{"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":"<p><p>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.</p>","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}
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":"<p><p>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.</p>","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}
{"title":"Development of Simultaneous HPTLC Method and Validation for the Quality Assessment of Ayurvedic Formulation-Ayush Kvatha Churna by Using Marker Compound Rosmarinic Acid, Trans-Cinnamaldehyde and Piperine.","authors":"Umakant Sahu, Nagendra Singh Chauhan, Arun Kumar Singh Parihar, Kamleshwar Singh Karbhal, Shrikant R Inchulkar, Prashant Kumar Gupta, Rajesh Kumar Singh","doi":"10.1093/chromsci/bmae019","DOIUrl":"10.1093/chromsci/bmae019","url":null,"abstract":"<p><p>Ayurveda emphasizes the propagation of nature in maintaining health. In the present scenario, we have seen the faith of people in herbal drugs during the Covid 19 outbreak. The raises in the number of peoples have been using herbal drugs to boost immunity against infectious diseases shows the popularity of this ancient system of medicine. The standardization of Ayush Kvatha Churna (AKC), work set out to establish a straightforward, accurate and sensitive HPTLC method for the identification and quantification of marker compounds. The Rosmarinic acid, trans-Cinnamaldehyde and Piperine were used for the estimation of markers in Ayush Kvatha Churna by using HPTLC with a solvent system, consisting of Toluene: Ethyl acetate: Ethyl alcohol: Formic acid (5.6:2.4:2: 0.3 v/v/v/v). The Rf value 0.33 for Rosmarinic Acid, 0.69 for Piperine and 0.77 for trans-Cinnamaldehyde was observed and it is exactly complying with the corresponding bands in Ayush Kvatha Churna. The technique has been effectively verified and validated, enabling it to be used for the standardization or quantitative analysis of Rosmarinic acid, trans-Cinnamaldehyde and piperine in Ayush Kvatha Churna.</p>","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":"140849768","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}
{"title":"A Validated High-Performance Thin-Layer Chromatography Technique for Routine Analysis of Curcumin in Four Different Species of Curcuma Viz. C. amada, C. caesia, C. longa and C. zedoaria.","authors":"Avinash Gangal, Manisha Duseja, Neeraj K Sethiya, Dheeraj Bisht, Sushil Kumar Chaudhary, Vijay Singh Rana","doi":"10.1093/chromsci/bmad063","DOIUrl":"10.1093/chromsci/bmad063","url":null,"abstract":"<p><p>In this study, we investigated a new, simple, sensitive, selective and precise high-performance thin-layer chromatography (HPTLC) fingerprint and quantitative estimation method for the routine analysis of curcumin in Curcuma species viz. Curcuma amada, Curcuma caesia, Curcuma longa and Curcuma zedoaria. Linear ascending development was carried out in a twin-trough glass chamber saturated with toluene:acetic acid (4:1; v/v with 20 minutes of saturation). The plate was dried and analyzed by CAMAG TLC scanner III at white light and 366 nm. The system was found to give compact spots for curcumin (Rf 0.42). The relationship between the concentration of standard solutions and the peak response is linear within the concentration range of 10-70 ng/spot for curcumin. In result, curcumin was not detected in any of C. caesia extracts. The percentage of curcumin was found between 0.042 and 4.908 (%w/w) in different Curcuma species obtained by two different extraction methods viz. Soxhlet and sonication, respectively. Further, extraction via Soxhlet method is most suitable method to get higher curcumin content from rhizomes. The proposed HPTLC method may be use for routine quality testing and quantification of curcumin in Curcuma samples.</p>","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":"10022099","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}
{"title":"First Detection of Food-Derived Agricultural Chemicals Residues in Waste Wool Fibers by Ultrasound-Assisted Extraction-QuEChERS Cleanup-UPLC-MS/MS.","authors":"Yingao Li, Jun Liu, Shuai Li, Huidan Deng, Hui Zhao, Lili Meng, Lixia Jia","doi":"10.1093/chromsci/bmae033","DOIUrl":"10.1093/chromsci/bmae033","url":null,"abstract":"<p><p>Food-derived agricultural chemical residues (FACRs) accumulate gradually in organisms and can damage their nervous system, endocrine system and reproductive system, posing significant harm. Currently, there is little literature on the detection of FACRs in waste wool fibers. In this paper, an ultrasound-assisted extraction-QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) cleanup-UPLC-Ms/Ms method was applied for the qualitative analysis and quantitative determination of trace FACRs in waste wool fibers with 0.2% formic acid-methanol as extraction solvent and multi-selective ion scanning. Using the external standard method, it was shown that the 13 target FACRs showed good linearity in the mass concentration range of 0.1-50 μg/kg. The limits of detection were 1.0- 10.0 μg/kg and the limits of quantification were 4.0-40.0 μg/kg. The recoveries of the 13 target FACRs ranged from 78 to 112.6% at the 5-, 10- and 20-fold detection limit spiked levels, and the intra- or inter-day relative standard deviations were 2.05-6.98% or 1.98-6.99%, respectively. This method satisfied the detection requirements and can be used in applications.</p>","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":"141173944","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}
