Biomedical Chromatography最新文献

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A Simple Rapid HPLC-UV Method for Assessing C-Terminal Arginine Content in Darbepoetin Alfa 高效液相色谱-紫外快速测定达必泊汀α中c端精氨酸含量的方法
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.70018
Dmitry I. Zybin, Anatoly A. Klishin, Natalia V. Orlova, Yuri A. Seregin, Tatiana S. Sorokina, Dmitry V. Kapustin
{"title":"A Simple Rapid HPLC-UV Method for Assessing C-Terminal Arginine Content in Darbepoetin Alfa","authors":"Dmitry I. Zybin,&nbsp;Anatoly A. Klishin,&nbsp;Natalia V. Orlova,&nbsp;Yuri A. Seregin,&nbsp;Tatiana S. Sorokina,&nbsp;Dmitry V. Kapustin","doi":"10.1002/bmc.70018","DOIUrl":"https://doi.org/10.1002/bmc.70018","url":null,"abstract":"<div>\u0000 \u0000 <p>Upon the development of biosimilar drugs, the structural, physical–chemical, and functional similarity to the original drug should be ensured. We have proposed a simple and rapid HPLC-UV method for assessing the content of C-terminal Arg<sup>166</sup> in darbepoetin alfa samples, in particular after their isolation from the culture fluid. All the stages of the described method (from the sample extraction to obtaining a chromatographic profile) take about 5 h. The proposed approach will be useful for laboratories developing a technology for producing recombinant darbepoetin alfa, to assess the quality of the product, and for subsequent optimization of the production process.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362870","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Quantitative Comparison of Different Parts of Tribulus terrestris L. at Different Harvest Times and Comparison of Antihypertensive Effects at the Same Harvest Time 不同收获期刺蒺藜不同部位的定量比较和相同收获期抗高血压作用的比较
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.70005
Fei Li, De-Feng DU, Ming-Yue Chen, Xiao-Meng Gong, Hui-Min Su, Yi-Fan Wang, Lei Shi, Chao Zhang, Fei Guo
{"title":"Quantitative Comparison of Different Parts of Tribulus terrestris L. at Different Harvest Times and Comparison of Antihypertensive Effects at the Same Harvest Time","authors":"Fei Li,&nbsp;De-Feng DU,&nbsp;Ming-Yue Chen,&nbsp;Xiao-Meng Gong,&nbsp;Hui-Min Su,&nbsp;Yi-Fan Wang,&nbsp;Lei Shi,&nbsp;Chao Zhang,&nbsp;Fei Guo","doi":"10.1002/bmc.70005","DOIUrl":"https://doi.org/10.1002/bmc.70005","url":null,"abstract":"<div>\u0000 \u0000 <p>The whole plant of <i>Tribulus terrestris</i> (TT) is used to treat hypertension and cardio-cerebrovascular diseases. The harvest time has an important influence on the quality of medicinal plants. Therefore, it is necessary to study the effect of harvest time on the content of components in different parts of TT and compare the antihypertensive effect of different parts of TT at harvest time with a relatively high content of 14 components. Ultraviolet–visible spectrometry (UV–Vis spectrometry) was used to determine the total saponin content in <i>T. terrestris</i> fruit (TTF), <i>T. terrestris</i> stems (TTS), and <i>T. terrestris</i> leaves (TTL) at different harvest times. Within the studied harvest times, the total saponin content was higher in TTL than in TTF or TTS. Ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry analysis revealed significant differences in the spatial and temporal differences in the content of 14 components in the three plant parts. The multivariate statistical analysis identified six components as markers of different TT content in the different parts. The suitable TTF harvest period was from August 11 to September 1, while TTS and TTL were suitable for harvesting from July 21 to September 11. The treatment effects on blood pressure, serum indexes, and thoracic aorta morphology confirmed that the antihypertensive effects of TTL were better than those of TTF or TTS. The study emphasized the effect of harvest time on the content of components in different parts of TT and confirmed that TTS and TTL also had medicinal value.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362871","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Pesticide Residues in Ectoparasiticide-Impregnated Collars Using Ultrasound-Assisted Extraction and Liquid Chromatography–Mass Spectrometry 超声辅助萃取-液相色谱-质谱法测定体外寄生虫浸渍项圈中农药残留
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.70010
