and high-sugar diet for two months and injected with streptozotocin (STZ) to induce type 2 diabetes (T2DM). The diabetic rats were randomized to given metformin (200 mg kg−1·d−1, n = 15), BHJRSTD extracts (40 g kg−1·d−1) and BHJRSTD extracts (10 g kg−1·d−1) by gavage for 8 weeks. The results confirmed that BHJRSTD significantly decreased the level of MDA and increased levels of catalase (CAT), superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px), it shows that the prescription has significant antioxidant activity in the treatment of T2DM.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47126953","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}
E. Zhang, Junying Chen, Xia Li, Lvqi Luo, Yizhe Ma, Qingwei Zhang, Xianqin Wang
Flavonoids are the most abundant components in Salvia plebeia, with significant pharmacological antioxidant and hepatoprotective properties. Hispidulin and homoplantaginin are the main flavonoid components in S. Plebeia. In this study, we established an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to determine hispidulin and homoplantaginin in rat plasma samples, which were precipitated using acetonitrile-methanol (9:1, v/v). We used a UPLC HSS T3 (100 mm × 2.1 mm, 1.7 μm diameter) chromatographic column, an acetonitrile-water (containing 0.1% formic acid) mobile phase, and a gradient elution flow rate of 0.4 mL min−1 in an elution time of 4 min. We used electrospray ionization (ESI) detection in positive ion mode, and multiple reaction monitoring mode (MRM) for quantitative analysis: m/z 301 → 286 for hispidulin, m/z 463 → 301 for homoplantaginin, and m/z 465 → 303 for internal standard (IS). In pharmacokinetic studies, 24 rats were orally administered hispidulin and homoplantaginin (5 mg kg−1) and received sublingual intravenous injections (1 mg kg−1) at two different doses, four groups with six rats/group. Differences in hispidulin and homoplantaginin pharmacokinetics in rat plasma were evaluated. The calibration curve showed good linearity in the 0.5–1,000 ng mL−1 range, with r > 0.99. Precision, accuracy, recovery, matrix effects, and stability results all met standard biological sample detection requirements. Our pharmacokinetic studies showed hispidulin bioavailability was much higher than homoplantaginin at 17.8% and 0.1%, respectively.
{"title":"An improved ultra-high performance liquid chromatography-tandem mass spectrometry method determining hispidulin and homoplantaginin in rat plasma and associated pharmacokinetic studies","authors":"E. Zhang, Junying Chen, Xia Li, Lvqi Luo, Yizhe Ma, Qingwei Zhang, Xianqin Wang","doi":"10.1556/1326.2022.01082","DOIUrl":"https://doi.org/10.1556/1326.2022.01082","url":null,"abstract":"\u0000 Flavonoids are the most abundant components in Salvia plebeia, with significant pharmacological antioxidant and hepatoprotective properties. Hispidulin and homoplantaginin are the main flavonoid components in S. Plebeia. In this study, we established an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to determine hispidulin and homoplantaginin in rat plasma samples, which were precipitated using acetonitrile-methanol (9:1, v/v). We used a UPLC HSS T3 (100 mm × 2.1 mm, 1.7 μm diameter) chromatographic column, an acetonitrile-water (containing 0.1% formic acid) mobile phase, and a gradient elution flow rate of 0.4 mL min−1 in an elution time of 4 min. We used electrospray ionization (ESI) detection in positive ion mode, and multiple reaction monitoring mode (MRM) for quantitative analysis: m/z 301 → 286 for hispidulin, m/z 463 → 301 for homoplantaginin, and m/z 465 → 303 for internal standard (IS). In pharmacokinetic studies, 24 rats were orally administered hispidulin and homoplantaginin (5 mg kg−1) and received sublingual intravenous injections (1 mg kg−1) at two different doses, four groups with six rats/group. Differences in hispidulin and homoplantaginin pharmacokinetics in rat plasma were evaluated. The calibration curve showed good linearity in the 0.5–1,000 ng mL−1 range, with r > 0.99. Precision, accuracy, recovery, matrix effects, and stability results all met standard biological sample detection requirements. Our pharmacokinetic studies showed hispidulin bioavailability was much higher than homoplantaginin at 17.8% and 0.1%, respectively.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44455191","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}
