L. Pérez-López, Norma Cavazos-Rocha, Cecilia Delgado-Montemayor, N. Waksman-Minsky, M. Hernández-Salazar, Omar J. Portillo-Castillo
The analysis of phenolic acids (PAs) is of great importance, because they are frequently present in natural products and their derivatives, and these compounds also have multiple beneficial effects to human health. This work is focusing on the separation of seven PAs (caffeic acid, coumaric acid, gallic acid, ferulic acid, protocatechuic acid, sinapic acid, and syringic acid), in a reversed-phase liquid chromatographic (RP-HPLC) isocratic method using a hydrophilic deep eutectic solvent (DES) as a mobile phase additive. The analysis was carried out with a diode array detector. The used DES was composed by choline chloride and glycerol, and it was characterized by infrared spectroscopy. The combination of choline chloride:glycerol (1:4) added at 0.25% to mobile phase composed of 0.15% formic acid aqueous solution and methanol (80:20), showed the best separation for target analytes. The new proposed method was validated, and results indicated that the proposed method is linear, selective for almost all analytes, provided high sensitivity with limit of detection ranges from 0.009 to 0.023 mg mL−1, and has satisfactory precision and accuracy, with values of relative standard deviation of 0.24–2.65% and recoveries of 97.97–109%, respectively. Additionally, this method was successfully applied to simultaneous determination of phenolic acids in three kinds of samples of powder to prepare lemon flavour drink enriched with black tea extract.
{"title":"A simple HPLC-DAD method for analysis of phenolic acids: Addition effect of a hydrophilic deep eutectic solvent to the mobile phase","authors":"L. Pérez-López, Norma Cavazos-Rocha, Cecilia Delgado-Montemayor, N. Waksman-Minsky, M. Hernández-Salazar, Omar J. Portillo-Castillo","doi":"10.1556/1326.2022.01055","DOIUrl":"https://doi.org/10.1556/1326.2022.01055","url":null,"abstract":"\u0000 The analysis of phenolic acids (PAs) is of great importance, because they are frequently present in natural products and their derivatives, and these compounds also have multiple beneficial effects to human health. This work is focusing on the separation of seven PAs (caffeic acid, coumaric acid, gallic acid, ferulic acid, protocatechuic acid, sinapic acid, and syringic acid), in a reversed-phase liquid chromatographic (RP-HPLC) isocratic method using a hydrophilic deep eutectic solvent (DES) as a mobile phase additive. The analysis was carried out with a diode array detector. The used DES was composed by choline chloride and glycerol, and it was characterized by infrared spectroscopy. The combination of choline chloride:glycerol (1:4) added at 0.25% to mobile phase composed of 0.15% formic acid aqueous solution and methanol (80:20), showed the best separation for target analytes. The new proposed method was validated, and results indicated that the proposed method is linear, selective for almost all analytes, provided high sensitivity with limit of detection ranges from 0.009 to 0.023 mg mL−1, and has satisfactory precision and accuracy, with values of relative standard deviation of 0.24–2.65% and recoveries of 97.97–109%, respectively. Additionally, this method was successfully applied to simultaneous determination of phenolic acids in three kinds of samples of powder to prepare lemon flavour drink enriched with black tea extract.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-06-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46910689","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}
H. Gebretsadik, G. Kahsay, Tadele Eticha, Tesfamichael Gebretsadikan
As per the World Health Organization, 10% of medicines in low- and middle-income nations are of poor quality and pose a huge public health risk. The development and implementation of cost-effective, efficient and quick analytical methods to control the quality of these medicines is one of the immediate strategies to avoid such a situation. Hence, the main goal of this study was to develop and validate a simple, specific and precise new RP–HPLC method for simultaneous analysis of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations. The chromatographic analysis was achieved using Shodex C18 (250 × 4.6 mm, 5 μm) column with UV detection at 225 nm. The mobile phase was a gradient mixture of 30 mM phosphate buffer, pH 4.0 (mobile phase A) and acetonitrile (mobile phase B). Efficient separation of the three drugs was obtained using the final optimized chromatographic conditions. The developed method was validated for its specificity, linearity, precision, accuracy and robustness as per the ICH guidelines. The validation results showed that the method was specific, linear, precise, accurate and robust for the simultaneous determination of the three drugs. The developed method was applied to determine the content of the three drugs in pharmaceutical formulations. The assay results of the preparations showed that their drug content was within the pharmacopeial limit stipulated for each drug product. It can be concluded that the proposed method is suitable for simultaneous determination of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations in industries and regulatory laboratories.
