Journal of chromatographic science最新文献_第10页

A Simple and Sensitive LC-MS/MS Method for Determination of Dapagliflozin and Its Major Metabolite in Human Plasma. hplc -MS/MS法测定人血浆中达格列净及其主要代谢物的含量

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf019

Zhijun Liu, Yanru Liu, Zhipeng Wang, Huiping Lu, Xiujing Zhu, Yuxi Bao, Bingyan Cai, Shouhong Gao, Xia Tao, Deduo Xu

{"title":"A Simple and Sensitive LC-MS/MS Method for Determination of Dapagliflozin and Its Major Metabolite in Human Plasma.","authors":"Zhijun Liu, Yanru Liu, Zhipeng Wang, Huiping Lu, Xiujing Zhu, Yuxi Bao, Bingyan Cai, Shouhong Gao, Xia Tao, Deduo Xu","doi":"10.1093/chromsci/bmaf019","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf019","url":null,"abstract":"Dapagliflozin (DAPA), an inhibitor of sodium-dependent glucose cotransporter-2, has been created to treat individuals with type 2 diabetes mellitus. A method was developed and validated using high-performance liquid chromatography coupled to tandem mass spectrometry to aid in studying the connection between clinical effectiveness and concentration of DAPA and its primary metabolite dapagliflozin 3-O-glucuronide (D3OG) in human plasma. The two analytes were separated using the Waters XSELECT HSS T3 (2.1 × 100 mm, 3.5 μm; Waters Co., Milford, USA) chromatographic column, with a mobile phase flow rate of 0.3 mL/min. The elution program was performed after protein precipitation with methanol, which only required a 5-min duration. The extraction recovery was from 99.8 to 109% for DAPA and from 101 to 103% for D3OG. Validation of the method for detecting DAPA within the range of 5-50 ng/mL and D3OG within the range of 50-500 ng/mL demonstrated satisfactory inter- and intra-day precision and accuracy. The method was successfully developed and validated, and it was used to measure the levels of DAPA and D3OG in plasma samples from patients with type 2 diabetes mellitus.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144013080","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}

引用次数: 0

A New Method for the Quantification of Ethyl Sulfate and Isopropyl Sulfate Contents in Abacavir Sulfate by Ion Chromatography. 离子色谱法测定硫酸阿巴卡韦中硫酸乙酯和硫酸异丙酯含量的新方法。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf023

Venkata Ramana Reddy Junuthula, Surendra Babu Manabolu Surya, Naresh Kumar Katari, Chandrasekhar Reddy Kandati, Narendra Kumar Masani, Hemant Kumar Sharma

{"title":"A New Method for the Quantification of Ethyl Sulfate and Isopropyl Sulfate Contents in Abacavir Sulfate by Ion Chromatography.","authors":"Venkata Ramana Reddy Junuthula, Surendra Babu Manabolu Surya, Naresh Kumar Katari, Chandrasekhar Reddy Kandati, Narendra Kumar Masani, Hemant Kumar Sharma","doi":"10.1093/chromsci/bmaf023","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf023","url":null,"abstract":"A predictable new method was developed and validated for the determination of ethyl sulfate (EtS) and isopropyl sulfate (IprS) contents in abacavir sulfate (ABS) drug substance by ion chromatography (IC). Ethyl alcohol, isopropyl alcohol and sulfuric acids were used in the manufacturing process of ABS. Therefore, there is a possibility to form respective sulfate impurities, i.e., EtSs and IprSs. Hence, a control strategy is required for EtS and IprS contents in ABS. Chromatographic separation of EtS and IprS contents in Abacavir sulfate was achieved on Metrosep A Supp 10 (250 mm × 4.0 mm) column and particles of 4.6 μm size. The mobile phase consists of buffer (3.2 mM Sodium carbonate and 1.0 mM of sodium bicarbonate) and acetonitrile in the ratio of 90:10 (v/v) with the flow rate of 0.6 mL min-1 by applying 30°C column oven temperature. The analytes were monitored by conductometric detector. The performance of the method was assessed by evaluating the specificity, linearity, sensitivity, precision, robustness and accuracy experiments. The limit of detection and limit of quantification values for EtS were 0.3 and 0.8 μg mL-1 and for IprS were 0.3 and 0.8 μg mL-1, respectively. The correlation co-efficient value of linearity experiment was 0.9999 for EtS, 0.9998 for IprS. The average recovery for EtS was 98.7% and for IprS was 100.9%. The method is robust for EtS and IprS contents and also specific from other common anions, i.e., chloride, bromide, nitrate, sulfate, methyl sulfate and methanesulfonic acids. The results proved that the validated method was simple and cost-effective for controlling EtS and IprS contents in ABS drug substance, and the method can be successfully applied in the quality control analysis.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144026661","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}