Waqar Siddique, R. M. Sarfraz, Muhammad Zaman, Riffat Khan, M. Gul, F. Asghar, Tangina Malik, A. Saif, Qurat-Ul-Ain Shamim, A. Salawi, Meshal Alshamrani, Yosif Almoshari, F. Y. Sabei
One of the most effective, rapid, and simple methods reversed-phase high-performance liquid chromatography (RP-HPLC) was used for simultaneous development and validation of Eletriptan hydrobromide (ELE HBR) and Itopride hydrochloride (ITP HCL) in combination. The method was validated based on the regulations of United States Pharmacopeia (USP) and International Conference on Harmonization (ICH) guidelines. Separation of both drugs was achieved within approximately 5 min by using a mobile phase made up of a 70:30 ratio of phosphate buffer and acetonitrile having a flow rate of 1 mL min−1. Furthermore, a comprehensive study was conducted on precision, accuracy, linearity, inter-day, intra-day studies, an assay of formulated films, and stability studies of combined prepared film. Co-efficient of correlation ranged between 0.9993, and 0.9965 for ELE HBR and ITP HCL respectively. The accuracy of the developed method was accurate as drug recoveries in both cases of ITP HCL, and ELE HBR falls between (99.87, 99.96, and 99.84%) to (99.81, 99.12, and 98.44%) respectively having a concentration range of solutions between 10, 30 and 50 μg mL−1 dilution. Films developed by using both drugs in combination were then validated for assay studies, and it was found that substantial results of 99.05%, and 99.87% were found in the case of ITP HCL and ELE HBR respectively. The stability of the solution and mobile phase showed the method's accuracy as the results were 97% for ITP HCL and 99% for ELE HBR. The proposed method developed for simultaneous determination of ITP HCL and ELE HBR was developed and validation and no interaction of any excipient were found.
{"title":"Method development and validation for simultaneous determination of Eletriptan hydrobromide and Itopride hydrochloride from fast dissolving buccal films by using RP-HPLC","authors":"Waqar Siddique, R. M. Sarfraz, Muhammad Zaman, Riffat Khan, M. Gul, F. Asghar, Tangina Malik, A. Saif, Qurat-Ul-Ain Shamim, A. Salawi, Meshal Alshamrani, Yosif Almoshari, F. Y. Sabei","doi":"10.1556/1326.2022.01072","DOIUrl":"https://doi.org/10.1556/1326.2022.01072","url":null,"abstract":"\u0000 One of the most effective, rapid, and simple methods reversed-phase high-performance liquid chromatography (RP-HPLC) was used for simultaneous development and validation of Eletriptan hydrobromide (ELE HBR) and Itopride hydrochloride (ITP HCL) in combination. The method was validated based on the regulations of United States Pharmacopeia (USP) and International Conference on Harmonization (ICH) guidelines. Separation of both drugs was achieved within approximately 5 min by using a mobile phase made up of a 70:30 ratio of phosphate buffer and acetonitrile having a flow rate of 1 mL min−1. Furthermore, a comprehensive study was conducted on precision, accuracy, linearity, inter-day, intra-day studies, an assay of formulated films, and stability studies of combined prepared film. Co-efficient of correlation ranged between 0.9993, and 0.9965 for ELE HBR and ITP HCL respectively. The accuracy of the developed method was accurate as drug recoveries in both cases of ITP HCL, and ELE HBR falls between (99.87, 99.96, and 99.84%) to (99.81, 99.12, and 98.44%) respectively having a concentration range of solutions between 10, 30 and 50 μg mL−1 dilution. Films developed by using both drugs in combination were then validated for assay studies, and it was found that substantial results of 99.05%, and 99.87% were found in the case of ITP HCL and ELE HBR respectively. The stability of the solution and mobile phase showed the method's accuracy as the results were 97% for ITP HCL and 99% for ELE HBR. The proposed method developed for simultaneous determination of ITP HCL and ELE HBR was developed and validation and no interaction of any excipient were found.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47041164","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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