Marija Čarapić, B. Marković, Milena Pavlović, D. Agbaba, K. Nikolić
Ziprasidone is the second generation antipsychotic drug with unique multipotent G-protein-coupled (GPCR) receptor binding profile. Since ziprasidone is a highly lipophilic and unstable compound, development of efficient method for a concurrent assay of ziprasidone and its main impurities was a very challenging task. The UHPLC-MS/MS method that we developed for simultaneous determination of ziprasidone and its main impurities (BITP, Chloroethyl-chloroindolinone, Zip-oxide, Zip-dimer, and Zip-BIT) was compared with some other related HPLC-UV methods of our own and other authorship. An increase of the mobile phase pH value from 2.5 to 4.7 units in the examined analytical methods influenced elution order of the investigated compounds. It was found out that the UHPLC-MS/MS method is more selective and sensitive than the earlier developed HPLC-UV method. Similar to our earlier HPLC-UV method, the UHPLC-MS/MS method is linear with a correlation coefficient (r) above 0.99 for all the analysed compounds, but with a negligibly lower precision and accuracy. Finally, with shorter analysis time, smaller column size and reduction of solvent consumption, UHPLC-MS/MS is assumed as a greener method than HPLC-UV for the ziprasidone purity assay. After transfer of the UHPLC-MS/MS method to the UHPLC-DAD system, suitability of the UHPLC-DAD method for routine control of ziprasidone and its main impurities is examined and confirmed based on the retained good selectivity, resolution and short analysis time.
{"title":"Comparative study of performances of UHPLC-MS/MS and HPLC/UV methods for analysis of ziprasidone and its main impurities","authors":"Marija Čarapić, B. Marković, Milena Pavlović, D. Agbaba, K. Nikolić","doi":"10.1556/1326.2022.01060","DOIUrl":"https://doi.org/10.1556/1326.2022.01060","url":null,"abstract":"\u0000 Ziprasidone is the second generation antipsychotic drug with unique multipotent G-protein-coupled (GPCR) receptor binding profile. Since ziprasidone is a highly lipophilic and unstable compound, development of efficient method for a concurrent assay of ziprasidone and its main impurities was a very challenging task.\u0000 The UHPLC-MS/MS method that we developed for simultaneous determination of ziprasidone and its main impurities (BITP, Chloroethyl-chloroindolinone, Zip-oxide, Zip-dimer, and Zip-BIT) was compared with some other related HPLC-UV methods of our own and other authorship. An increase of the mobile phase pH value from 2.5 to 4.7 units in the examined analytical methods influenced elution order of the investigated compounds. It was found out that the UHPLC-MS/MS method is more selective and sensitive than the earlier developed HPLC-UV method. Similar to our earlier HPLC-UV method, the UHPLC-MS/MS method is linear with a correlation coefficient (r) above 0.99 for all the analysed compounds, but with a negligibly lower precision and accuracy. Finally, with shorter analysis time, smaller column size and reduction of solvent consumption, UHPLC-MS/MS is assumed as a greener method than HPLC-UV for the ziprasidone purity assay.\u0000 After transfer of the UHPLC-MS/MS method to the UHPLC-DAD system, suitability of the UHPLC-DAD method for routine control of ziprasidone and its main impurities is examined and confirmed based on the retained good selectivity, resolution and short analysis time.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-06-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41530635","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}
Wild edible plants (WEPs) can be widely found in the world and defined as native species that grow naturally in their natural habitat. They have become part of the traditional food as human diet and used in folk medicine to treat diseases. They are very rich in terms of nutraceuticals. Melatonin is a natural hormone providing several benefits for human health. It has functions such as regulating growth and development and increasing tolerance to environmental stress factors in plants. It is stated that the serum melatonin level in humans increases after intake of foods containing melatonin. This study examined the presence of melatonin in wild grown cornelian cherry fruits by UFLC-FD and determined suitable extraction and chromatographic conditions. The optimum mobile phase, excitation/emission wavelength, and extraction solvent were determined as methanol: water: acetic acid, 275/345 nm, and methanol: water: HCl, respectively. Melatonin content in fruits ranged from 130.82 to 201.84 ng g−1 in fresh fruit.
{"title":"Extraction and quantification of melatonin in cornelian cherry (Cornus mas L.) by ultra-fast liquid chromatography coupled to fluorescence detector (UFLC-FD)","authors":"Y. Uğur","doi":"10.1556/1326.2022.01052","DOIUrl":"https://doi.org/10.1556/1326.2022.01052","url":null,"abstract":"\u0000 Wild edible plants (WEPs) can be widely found in the world and defined as native species that grow naturally in their natural habitat. They have become part of the traditional food as human diet and used in folk medicine to treat diseases. They are very rich in terms of nutraceuticals. Melatonin is a natural hormone providing several benefits for human health. It has functions such as regulating growth and development and increasing tolerance to environmental stress factors in plants. It is stated that the serum melatonin level in humans increases after intake of foods containing melatonin. This study examined the presence of melatonin in wild grown cornelian cherry fruits by UFLC-FD and determined suitable extraction and chromatographic conditions. The optimum mobile phase, excitation/emission wavelength, and extraction solvent were determined as methanol: water: acetic acid, 275/345 nm, and methanol: water: HCl, respectively. Melatonin content in fruits ranged from 130.82 to 201.84 ng g−1 in fresh fruit.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46698508","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}
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}
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