引用次数: 0

Quality Evaluation of Qingwei Huanglian Pills Based on Fingerprint and Quantitative Analysis of Multi-Index Components Combined with Chemical Pattern Recognition Analysis. 基于指纹图谱和多指标成分定量分析结合化学模式识别分析的清胃黄连丸质量评价。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmaf018

Xiaowei Shao, Nan Zhao, Yuping Li, Hongming Wang, Xueli Xu, Shuyue Wang

{"title":"Quality Evaluation of Qingwei Huanglian Pills Based on Fingerprint and Quantitative Analysis of Multi-Index Components Combined with Chemical Pattern Recognition Analysis.","authors":"Xiaowei Shao, Nan Zhao, Yuping Li, Hongming Wang, Xueli Xu, Shuyue Wang","doi":"10.1093/chromsci/bmaf018","DOIUrl":"10.1093/chromsci/bmaf018","url":null,"abstract":"Qingwei Huanglian Pills (QHPs) is one of the most commonly used traditional Chinese medicine preparations for the treatment of mouth and tongue sores, but the existing quality evaluation standards have certain shortcomings and deficiencies. An effective and scientific quality evaluation method plays a vital role in medication safety. In this study, fingerprint and quantitative analysis of multi-index components combined with chemical pattern recognition analysis was used to comprehensively evaluate the quality of QHPs. The fingerprints of 15 batches of QHPs were generated and evaluated for similarity, with 10 characteristic peaks identified. Clustering hierarchical cluster analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) were employed to cluster and rank the 15 batches, while simultaneously identifying the components responsible for differences between batches. The HPLC fingerprints of QHPs, along with the content determination of 10 components, were established. Twenty-eight common peaks were identified, and 10 components were specified. The similarity between the 15 batches of samples ranged from 0.983 to 0.999. Cluster analysis and comprehensive score ranking of 15 batches of samples were performed by HCA and PCA, respectively, and 13 chemical markers affecting batch differences were screened by OPLS-DA. The method established here can serve as a reference for the quality evaluation and product quality control of QHPs.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143752994","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}

引用次数: 0

A General Strategy to Rapid and Sensitive Determination of Five High Boiling Point Solvents in Pharmaceuticals by RP-HPLC Combined with Precipitation Method. 结合沉淀法的 RP-HPLC 快速灵敏测定药物中五种高沸点溶剂的一般策略

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-03-27 DOI: 10.1093/chromsci/bmae057

Chenxia Zhang, Zeyi Wu, Meiyan Qiu, Yanhua Li, Zhongqing Wang, Xiaomei Fan, Shaoyu Cai, Wanbing Rao

{"title":"A General Strategy to Rapid and Sensitive Determination of Five High Boiling Point Solvents in Pharmaceuticals by RP-HPLC Combined with Precipitation Method.","authors":"Chenxia Zhang, Zeyi Wu, Meiyan Qiu, Yanhua Li, Zhongqing Wang, Xiaomei Fan, Shaoyu Cai, Wanbing Rao","doi":"10.1093/chromsci/bmae057","DOIUrl":"10.1093/chromsci/bmae057","url":null,"abstract":"The difficulty on determination of high boiling point solvents, always exist due to their low vapor pressure in headspace (HS) vial. What's worse, the commonly used GC diluents, such as N, N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, dimethyl sulfoxide, N, N-dimethylformamide and N-methylpyrrolidone are often remained in HS instrument after frequent injection into HS, thus would result in terrible positive interference problem. In this work, a fast and sensitive HPLC method in combination with a sample precipitation method, was proposed for the determination of above five high boiling point solvents in drug substances within 14.5 min. The final method was validated with regard to limit of detection and limit of quantitation, precision, linearity and accuracy in accordance with ICH Q2 (R1). Finally, the proposed strategy was successfully applied for the analysis of high boiling point solvents used in three active pharmaceutical ingredients. The established generic strategy would provide another choice for the determination of high boiling point solvents in pharmaceuticals.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142621360","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}