根据世界卫生组织的数据，低收入和中等收入国家10%的药品质量差，对公共卫生构成巨大风险。开发和实施具有成本效益、高效和快速的分析方法来控制这些药物的质量是避免这种情况的直接战略之一。因此，本研究的主要目的是建立一种简便、特异、精确的反相高效液相色谱同时分析阿莫西林、氨苄西林和氯西林的新方法。色谱柱为Shodex C18 (250 × 4.6 mm, 5 μm)，紫外检测波长225 nm。流动相为pH为4.0的30 mM磷酸盐缓冲液(流动相a)和乙腈(流动相B)的梯度混合物。采用优化后的色谱条件对三种药物进行了高效分离。根据ICH指南验证了该方法的特异性、线性度、精密度、准确性和稳健性。验证结果表明，该方法专属性强、线性好、精密度高、准确度高、鲁棒性好，可用于三种药物的同时测定。将所建立的方法应用于制剂中这三种药物的含量测定。制剂的测定结果表明，其药物含量在药典规定的限量范围内。结果表明，该方法适用于工业和监管实验室制剂中阿莫西林、氨苄西林和氯西林的同时测定。
{"title":"A validated new RP-HPLC method for simultaneous determination of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations","authors":"H. Gebretsadik, G. Kahsay, Tadele Eticha, Tesfamichael Gebretsadikan","doi":"10.1556/1326.2022.01043","DOIUrl":"https://doi.org/10.1556/1326.2022.01043","url":null,"abstract":"\u0000 As per the World Health Organization, 10% of medicines in low- and middle-income nations are of poor quality and pose a huge public health risk. The development and implementation of cost-effective, efficient and quick analytical methods to control the quality of these medicines is one of the immediate strategies to avoid such a situation. Hence, the main goal of this study was to develop and validate a simple, specific and precise new RP–HPLC method for simultaneous analysis of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations. The chromatographic analysis was achieved using Shodex C18 (250 × 4.6 mm, 5 μm) column with UV detection at 225 nm. The mobile phase was a gradient mixture of 30 mM phosphate buffer, pH 4.0 (mobile phase A) and acetonitrile (mobile phase B). Efficient separation of the three drugs was obtained using the final optimized chromatographic conditions. The developed method was validated for its specificity, linearity, precision, accuracy and robustness as per the ICH guidelines. The validation results showed that the method was specific, linear, precise, accurate and robust for the simultaneous determination of the three drugs. The developed method was applied to determine the content of the three drugs in pharmaceutical formulations. The assay results of the preparations showed that their drug content was within the pharmacopeial limit stipulated for each drug product. It can be concluded that the proposed method is suitable for simultaneous determination of amoxicillin, ampicillin and cloxacillin in pharmaceutical formulations in industries and regulatory laboratories.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48612803","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}
Development and validation of a selective analytical method to accurately and precisely quantify nicotine and cotinine levels in rat's plasma after exposure to tobacco cigarettes and tobacco water-pipe. An easy HPLC-Photodiode-Array Detection (PDA) method was developed and validated for simultaneous determination of nicotine and cotinine levels in plasma of 15 rats (10 rats after tobacco products exposure and 5 control rats). Nicotine and cotinine were extracted in one step from plasma using acetonitrile and concentrated to lowest volume using nitrogen stream. The developed method offered a rapid analysis time of 14 min with single step of analytes extraction from rat's plasma with recovery percentage range between 93 and 95% and excellent linearity with correlation factor more than 0.994 with analytical range between 50 and 1000 ng mL−1 and LOD of 25 ng mL−1 and 23 ng mL−1 for nicotine and cotinine, respectively. The analysis of rat's plasma after 28 days of exposure to tobacco cigarettes and tobacco water-pipe revealed that the average concentrations of 376 ng mL−1 for cotinine and 223 ng mL−1 for nicotine were obtained after tobacco cigarettes exposure, and 220 ng mL−1 for cotinine and 192 ng mL−1 for nicotine after tobacco water-pipe exposure. Higher nicotine and cotinine levels were found in plasma after tobacco cigarettes exposure than water-pipe exposure which may have potential undesirable effects on passive smokers in both cases.