Pricília Santos Pereira Gomes, Luís Fabrício Santana Santos, Sandro Navickiene
{"title":"Determination of Pesticide Residues in Ectoparasiticide-Impregnated Collars Using Ultrasound-Assisted Extraction and Liquid Chromatography–Mass Spectrometry","authors":"Pricília Santos Pereira Gomes,&nbsp;Luís Fabrício Santana Santos,&nbsp;Sandro Navickiene","doi":"10.1002/bmc.70010","DOIUrl":"https://doi.org/10.1002/bmc.70010","url":null,"abstract":"<div>\u0000 \u0000 <p>Ectoparasiticide-impregnated collars are used on dogs and cats to control zoonoses, acting as repellents and/or killing vectors. The contact of animals or people with pesticides can cause intoxication, so ectoparasiticide-impregnated collars may be a potentially important source of these compounds. The aim of this work was to develop a method for the determination of propoxur, dichlorvos, diazinon, chlorpyrifos, deltamethrin, and flumethrin in commercial ectoparasiticide-impregnated collars, using ultrasound-assisted extraction and liquid chromatography–mass spectrometry. The total ultrasound extraction time was 45 min, resulting in recovery values between 40 ± 6% and 103 ± 8%, in the concentration range from 0.005 to 1.0 mg L<sup>−1</sup>. Under optimal conditions, good linearity and sensitivity were obtained in the concentration range from 0.005 to 5.0 mg L<sup>−1</sup> with coefficients of determination above 0.99. The relative standard deviations for triplicate determinations were lower than 24%, and the limits of detection and quantification were in the ranges 0.013–1.36 and 0.036–4.13 mg kg<sup>−1</sup>, respectively. The proposed method was applied in the analysis of a commercial collar, after its expiry date, and flumethrin residues were found.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362879","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A Selective and Sensitive Method Development and Validation for Impurity Quantification in Cysteamine Bitartrate Bulk and Formulation by RP-HPLC 反相高效液相色谱法测定重酒石酸半胱胺原料药和制剂中杂质的选择性和灵敏度
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.70007
Prasanth Katakam, Umesh N. Pathak, Vijay Kumar Chollety, Bharat Kumar Tripuramallu
{"title":"A Selective and Sensitive Method Development and Validation for Impurity Quantification in Cysteamine Bitartrate Bulk and Formulation by RP-HPLC","authors":"Prasanth Katakam,&nbsp;Umesh N. Pathak,&nbsp;Vijay Kumar Chollety,&nbsp;Bharat Kumar Tripuramallu","doi":"10.1002/bmc.70007","DOIUrl":"https://doi.org/10.1002/bmc.70007","url":null,"abstract":"<div>\u0000 \u0000 <p>RP-HPLC was used to develop and validate a simple, selective, and sensitive impurity quantification method for cysteamine bitartrate formulation. Chromatographic separation was achieved using Shim-pack Sceptre HD-C<sub>18</sub>-5 μm 4.6 × 250 mm column. The mobile phase-A was 43 mM 1-hexane sulfonic acid sodium salt monohydrate buffer adjusted to pH 2.2 with 0.1% orthophosphoric acid. Mobile phase-B was acetonitrile. The column oven temperature was 40°C, and gradient elution was done at 0.8 mL per minute, and the gradient program was T/A: 0/100, 12/100, 12.1/90, 30/80, 35/70, 45/70, 45.1/100, and 60/100. To measure component quantities, a 200 nm wavelength and 10 μL injection volumes were utilized. The drug product and drug substance were subjected to the stress conditions such as acid, base, oxidation, heat, and photolysis as per the recommendations of the International Conference on Harmonization (Q2) methodology. Stress research shows that the approach is stable and peak homogeneous. High accuracy (97%–103% recoveries), precision (≤ 1.0%), specificity (R2 &gt; 0.999), and linearity (R2  &gt; 0.999) were achieved with the approach. The detection limit (LOD) was 0.3 μg mL<sup>−1</sup>, whereas the quantification limit (LOQ) was 1.0 μg mL<sup>−1</sup>. The analytical method was validated according to ICH and USP &lt; 1225 &gt; guidelines. For quality control, the method was exact, particular, linear, accurate, and resilient.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362880","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A Validated Liquid Chromatography–Tandem Mass Spectrometry Assay for the Determination of NX-5948 in Beagle Dog Plasma: Application to a Pharmacokinetic Study 液相色谱-串联质谱法测定比格犬血浆中NX-5948:在药代动力学研究中的应用