引用次数: 0

Verifying the Equivalence of Hawthorn Leaves Standard Decoction and Formula Granules by LC-MS and Oxidative Stress Test. 用LC-MS和氧化应激试验验证山楂叶标准汤和配方颗粒的等效性。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-02-08 DOI: 10.1093/chromsci/bmad089

Ling-Di Wang, Jing-Yun Gao, Li-Ying Duan, Hai-Feng Pan

{"title":"Verifying the Equivalence of Hawthorn Leaves Standard Decoction and Formula Granules by LC-MS and Oxidative Stress Test.","authors":"Ling-Di Wang, Jing-Yun Gao, Li-Ying Duan, Hai-Feng Pan","doi":"10.1093/chromsci/bmad089","DOIUrl":"10.1093/chromsci/bmad089","url":null,"abstract":"Objective: To verify the equivalence of hawthorn leaves standard decoction and formula granules.Methods: In this experiment, liquid chromatograph mass spectrometer (LC-MS) was used to examine the chemical composition of hawthorn leaves standard decoction and formula granules, separately. In addition, oxidative stress test was used to explore the antioxidant capacity of them.Results: 71 chemical components were identified by LC-MS. Among them, 64 and 56 compounds were identified in the standard decoction and formula granules, respectively. There were a total of 49 common components, with no significant difference in content. Oxidative stress test showed that hawthorn leaves standard decoction and formula granules had no obvious toxicity to human umbilical vein endothelial cells. Compared with the model group, the same dose of hawthorn leaves formula granule and standard decoction could inhibit the secretion of lactate dehydrogenase and malondialdehyde (P < 0.05), and increase the content of superoxide dismutase (P < 0.01), with no statistically significant difference.Conclusions: There is no significant difference in the main active ingredients between the standard decoction and the formula granules, and the antioxidant activity in vitro is equivalent, providing an important theoretical basis for the further development of hawthorn leaves formula granules.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138482424","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}

引用次数: 0

Study of Pharmacokinetics for Ivermectin B1a from Beagle Dogs. 比格犬伊维菌素 B1a 的药代动力学研究

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-02-08 DOI: 10.1093/chromsci/bmad092

Yuyang Chen, Xiaofang Huang, Zizheng Guo, Jingyu Zhang, Lixin Zhang, Renke Dai

{"title":"Study of Pharmacokinetics for Ivermectin B1a from Beagle Dogs.","authors":"Yuyang Chen, Xiaofang Huang, Zizheng Guo, Jingyu Zhang, Lixin Zhang, Renke Dai","doi":"10.1093/chromsci/bmad092","DOIUrl":"10.1093/chromsci/bmad092","url":null,"abstract":"Ivermectin has been widely used for antiparasitic drug, and has recently shown a broad-spectrum antiviral activity, including anti-Severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2). However, the pharmacokinetic property of ivermectin has not been fully investigated yet. During the plasma preparation, ~32-46% of ivermectin was found in the precipitation. An Liquid Chromatograph-Mass Spectrometer (LC-MS/MS) method for ivermectin in the whole blood samples from beagle dogs was developed and validated. The specificity, accuracy, precision (intra-day and inter-day), matrix effect, recovery and stability of analyte reported here are satisfied with the criteria of Food and Drug Administration (FDA)-Bioanalysis guideline. The oral administrations pharmacokinetics of ivermectin in beagle dogs under fasting and after high-fat meal were studied, and the following parameters were obtained: fasting Cmax, 104 ± 35 μg·L-1; area under the concentration-time curve (AUC0-∞), 2,555 ± 941 h·μg·L-1; and high-fat meal Cmax, 147 ± 35 μg·L-1; AUC0-∞, 4,198 ± 1,279 h·μg·L-1. When the P-gp inhibitor curcumin was also coadministrated orally, Cmax and AUC0-∞ were found to be 177 ± 57 and 4,213 ± 948 h·μg·L-1, respectively. With the comparison to fasting treatment, coadministration of P-gp inhibitor curcumin resulted in increase of the exposure of ivermectin by 1.6-fold, while the exposure after the high-fat diet versus fasting was increased approximately in 1.4-fold, indicating that alternative absorption might play an important role for increasing the exposure of ivermectin for future clinic applications.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138885095","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}

引用次数: 0

An Analytical Approach by Tri-Combination of Gradient UFLC, Response Surface Methodology and Green Chemistry Principle for Simultaneous Quantification of Azelnidipine and Chlorthalidone in Rabbit Plasma. 梯度超高效液相色谱法、响应面法和绿色化学原理三结合分析法用于兔血浆中阿折地平与氯沙坦酮的同时定量分析