一种选择性分析方法的开发和验证，该方法可准确准确地定量大鼠接触烟草香烟和烟草水管后血浆中的尼古丁和可替宁水平。开发并验证了一种简单的HPLC光电二极管阵列检测（PDA）方法，用于同时测定15只大鼠（10只烟草制品暴露后的大鼠和5只对照大鼠）血浆中的尼古丁和可替宁水平。使用乙腈一步从血浆中提取尼古丁和可替宁，并使用氮气流浓缩至最低体积。所开发的方法提供了14的快速分析时间 min，从大鼠血浆中一步提取分析物，回收率在93%至95%之间，线性良好，相关系数大于0.994，分析范围在50至1000之间 ng mL−1，LOD为25 ng mL−1和23 尼古丁和可替宁分别为ng mL−1。对暴露于烟草香烟和烟草水管28天后大鼠血浆的分析显示，376 ng mL−1用于可替宁和223 尼古丁的浓度为ng mL−1，在接触烟草香烟后，浓度为220 ng mL−1用于可替宁和192 烟草水管暴露后尼古丁浓度为ng mL−1。烟草烟雾暴露后血浆中的尼古丁和可替宁水平高于水管暴露，这可能对被动吸烟者产生潜在的不良影响。
{"title":"Simple HPLC method for simultaneous quantification of nicotine and cotinine levels in rat plasma after exposure to two different tobacco products","authors":"Ala A. Alhusban, A. Hammad, Lujain F. Alzaghari","doi":"10.1556/1326.2022.01054","DOIUrl":"https://doi.org/10.1556/1326.2022.01054","url":null,"abstract":"\u0000 \u0000 \u0000 Development and validation of a selective analytical method to accurately and precisely quantify nicotine and cotinine levels in rat's plasma after exposure to tobacco cigarettes and tobacco water-pipe.\u0000 \u0000 \u0000 \u0000 An easy HPLC-Photodiode-Array Detection (PDA) method was developed and validated for simultaneous determination of nicotine and cotinine levels in plasma of 15 rats (10 rats after tobacco products exposure and 5 control rats). Nicotine and cotinine were extracted in one step from plasma using acetonitrile and concentrated to lowest volume using nitrogen stream.\u0000 \u0000 \u0000 \u0000 The developed method offered a rapid analysis time of 14 min with single step of analytes extraction from rat's plasma with recovery percentage range between 93 and 95% and excellent linearity with correlation factor more than 0.994 with analytical range between 50 and 1000 ng mL−1 and LOD of 25 ng mL−1 and 23 ng mL−1 for nicotine and cotinine, respectively. The analysis of rat's plasma after 28 days of exposure to tobacco cigarettes and tobacco water-pipe revealed that the average concentrations of 376 ng mL−1 for cotinine and 223 ng mL−1 for nicotine were obtained after tobacco cigarettes exposure, and 220 ng mL−1 for cotinine and 192 ng mL−1 for nicotine after tobacco water-pipe exposure.\u0000 \u0000 \u0000 \u0000 Higher nicotine and cotinine levels were found in plasma after tobacco cigarettes exposure than water-pipe exposure which may have potential undesirable effects on passive smokers in both cases.\u0000","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46690376","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 precise, sensitive, specific and accurate stability indicating densitometric method was developed and validated for alpha-lipoic acid (ALA) in bulk and capsule dosage form. The study employed pre-coated silica gel 60F254 TLC plates as stationary phase and toluene: chloroform: methanol: formic acid (5:3:1:0.05; v/v/v/v) as mobile phase. The developed method furnished compact spots of alpha-lipoic acid (Rf 0.28 ± 0.05) after derivatization, offered good linearity in range 80–400 ng/spot with correlation coefficient of 0.998. The values for detection and quantitation were found 18.022 and 54.612 ng/spot respectively. ALA was subjected to stress degradation studies and total 13 degradation products were resolved. Thus, the proposed method offered good results according to ICH guidelines, and can be used for identification, routine quantitative determination as well as for monitoring the stability of ALA in bulk and in capsules.