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.6090
Fang Wang, Wenfei Sun, Zheheng Ma, Furui Chu
{"title":"A Validated Liquid Chromatography–Tandem Mass Spectrometry Assay for the Determination of NX-5948 in Beagle Dog Plasma: Application to a Pharmacokinetic Study","authors":"Fang Wang,&nbsp;Wenfei Sun,&nbsp;Zheheng Ma,&nbsp;Furui Chu","doi":"10.1002/bmc.6090","DOIUrl":"https://doi.org/10.1002/bmc.6090","url":null,"abstract":"<div>\u0000 \u0000 <p>Proteolysis targeting chimera (PROTAC) has been developed and currently enjoys widespread interest among the field of pharmaceutical manufacturing in recent decades. NX-5948 is an orally active PROTAC Bruton tyrosine kinase degrader, which shows anti-inflammatory and antitumor activities. In this study, a simple and fast bioanalytical method for the quantification of NX-5948 in beagle dog plasma was developed using liquid chromatography–tandem mass spectrometry (LC-MS/MS). A full method validation was performed according to regulatory guidelines. For the quantification, [M + H]<sup>+</sup> was formed using an electrospray ionization (ESI) source in the positive ion mode, and selective reaction monitoring (SRM) was employed using a triple quadrupole mass spectrometry. The monitored precursor-to-product transitions were <i>m/z</i> 807.5 &gt; 790.5 for NX-5948 and <i>m/z</i> 812.4 &gt; 452.1 for internal standard. A linear response was obtained at the concentration range of 0.5–200 ng/mL, with correlation coefficient &gt; 0.99. The interday accuracy ranged from −9.03% to 5.99% (RSD &lt; 7.84%), and the intraday accuracy from −5.15% to 8.56% (RSD &lt; 6.90%). NX-5948 was demonstrated to be stable under the present storage conditions. After validation, the method was successfully applied for the quantification of NX-5948 in beagle dog plasma after oral and intravenous administration of the NX-5948.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362883","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Simultaneous Determination and Pharmacokinetics of Three Steroidal Alkaloids in Rat Plasma by UHPLC–MS After Oral Administration of Three Different Preparations of Fritillaria ussuriensis Maxim Bulb UHPLC-MS同时测定三种乌苏贝母制剂大鼠血浆中三种甾体生物碱的药动学
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.6087
Haibo Wu, Chunjuan Yang, Jingnan Chen, Sen Li, Yuxin Wei, Meng Wang, Xinlan Li, YanYan Wang, Haixue Kuang, Zhibin Wang
{"title":"Simultaneous Determination and Pharmacokinetics of Three Steroidal Alkaloids in Rat Plasma by UHPLC–MS After Oral Administration of Three Different Preparations of Fritillaria ussuriensis Maxim Bulb","authors":"Haibo Wu,&nbsp;Chunjuan Yang,&nbsp;Jingnan Chen,&nbsp;Sen Li,&nbsp;Yuxin Wei,&nbsp;Meng Wang,&nbsp;Xinlan Li,&nbsp;YanYan Wang,&nbsp;Haixue Kuang,&nbsp;Zhibin Wang","doi":"10.1002/bmc.6087","DOIUrl":"https://doi.org/10.1002/bmc.6087","url":null,"abstract":"<div>\u0000 \u0000 <p>Pharmacokinetic studies can provide a method for optimizing preparations. In this study, three most abundant compounds from <i>Fritillaria ussuriensis</i> bulb were isolated, and a selective, sensitive new analytical method was developed. This method aims for the simultaneous determination of peimisine-3-O-β-D-glucopyranoside (<b>1</b>), karelinine (<b>2</b>), and peimisine (<b>3</b>) in rat plasma after oral administration of <i>F. ussuriensis</i> bulb powder (FUP), total alkaloid extract (FUE), and its nanodispersion preparation (FUN) using UHPLC–MS/MS. The chromatographic separation was performed on the UHPLC Waters BEH C18 column. The pharmacokinetic results showed that among three groups, <b>1</b> and <b>3</b> exhibited slower absorption and elimination processes when rats were orally administered with FUP and FUE. Steroidal alkaloids <b>1</b> ~ <b>3</b> from FUN reached peak concentrations within 3 h. Compared with FUE and FUP, the absorption and elimination rates were accelerated, and the area under the curve (AUC) significantly increased. In this study, the pharmacokinetic characteristics of <b>1</b> ~ <b>2</b> were first detected and calculated parameters in rat plasma when orally administered in different dosage forms. And a new nanodispersion preparation, FUN, has been developed. FUN has better absorption efficiency and higher bioavailability compared with traditional powder oral administration.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362842","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Bioanalytical Tandem Mass Spectrometry Method for Precise Measurement of Tranexamic Acid in Human Plasma With Unveiling Methodological Advancement: Green Assessment With Advanced Metrics 生物分析串联质谱法精确测量人血浆中氨甲环酸的方法学进展:绿色评价与先进指标