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-02-08 DOI: 10.1093/chromsci/bmae032

C Bhagyalakshmi, T N Rekha, Piyongsola Longkumer, Koushik Nandan Dutta, Bhargab Jyoti Sahariah, B Ramesh, Manish Majumder

{"title":"An Analytical Approach by Tri-Combination of Gradient UFLC, Response Surface Methodology and Green Chemistry Principle for Simultaneous Quantification of Azelnidipine and Chlorthalidone in Rabbit Plasma.","authors":"C Bhagyalakshmi, T N Rekha, Piyongsola Longkumer, Koushik Nandan Dutta, Bhargab Jyoti Sahariah, B Ramesh, Manish Majumder","doi":"10.1093/chromsci/bmae032","DOIUrl":"10.1093/chromsci/bmae032","url":null,"abstract":"In this study, a sustainable and eco-friendly method is developed to quantify azelnidipine and chlorthalidone in rabbit plasma by gradient liquid chromatography based on green chemistry principle and analytical quality by design. The separation was achieved on a Shim pack C18 (25 cm × 5 cm × 4.6 μm) column with L1 packing. The mobile phase compromised of ethanol and 50-Mm ammonium acetate buffer (pH.6) at flow rate of 0.6 mL/min with 25-min runtime. The resolution and asymmetric factor were identified as critical analytical attributes (CAAs). The screening studies employing Control Noise Experimentation revealed that mobile phase pH, flow rate and ethanol concentration at 6 and 15 min significantly affected the CAAs method. The critical method parameters were optimized using Central Composition design. Chromatogram showed peak of the drugs at retention time of 9.03 min for chlorthalidone and 16.83 min for azelnidipine. The greenness score of the analytical method was found to be 1876.43 using analytical method greenness score calculator. The validation of the developed method was done which showed linearity at the range of 16-520 ng/mL, with R2 of 0.9992 and 0.9996 for azelnidipine and chlorthalidone, respectively, furthermore accuracy, precision, recovery and stability studies are carried out.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141076129","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}

引用次数: 0

Molecularly imprinted polymer for solid-phase extraction of oleanolic acid from Ligustrum lucidum fruit. 分子印迹聚合物固相萃取女贞子中齐墩果酸。

IF 1.3 4区化学

Journal of chromatographic science Pub Date : 2025-02-08 DOI: 10.1093/chromsci/bmaf010

Jianling Xu, Wenna Wang, Yixin Chen, Xiaotian Xu, Ao Duan, Yongyan Zhu, Quanhong Zhu

{"title":"Molecularly imprinted polymer for solid-phase extraction of oleanolic acid from Ligustrum lucidum fruit.","authors":"Jianling Xu, Wenna Wang, Yixin Chen, Xiaotian Xu, Ao Duan, Yongyan Zhu, Quanhong Zhu","doi":"10.1093/chromsci/bmaf010","DOIUrl":"10.1093/chromsci/bmaf010","url":null,"abstract":"A molecularly imprinted polymer (MIP) was synthesized for the selective extraction of oleanolic acid (OA), employing OA as the template molecule, acrylamide as the functional monomer, ethylene glycol dimethacrylate as the cross-linking agent, azobisisobutyronitrile as the initiator, and chloroform as the porogenic solvent. The characterization of the obtained MIPs was evaluated by scanning electron microscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller (BET) analysis and X-ray photoelectron spectroscopy. The MIPs reached adsorption equilibrium within 2 hours to OA, with high adsorption capacity of 124.68 mg/g. Subsequently, these MIPs were packed in empty solid-phase extraction (SPE) cartridge to enrichment OA from Ligustrum lucidum fruit extract. The parameters of SPE were optimized as follows: loading 0.5 ml of a 1.0 mg/ml OA reference solution, washing with 0.5 ml of toluene, and eluting with 4 ml of methanol. Under these conditions, the enrichment rate of OA from L. lucidum extract reached 76.0%. Additionally, an high-performance liquid chromatography method for determining OA content was validated. This study provides an effective approach for the separation and enrichment of OA from complex matrices and also provides practical feasibility for the separation and enrichment of other triterpenoids.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 3","pages":""},"PeriodicalIF":1.3,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143472418","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}