{"title":"Stress degradation studies and development of validated stability indicating densitometric method for estimation of alpha lipoic acid in bulk and capsule dosage form","authors":"S. Srivastava, S. Dhaneshwar, N. Kawathekar","doi":"10.1556/1326.2022.01034","DOIUrl":"https://doi.org/10.1556/1326.2022.01034","url":null,"abstract":"\u0000 A precise, sensitive, specific and accurate stability indicating densitometric method was developed and validated for alpha-lipoic acid (ALA) in bulk and capsule dosage form. The study employed pre-coated silica gel 60F254 TLC plates as stationary phase and toluene: chloroform: methanol: formic acid (5:3:1:0.05; v/v/v/v) as mobile phase. The developed method furnished compact spots of alpha-lipoic acid (Rf 0.28 ± 0.05) after derivatization, offered good linearity in range 80–400 ng/spot with correlation coefficient of 0.998. The values for detection and quantitation were found 18.022 and 54.612 ng/spot respectively. ALA was subjected to stress degradation studies and total 13 degradation products were resolved. Thus, the proposed method offered good results according to ICH guidelines, and can be used for identification, routine quantitative determination as well as for monitoring the stability of ALA in bulk and in capsules.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42252377","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}
Modafinil has a strong and long-lasting awakening effect. Short-term use can improve cognitive and work efficiency. Therefore, it has been known to be abused by students and parents as a “smart drug.” It is in the first category of psychotropic drugs and strictly controlled. To detect modafinil in rat plasma and study the differences in the pharmacokinetics of modafinil between oral and sublingual administration in rats, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed. Rats were injected with modafinil by oral gavage and sublingual vein, respectively, blood was collected within a certain period, and the plasma was obtained by centrifugation. Midazolam was used as the internal standard, and the concentration of modafinil in the plasma was determined by UPLC-MS/MS, where a drug-time curve was created to calculate the pharmacokinetic parameters. The standard curve for modafinil ranged from 1 to 2000 ng mL−1 with good linearity. The intra-day accuracy of modafinil was between 86% and 104%, and the intra-day accuracy was between 90% and 103%. Intra-day precision (RSD%) was less than 15%, inter-day precision (RSD%) was less than 15%. The matrix effect was between 93% and 102%, and the recovery was greater than 91%. The UPLC-MS/MS method established in this work has good selectivity and high sensitivity, and the UPLC-MS/MS method was successfully applied to the pharmacokinetics of modafinil by oral gavage and sublingual injection in rats. The bioavailability of modafinil was calculated to be 55.8%.
{"title":"Determination of modafinil in rat plasma by UPLC-MS/MS and a study of its pharmacokinetics and bioavailability","authors":"Yan He, Yizhe Ma, Lvqi Luo, Junying Chen, Congcong Wen, Meiling Zhang","doi":"10.1556/1326.2022.01041","DOIUrl":"https://doi.org/10.1556/1326.2022.01041","url":null,"abstract":"\u0000 Modafinil has a strong and long-lasting awakening effect. Short-term use can improve cognitive and work efficiency. Therefore, it has been known to be abused by students and parents as a “smart drug.” It is in the first category of psychotropic drugs and strictly controlled. To detect modafinil in rat plasma and study the differences in the pharmacokinetics of modafinil between oral and sublingual administration in rats, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed. Rats were injected with modafinil by oral gavage and sublingual vein, respectively, blood was collected within a certain period, and the plasma was obtained by centrifugation. Midazolam was used as the internal standard, and the concentration of modafinil in the plasma was determined by UPLC-MS/MS, where a drug-time curve was created to calculate the pharmacokinetic parameters. The standard curve for modafinil ranged from 1 to 2000 ng mL−1 with good linearity. The intra-day accuracy of modafinil was between 86% and 104%, and the intra-day accuracy was between 90% and 103%. Intra-day precision (RSD%) was less than 15%, inter-day precision (RSD%) was less than 15%. The matrix effect was between 93% and 102%, and the recovery was greater than 91%. The UPLC-MS/MS method established in this work has good selectivity and high sensitivity, and the UPLC-MS/MS method was successfully applied to the pharmacokinetics of modafinil by oral gavage and sublingual injection in rats. The bioavailability of modafinil was calculated to be 55.8%.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-05-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44192088","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 UPLC-MS/MS method was developed to determinate curdione in the mouse blood, and the pharmacokinetics of curdione in mice after intravenous (5 mg kg−1) and oral (20 mg kg−1) administration were studied. The HSS T3 column was used for separation, and column temperature was set at 40 °C. Multiple reaction monitoring (MRM) mode were used for determination of curdione. Blood samples were taken from the caudal vein of Institute of Cancer Research (ICR) mice after administration of curdione. It showed a good linear relationship in the range of 1–500 ng mL−1 (r > 0.998); the intra-day precision was <13%, the inter-day precision was <15%, and the accuracy was 90%–105%, the recovery was >77%, and the matrix effect was 97%–107%. The half-life was relatively short, and the bioavailability was 6.5%. The developed method was suitable for the pharmacokinetics of curdione in mice.