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.6086
Anil Kollapareddy, Kousrali Sayyad, Leela Prasad Kowtharapu, Naresh Konduru, Tanmoy Mondal, Mohan Varkolu, Sreedhar Gundekari
{"title":"Bioanalytical Tandem Mass Spectrometry Method for Precise Measurement of Tranexamic Acid in Human Plasma With Unveiling Methodological Advancement: Green Assessment With Advanced Metrics","authors":"Anil Kollapareddy,&nbsp;Kousrali Sayyad,&nbsp;Leela Prasad Kowtharapu,&nbsp;Naresh Konduru,&nbsp;Tanmoy Mondal,&nbsp;Mohan Varkolu,&nbsp;Sreedhar Gundekari","doi":"10.1002/bmc.6086","DOIUrl":"https://doi.org/10.1002/bmc.6086","url":null,"abstract":"<div>\u0000 \u0000 <p>For the control of excessive blood loss occurring from major trauma, postpartum bleeding, surgery, or hereditary angioedema, antifibrinolytic compound tranexamic acid (TXM) is highly efficient in controlling blood loss by reversibly binding with on lysine receptor sites. A selective and sensitive method has been developed and validated for the quantitation of TXM in human plasma using high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Tranexamic acid-D2 (TXM-D2) was used as internal standard (ISTD) to minimize the errors in TXM quantification. TXM quantification was performed with positive polarity mode using a Shimadzu high performance liquid chromatography coupled with AB-SCIEX API-4000 tandem mass spectrometer. A Zorbax Eclipse C18 (150 × 4.6 mm, 5 μ) column was used for the TXM quantification, 8-mM ammonium formate buffer with 0.1% formic acid ionization enhancer was used as a mobile phase-A, and acetonitrile was used as a mobile phase-B. (38:62) v/v portion of mobile phases A and B selected to elute the TXM and TXM-D2 with the flow rate of 0.8 mL/min. An electrospray ionization (ESI) technique was selected for detection of TXM in the human plasma. Linearity was assessed in the concentration range from 75 to 15,000 ng/mL by using least squares of weighting factor linear regression (1/X<sup>2</sup>).</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362844","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
LGZGD for Gestational Diabetes Mellitus: Integration of Traditional Chinese Medicine With Modern Research Evidence—A Letter to the Editor LGZGD治疗妊娠期糖尿病:中医与现代研究证据的结合——致编辑的一封信
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.70015
Lien-Chung Wei, Hsien-Jane Chiu
{"title":"LGZGD for Gestational Diabetes Mellitus: Integration of Traditional Chinese Medicine With Modern Research Evidence—A Letter to the Editor","authors":"Lien-Chung Wei,&nbsp;Hsien-Jane Chiu","doi":"10.1002/bmc.70015","DOIUrl":"https://doi.org/10.1002/bmc.70015","url":null,"abstract":"<div>\u0000 \u0000 <p>This letter responds to recent research on Lingguizhugan decoction (LGZGD) in treating gestational diabetes mellitus (GDM). While acknowledging the significance of their findings regarding PI3K-AKT pathway modulation and oxidative stress reduction, we suggest expanding future research directions. We highlight the importance of incorporating animal models alongside cell studies, considering multiple mechanistic pathways, and integrating traditional Chinese medicine approaches with modern research methodologies. Recent studies on natural antioxidants and traditional Chinese medicines in GDM treatment provide supporting evidence for these recommendations. These perspectives aim to enhance understanding of LGZGD's therapeutic potential and contribute to developing more effective GDM treatments.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362873","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Unique Liquid Chromatography Technique for Determining a New Selective PPARα Modulator Drug (Pemafibrate) in the Tablet Dosage Form, Robustness by Design Expert in the Light of Quality by Design 独特的液相色谱法测定新型选择性PPARα调节剂(培马非特)片剂剂型的稳健性
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.70006
Fei Han, Yankun Yang, Zhonghu Bai, Rathnakar Nathi, Naresh Konduru