引用次数: 0

Characterization of Chemical Constituents and Metabolites in Rat Plasma after Oral Administration of Zhi-Zi-Hou-Po Decoction by High Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry. 采用高效液相色谱-四极杆飞行时间质谱联用技术对大鼠口服栀子后补汤后血浆中化学成分及代谢物的研究

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-02-08 DOI: 10.1093/chromsci/bmaf012

Jianyi Shi, Jiao Guan, Xu Pan, Bo Feng, Heyun Zhu

{"title":"Characterization of Chemical Constituents and Metabolites in Rat Plasma after Oral Administration of Zhi-Zi-Hou-Po Decoction by High Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry.","authors":"Jianyi Shi, Jiao Guan, Xu Pan, Bo Feng, Heyun Zhu","doi":"10.1093/chromsci/bmaf012","DOIUrl":"10.1093/chromsci/bmaf012","url":null,"abstract":"Zhi-Zi-Hou-Po decoction (ZZHPD), consisting of Gardenia jasminoides Ellis, Magnolia officinalis cortex and Citrus aurantium L., is a classic traditional Chinese medicine prescription for the treatment of depression. However, the therapeutic material foundation of ZZHPD is still not very clear. In the present study, a high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method was developed to simultaneously characterize and identify the chemical constituents and metabolites of ZZHPD in rat plasma after oral administration for the first time. As a result, a total of 88 compounds including 12 iridoid glycosides, eight lignans, 37 flavonoids, eight coumarins, seven monoterpenoids, four crocetin, three organic acids, one alkaloid and eight other compounds were identified or tentatively characterized. After intragastric administration of ZZHPD to rats, 40 compounds were detected in rat plasma, including 29 prototype constituents and 11 metabolites. Results showed that glucuronidation and sulfation were the main metabolic pathways of ZZHPD in rats. The analytical method established in this study provides an effective method for the study of the chemical composition of ZZHPD in vitro and in vivo, and provides an important basis for the study of the pharmacodynamic material basis and mechanism of action of ZZHPD.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 3","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143556803","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}

引用次数: 0

Problems in Commercial Kits of 25-Hydroxy Vitamin D and the Development of Simple, Robust and Faster HPLC Method. 25-Hydroxy Vitamin D 商用试剂盒中存在的问题以及简单、稳健、快速的 HPLC 方法的开发。

IF 1.5 4区化学

Journal of chromatographic science Pub Date : 2025-02-08 DOI: 10.1093/chromsci/bmae042

Syed Muhammad Saad, Abdul Rafiq Khan, Khalid Mohammed Khan, Ali Al-Othaim

{"title":"Problems in Commercial Kits of 25-Hydroxy Vitamin D and the Development of Simple, Robust and Faster HPLC Method.","authors":"Syed Muhammad Saad, Abdul Rafiq Khan, Khalid Mohammed Khan, Ali Al-Othaim","doi":"10.1093/chromsci/bmae042","DOIUrl":"10.1093/chromsci/bmae042","url":null,"abstract":"Vitamin D is a lipid-soluble compound that plays a key role in bone mineral metabolism. The commercial current kits and several published assay methods (High-performance liquid chromatography (HPLC) and Immunoassay) are complicated due to the use of multiple reagents, larger sample volume, high backpressure, longer extraction time, evaporation under nitrogen after extraction, significant interference and antibody cross-reactivity. Here we report a new HPLC method for the determination of 25-hydroxyvitamin D2 (25-OHD2) and 25-hydroxyvitamin D3 (25-OHD3) that is simple (no evaporation), rapid (10-minute run time) and robust. Serum sample (300 μl) is mixed with 300 μl acetonitrile containing lauraphenone as internal standard. After vortexing and centrifugation, the supernatant was loaded into C18 extraction cartridges, washed with 70% methanol and then eluted with 200 μl of a mixture of 70% ethanol and 30% isopropyl alcohol (IPA). The eluent was mixed with 50 μl of water and injected into the HPLC-UV system for analysis. The method proved to be linear in the range of 10-750 nmol/L of 25-OHD2 and 25-OHD3. The intra- and inter-assay precision was less than 10 for both compounds at four different concentrations. The method was compared with (LC-MS/MS) and the correlation coefficients (R2) were 0.9454 and 0.9673 for 25-OHD2 and 25-OHD3 respectively. The proposed HPLC method is simple, rapid, robust and free from the most common problems encountered with commercial kits. It can be used in a high-volume laboratory that uses the HPLC method for the simultaneous determination of 25-OHD2 and 25-OHD3 in serum samples.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141442784","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}

引用次数: 0