建立了UPLC-MS/MS法测定小鼠血液中的curdione，并研究了静脉(5 mg kg - 1)和口服(20 mg kg - 1)给药后curdione在小鼠体内的药代动力学。采用HSS T3柱进行分离，柱温为40℃。采用多反应监测(MRM)法测定莪术酮的含量。在给药后从癌症研究所(ICR)小鼠尾静脉采血。在1 ~ 500 ng mL−1范围内呈良好的线性关系(r为0 0.998);日内精密度为77%，基质效应为97% ~ 107%。半衰期较短，生物利用度为6.5%。该方法适用于莪术酮在小鼠体内的药动学研究。
{"title":"Pharmacokinetics and bioavailability of curdione in mice by UPLC-MS/MS","authors":"Qishun Liang, Tianyu Chen, Lvqi Luo, Yizhe Ma, Congcong Wen, Xueli Huang","doi":"10.1556/1326.2022.01020","DOIUrl":"https://doi.org/10.1556/1326.2022.01020","url":null,"abstract":"\u0000 A UPLC-MS/MS method was developed to determinate curdione in the mouse blood, and the pharmacokinetics of curdione in mice after intravenous (5 mg kg−1) and oral (20 mg kg−1) administration were studied. The HSS T3 column was used for separation, and column temperature was set at 40 °C. Multiple reaction monitoring (MRM) mode were used for determination of curdione. Blood samples were taken from the caudal vein of Institute of Cancer Research (ICR) mice after administration of curdione. It showed a good linear relationship in the range of 1–500 ng mL−1 (r > 0.998); the intra-day precision was <13%, the inter-day precision was <15%, and the accuracy was 90%–105%, the recovery was >77%, and the matrix effect was 97%–107%. The half-life was relatively short, and the bioavailability was 6.5%. The developed method was suitable for the pharmacokinetics of curdione in mice.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-05-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46433360","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 rapid and simple ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for simultaneous determination of six analytes from the Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. leaves (ESL) in beagle dog plasma for the first time, including 3-O-α-l-rhamnopyranosyl-(1→2)-α-l-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-d-glucopyranosyl-(1→2)-α-l-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-d-glucopyranosyl-(1→2)-α-l-arabinopyranosyl-30-norlean-12,20 (29) –dien-28-olic acid, ciwujianoside E, guaianin N, and eleutheroside K. The chromatographic separation was performed using an ACQUITY UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) using a gradient elution way with a mobile phase of acetonitrile-water containing 0.1% formic acid. Analytes were detected on a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source with multiple reaction monitoring (MRM) mode. Calibration curves were all linear (r ≥ 0.9933) over the concentration range. The mean extraction recoveries and matrix effect of analytes and I.S. were ranged from 80.26% to 98.32% and from 91.27% to 111.67%, respectively. The intra-day and inter-day precision were ranged from 2.20% to 14.81%, and the accuracy range was 1.60–14.60%. The analytical method was successfully applied for the pharmacokinetic characteristics of the six analytes in beagle plasma after oral administration of ESL extracts. The T 1/2 of six analytes was more than 3.09 ± 0.78 h.
{"title":"Simultaneous determination of six triterpenoid saponins in beagle dog plasma by UPLC-MS/MS and its application to a pharmacokinetic study after oral administration of the extract of the Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. leaves","authors":"Zhibin Wang, Yaodan Chang, Feng Cao, Chunjuan Yang, Zhenyue Wang, Haixue Kuang","doi":"10.1556/1326.2022.01011","DOIUrl":"https://doi.org/10.1556/1326.2022.01011","url":null,"abstract":"\u0000 A rapid and simple ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for simultaneous determination of six analytes from the Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. leaves (ESL) in beagle dog plasma for the first time, including 3-O-α-l-rhamnopyranosyl-(1→2)-α-l-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-d-glucopyranosyl-(1→2)-α-l-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-d-glucopyranosyl-(1→2)-α-l-arabinopyranosyl-30-norlean-12,20 (29) –dien-28-olic acid, ciwujianoside E, guaianin N, and eleutheroside K. The chromatographic separation was performed using an ACQUITY UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) using a gradient elution way with a mobile phase of acetonitrile-water containing 0.1% formic acid. Analytes were detected on a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source with multiple reaction monitoring (MRM) mode. Calibration curves were all linear (r ≥ 0.9933) over the concentration range. The mean extraction recoveries and matrix effect of analytes and I.S. were ranged from 80.26% to 98.32% and from 91.27% to 111.67%, respectively. The intra-day and inter-day precision were ranged from 2.20% to 14.81%, and the accuracy range was 1.60–14.60%. The analytical method was successfully applied for the pharmacokinetic characteristics of the six analytes in beagle plasma after oral administration of ESL extracts. The T\u0000 1/2 of six analytes was more than 3.09 ± 0.78 h.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-05-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67652867","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}