{"title":"Unique Liquid Chromatography Technique for Determining a New Selective PPARα Modulator Drug (Pemafibrate) in the Tablet Dosage Form, Robustness by Design Expert in the Light of Quality by Design","authors":"Fei Han,&nbsp;Yankun Yang,&nbsp;Zhonghu Bai,&nbsp;Rathnakar Nathi,&nbsp;Naresh Konduru","doi":"10.1002/bmc.70006","DOIUrl":"https://doi.org/10.1002/bmc.70006","url":null,"abstract":"<div>\u0000 \u0000 <p>This research study presents a precise, accurate, and linear liquid-chromatography method for the determination of pemafibrate in tablet dosage forms, despite the presence of a high volume of excipients. Various challenges were addressed through experimental approaches and evidence-based solutions. The method employs a suitable stationary phase, X-Bridge C<sub>18</sub> (150 × 4.6 mm, 3.5 μm), and an appropriate isocratic program. Key parameters include a flow rate of 1.0 mL/min, a column temperature of 40°C, an injection volume of 10 μL, and a runtime of 15 min. The wavelength was set at 210 nm because of its high response. Mobile phase optimization, based on experimental results, consists of 0.1% H<sub>3</sub>PO<sub>4</sub> buffer and acetonitrile in a 40:60 v/v ratio. The method has been validated according to ICH Q2 (R2) and Ch. P &lt;9101&gt; guidelines, achieving a recovery rate of 99.1% to 100.5% at levels of 50%, 100%, and 150%. Linearity was demonstrated from 25% to 300% concentration levels, with a correlation coefficient (<i>r</i><sup>2</sup>) value of 1.000. Precision results showed %RSD values of 1.0 and 1.1. Forced degradation studies indicated sensitivity to acid hydrolysis stress conditions and stability under physical stress conditions.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362869","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Identification of Chemical Constituents and Rat Metabolites of Jianpihuazhuotiaozhi Granule by Ultra-High-Performance Liquid Chromatography Coupled With Quadrupole-Time-of-Flight Mass Spectrometry 超微高效液相色谱-四极杆飞行时间质谱联用鉴定健脾化浊调脂颗粒化学成分及大鼠代谢物
IF 1.8 4区 医学
Biomedical Chromatography Pub Date : 2025-02-07 DOI: 10.1002/bmc.6080
Guo-Dong Hao, Zhi-Qiang Li, Yu-Wei Wang, Yuan-Ying Fang, Zhi-Feng Li, Qi Wang
{"title":"Identification of Chemical Constituents and Rat Metabolites of Jianpihuazhuotiaozhi Granule by Ultra-High-Performance Liquid Chromatography Coupled With Quadrupole-Time-of-Flight Mass Spectrometry","authors":"Guo-Dong Hao,&nbsp;Zhi-Qiang Li,&nbsp;Yu-Wei Wang,&nbsp;Yuan-Ying Fang,&nbsp;Zhi-Feng Li,&nbsp;Qi Wang","doi":"10.1002/bmc.6080","DOIUrl":"https://doi.org/10.1002/bmc.6080","url":null,"abstract":"<div>\u0000 \u0000 <p>Jianpihuazhuotiaozhi granules (JPHZTZ) are traditional Chinese medicine formula. An analytical method using ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry was established to characterize the chemical constituents of JPHZTZ and determine its metabolic profile in rat urine and plasma after oral administration. A total of 220 compounds were identified in JPHZTZ extract, including 61 flavonoids, 16 alkaloids, 53 organic acids, 31 terpenoids, and 59 other compounds. Among these compounds, 11 were tentatively identified by comparing the retention times and mass spectral data with the corresponding reference standards and the literature; the other 209 components were tentatively identified based on their mass spectra alone. After the oral administration of JPHZTZ extract to rats, 13 prototypes and 54 metabolites were identified or tentatively characterized based on their retention time and mass spectra. The primary in vivo metabolic reactions that occurred after the administration of JPHZTZ extract included glucuronidation, sulfation, hydroxylation, and methylation. The 13 prototypes and 54 metabolites were identified in rat urine and plasma and were confirmed to be the potential active ingredients of JPHZTZ. Our findings provide a starting point for the further elucidation of the mechanism of action of JPHZTZ.</p>\u0000 </div>","PeriodicalId":8861,"journal":{"name":"Biomedical Chromatography","volume":"39 3","pages":""},"PeriodicalIF":1.8,"publicationDate":"2025-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143362872","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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