Hengyi Yu, Xiuhua Ren, Lu Liu, Dong Xiang, Xiping Li, Juan Li, Dong Liu, X. Gong
Epilepsy is one of the most prevalent neurological conditions and antiepileptic drugs are the mainstay of epilepsy treatment. High variation in pharmacokinetic profiles of several antiepileptic drugs highlights the importance of therapeutic drug monitoring to estimate pharmacokinetic properties and consequently individualize drug posology. In this work, a simple, rapid and robust liquid chromatography-tandem mass spectrometry method was developed for simultaneous quantification of carbamazepine and its metabolite carbamazepine-10,11-epoxide, gabapentin, levetiracetam, lamotrigine, oxcarbazepine and its metabolite mono-hydroxy-derivative metabolite, phenytoin, topiramate, and valproic acid in human plasma for therapeutic drug monitoring. d 6 -Levetiracetam, d 4 -gabapentin and d 6 -valproic acid were used as internal standards. After addition of internal standards along with two-step protein precipitation and dilution sample preparation, plasma samples were analyzed on a C18 column using a gradient elution in 5 min without interference. The calibration curves were linear over a 100-fold concentration range, with determination coefficients (r 2 ) greater than 0.99 for all analytes. The limit of quantification was 0.5 μg mL−1 (0.1 μg mL−1 for oxcarbazepine, 2 μg mL−1 for levetiracetam, and 10 μg mL−1 for valproic acid) with precision and accuracy ranging from 3% to 9% and from 94% to 112%, respectively. Intra- and inter-day precision and accuracy values were within 15% at low, medium and high quality control levels. No significant matrix effect was observed in the normal, hemolyzed, lipemic, and hyperbilirubin blood samples. This method was successfully used in the identification and quantitation of antiepileptic drugs in patients undergoing mono- or polytherapy for epilepsy.
{"title":"Simultaneous determination of eight antiepileptic drugs and two metabolites in human plasma by liquid chromatography/tandem mass spectrometry","authors":"Hengyi Yu, Xiuhua Ren, Lu Liu, Dong Xiang, Xiping Li, Juan Li, Dong Liu, X. Gong","doi":"10.1556/1326.2022.01024","DOIUrl":"https://doi.org/10.1556/1326.2022.01024","url":null,"abstract":"\u0000 Epilepsy is one of the most prevalent neurological conditions and antiepileptic drugs are the mainstay of epilepsy treatment. High variation in pharmacokinetic profiles of several antiepileptic drugs highlights the importance of therapeutic drug monitoring to estimate pharmacokinetic properties and consequently individualize drug posology. In this work, a simple, rapid and robust liquid chromatography-tandem mass spectrometry method was developed for simultaneous quantification of carbamazepine and its metabolite carbamazepine-10,11-epoxide, gabapentin, levetiracetam, lamotrigine, oxcarbazepine and its metabolite mono-hydroxy-derivative metabolite, phenytoin, topiramate, and valproic acid in human plasma for therapeutic drug monitoring. d\u0000 \u0000 6\u0000 -Levetiracetam, d\u0000 \u0000 4\u0000 -gabapentin and d\u0000 \u0000 6\u0000 -valproic acid were used as internal standards. After addition of internal standards along with two-step protein precipitation and dilution sample preparation, plasma samples were analyzed on a C18 column using a gradient elution in 5 min without interference. The calibration curves were linear over a 100-fold concentration range, with determination coefficients (r\u0000 \u0000 2\u0000 ) greater than 0.99 for all analytes. The limit of quantification was 0.5 μg mL−1 (0.1 μg mL−1 for oxcarbazepine, 2 μg mL−1 for levetiracetam, and 10 μg mL−1 for valproic acid) with precision and accuracy ranging from 3% to 9% and from 94% to 112%, respectively. Intra- and inter-day precision and accuracy values were within 15% at low, medium and high quality control levels. No significant matrix effect was observed in the normal, hemolyzed, lipemic, and hyperbilirubin blood samples. This method was successfully used in the identification and quantitation of antiepileptic drugs in patients undergoing mono- or polytherapy for epilepsy.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43961100","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 rapid, selective, and precise high performance thin layer chromatographic method was developed and validated for the simultaneous analysis of paracetamol, caffeine, phenylephrine and chlorpheniramine in tablets. The chromatographic analysis was carried out on glass plates pre-coated with silica gel 60 F254 as a stationary phase. The optimized mobile phase was methanol : n-butanol : toluene : acetic acid (8:6:4:0.2 v/v). TLC chamber of 10 × 20 cm was used with saturation time of 15 min. The retardation factor (RF) for chlorpheniramine, phenylephrine, caffeine and paracetamol was found to be 0.15 ± 0.02, 0.29 ± 0.02, 0.50 ± 0.02, 0.68 ± 0.02 respectively. Detection was carried out at 212 nm. Validation study was done following ICH Q2 (R1) guideline. The regression data for the calibration plots showed good linear relationship with R 2 = 0.997 over the concentration range of 300–1,500 ng band−1 for caffeine, R 2 = 0.996 over the concentration range of 100–500 ng band−1 for phenylephrine, R 2 = 0.996 over the concentration range of 200–600 ng band−1 for chlorpheniramine, R 2 = 0.998 over the concentration range of 400–2,400 ng band−1 for paracetamol. The method was validated for precision, accuracy and recovery. Minimum detectable amounts were found to be 304.9 ng band−1, 87.88 ng band−1, 117.18 ng band−1 and 143.06 ng band−1 for caffeine, phenylephrine, chlorpheniramine, and paracetamol respectively while the limit of quantification was found to be 923.95 ng band−1, 266.32 ng band−1, 355.11 ng band−1, and 433.53 ng band−1 in the same order. The method was successfully applied to analyze two marketed tablets in a selective and reproducible manner.
{"title":"High performance thin layer chromatography (HPTLC) method development and validation for the simultaneous determination of paracetamol, caffeine, chlorpheniramine and phenylepherine in tablet formulation","authors":"Almas Arage, T. Layloff, A. Hymete, A. Ashenef","doi":"10.1556/1326.2022.01028","DOIUrl":"https://doi.org/10.1556/1326.2022.01028","url":null,"abstract":"\u0000 A rapid, selective, and precise high performance thin layer chromatographic method was developed and validated for the simultaneous analysis of paracetamol, caffeine, phenylephrine and chlorpheniramine in tablets. The chromatographic analysis was carried out on glass plates pre-coated with silica gel 60 F254 as a stationary phase. The optimized mobile phase was methanol : n-butanol : toluene : acetic acid (8:6:4:0.2 v/v). TLC chamber of 10 × 20 cm was used with saturation time of 15 min. The retardation factor (RF) for chlorpheniramine, phenylephrine, caffeine and paracetamol was found to be 0.15 ± 0.02, 0.29 ± 0.02, 0.50 ± 0.02, 0.68 ± 0.02 respectively. Detection was carried out at 212 nm. Validation study was done following ICH Q2 (R1) guideline. The regression data for the calibration plots showed good linear relationship with R\u0000 2 = 0.997 over the concentration range of 300–1,500 ng band−1 for caffeine, R\u0000 2 = 0.996 over the concentration range of 100–500 ng band−1 for phenylephrine, R\u0000 2 = 0.996 over the concentration range of 200–600 ng band−1 for chlorpheniramine, R\u0000 2 = 0.998 over the concentration range of 400–2,400 ng band−1 for paracetamol. The method was validated for precision, accuracy and recovery. Minimum detectable amounts were found to be 304.9 ng band−1, 87.88 ng band−1, 117.18 ng band−1 and 143.06 ng band−1 for caffeine, phenylephrine, chlorpheniramine, and paracetamol respectively while the limit of quantification was found to be 923.95 ng band−1, 266.32 ng band−1, 355.11 ng band−1, and 433.53 ng band−1 in the same order. The method was successfully applied to analyze two marketed tablets in a selective and reproducible manner.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43178702","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}
Perampanel (PER) is the first clinically available selective antagonist of α-amino-3-hydroxy-5-methylisoxazole-4-propionic acid (AMPA) receptor approved globally for the treatment of epilepsy. Studies have recently underlined the significant association between dose-exposure-effect-adverse events of PER in patients with epilepsy, so the therapeutic drug monitoring (TDM) of PER is critical in clinical practices, especially for pediatric patients with drug-resistant epilepsy. Due to several limits in previous published analytical methods, herein, we describe the development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) method for monitoring PER in human plasma samples. Protein precipitation method by acetonitrile containing PER-d5 as internal standard was applied for the sample clean-up. Formic acid (FA, 0.2 mM) in both aqueous water and acetonitrile were used as the mobile phases and the analyte was separated by an isocratic elution. Qualification and quantification were performed under positive electrospray ionization (ESI) mode using the m/z 350.3 → 219.1 and 355.3 → 220.0 ions pairs transitions for PER and PER-d5, respectively. Potential co-medicated anti-seizure medications (ASMs) have no interference to the analysis. Calibration curves were linear in the concentration range of 1.00–2,000 ng mL−1 for PER. The intra- and inter-batch precision, accuracy, recovery, dilution integrity, and stability of the method were all within the acceptable criteria and no matrix effect or carryover was found. This method was then successfully implemented on the TDM of PER in Chinese children with drug-resistant epilepsy. We firstly confirmed the apparent inter- and intra-individual PER concentration variabilities and potential drug-drug interactions between PER and several concomitant ASMs occurred in Chinese pediatric patients, which were also in line with previous studies in patients of other race.
Perampanel（PER）是第一种临床上可用的α-氨基-3-羟基-5-甲基异恶唑-4-丙酸（AMPA）受体选择性拮抗剂，在全球范围内被批准用于治疗癫痫。最近的研究强调了癫痫患者PER的剂量暴露效应不良事件之间的显著关联，因此PER的治疗药物监测（TDM）在临床实践中至关重要，尤其是对于耐药癫痫的儿科患者。由于先前发表的分析方法存在一些局限性，在此，我们描述了一种新的液相色谱-串联质谱（LC-MS/MS）方法的开发和验证，该方法用于监测人类血浆样品中的PER。采用以PER-d5为内标的乙腈沉淀蛋白质的方法对样品进行净化。甲酸（FA，0.2 mM）作为流动相，并通过等度洗脱分离分析物。使用m/z 350.3在正电喷雾电离（ESI）模式下进行鉴定和定量→ 219.1和355.3→ PER和PER-d5分别有220.0个离子对跃迁。潜在的联合用药抗癫痫药物（ASM）对分析没有干扰。在1.00–2000的浓度范围内，校准曲线呈线性 ng mL−1表示PER。该方法的批内和批间精密度、准确度、回收率、稀释完整性和稳定性均在可接受的标准范围内，未发现基质效应或残留。该方法随后在中国耐药癫痫儿童的PER TDM中成功实施。我们首先证实了在中国儿科患者中发生的PER和几种伴发ASM之间的明显个体间和个体内PER浓度变化以及潜在的药物-药物相互作用，这也与之前在其他种族患者中的研究一致。
{"title":"LC-MS/MS assay for the therapeutic drug monitoring of perampanel in children with drug-resistant epilepsy","authors":"Hao Dai, Ya-Hui Hu, Jia-Yi Long, Ying Xia, Hongli Guo, Jing Xu, Xuan-Sheng Ding, Jingkai Chen, Xiao-peng Lu, Feng Chen","doi":"10.1556/1326.2022.01023","DOIUrl":"https://doi.org/10.1556/1326.2022.01023","url":null,"abstract":"\u0000 Perampanel (PER) is the first clinically available selective antagonist of α-amino-3-hydroxy-5-methylisoxazole-4-propionic acid (AMPA) receptor approved globally for the treatment of epilepsy. Studies have recently underlined the significant association between dose-exposure-effect-adverse events of PER in patients with epilepsy, so the therapeutic drug monitoring (TDM) of PER is critical in clinical practices, especially for pediatric patients with drug-resistant epilepsy. Due to several limits in previous published analytical methods, herein, we describe the development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) method for monitoring PER in human plasma samples. Protein precipitation method by acetonitrile containing PER-d5 as internal standard was applied for the sample clean-up. Formic acid (FA, 0.2 mM) in both aqueous water and acetonitrile were used as the mobile phases and the analyte was separated by an isocratic elution. Qualification and quantification were performed under positive electrospray ionization (ESI) mode using the m/z 350.3 → 219.1 and 355.3 → 220.0 ions pairs transitions for PER and PER-d5, respectively. Potential co-medicated anti-seizure medications (ASMs) have no interference to the analysis. Calibration curves were linear in the concentration range of 1.00–2,000 ng mL−1 for PER. The intra- and inter-batch precision, accuracy, recovery, dilution integrity, and stability of the method were all within the acceptable criteria and no matrix effect or carryover was found. This method was then successfully implemented on the TDM of PER in Chinese children with drug-resistant epilepsy. We firstly confirmed the apparent inter- and intra-individual PER concentration variabilities and potential drug-drug interactions between PER and several concomitant ASMs occurred in Chinese pediatric patients, which were also in line with previous studies in patients of other race.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43570409","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}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：