{"title":"Analytical Methods for Estimating Metformin Hydrochloride, Pioglitazone and Teneligliptin in Diabetes Management: a Comprehensive Review.","authors":"Sejal Pandya, Hitesh J Vekaria","doi":"10.1093/chromsci/bmaf013","DOIUrl":"10.1093/chromsci/bmaf013","url":null,"abstract":"<p><p>Diabetes mellitus remains a global health challenge, with a growing need for effective therapies. Metformin, Pioglitazone and Teneligliptin are widely prescribed medications for diabetes management. Accurate and precise estimation of these drugs is essential to ensure optimal therapeutic efficacy while minimizing side effects. This comprehensive review examines a multitude of analytical methods employed for the quantification of Metformin, Pioglitazone and Teneligliptin individually as well as in combine pharmaceutical dosage form focusing on their strengths, limitations and applicability within the realm of diabetes treatment. The choice of analytical method depends on various factors, such as the specific formulation, sample matrix complexity and the required sensitivity and quantification range. This review encompasses a wide range of analytical techniques, including spectroscopic methods (ultraviolet-visible, Fourier transform infrared and nuclear magnetic resonance spectroscopy), chromatographic methods (high-performance liquid chromatography, ultra-high performance liquid chromatography, and gas chromatography, high-performance thin-layer chromatography, liquid chromatography-tandem mass spectrometry), electrochemical approaches and emerging technologies like mass spectrometry and biosensors. Additionally, it delves into the intricacies of method development and validation, sample preparation and the importance of stability-indicating methods. Recent advancements in sample extraction and preparation techniques are explored to enhance sensitivity and accuracy. By offering a comprehensive assessment of the analytical methods used for the estimation of Metformin, Pioglitazone and Teneligliptin for diabetes treatment, this review serves as a valuable resource for researchers, clinicians and pharmaceutical scientists. It aids in selecting the most suitable analytical method for specific applications, contributing to the continuous improvement of diabetes management and treatment.</p>","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":"143556798","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}
{"title":"Synthesis and Characterization of MIP Ghost Approach for Selective Extraction of Empagliflozin and Quantification by Liquid Chromatography.","authors":"Durga Panikumar Anumolu, Jampana Ramatulasi, Gorja Ashok, Syed Sara Afreen, Ceema Mathew, Pulusu Veera Shakar","doi":"10.1093/chromsci/bmaf008","DOIUrl":"10.1093/chromsci/bmaf008","url":null,"abstract":"<p><p>The valid method was developed for analyzing empagliflozin in serum/plasma/urine using a molecularly imprinted ghost polymer-solid-phase extraction approach (MISPE) with liquid chromatographic methodology. Methacrylic acid (MAA) was used as the monomer, 2,2 azobis isobutyronitrile as the initiator and ethylene glycol dimethacrylate as the cross-linker in the free radical polymerization procedure. Empagliflozin was loaded onto the polymer and eluted with 1 mL of a 9:1 MeOH:acetic acid solution. The PRONTOSIL C8 (250 × 4 mm × 5u) was used to design the optimized HPLC technique. Phosphate buffer (pH -5): ACN (40:60) was used as the mobile phase with a flow rate of 0.8 mL/min, and 230 nm was used for detection. Empagliflozin's calibration curve is linear between 0.08 and 200 μg/mL. The thresholds for quantification (limit of quantification) and detection (limit of detection) were 0.002 and 0.006 μg/mL, respectively. High binding affinity and selectivity were displayed by the polymer, and, at pH 8, the polymer's rebinding efficiency was effective. It was discovered that the extraction recovery of the analyte employing the molecular-imprinted solid-phase extraction coupled with high-performance liquid chromatography developed technique was 93% with relative standard deviation (RSD) <2%.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143052573","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}
{"title":"New Insights into the Quality Control Strategies of Inula racemosa Hook. F. (Pushkarmula) and Saussurea lappa Decne. (Kuth): Medicinal Crops of Alpine Himalaya.","authors":"Manish Kumar, Rishabh Bhardwaj, Anil Kumar, Dinesh Kumar","doi":"10.1093/chromsci/bmaf009","DOIUrl":"10.1093/chromsci/bmaf009","url":null,"abstract":"<p><p>Adulteration and illegal trade of Saussurea lappa in the name of Inula racemosa is a major issue. Therefore, accurate and easy methods are required to control malpractice and define authenticity. The current study is focused on authenticating and defining quality control methods for I. racemosa and S. lappa. Reference and market samples of S. lappa and I. racemosa were used to develop methods, including high-performance thin layer chromatography (HPTLC), Gas chromatography-mass spectrometry (GC-MS) and (Ultra Performance Liquid Chromatography-Photo Diode Array (UPLC-PDA). Multivariate analysis was used to define variations among samples. Costunolide, dehydrocostus lactone, isoalantolactone and alantolactone were used to develop and validate the quality control method. Phytochemical investigations and filter paper reagent tests clearly differentiate between Saussurea and Inula. HPTLC and GC-MS fingerprints were found significant to certify both species. From a quality control perspective, the UPLC-PDA method was found significant for the separation of targeted molecules. Altantolactones were found higher in I. racemosa while costunolides in S. lappa, whereas market samples closely resembled with Inula species and confirmed as I. racemosa. The current findings suggested that filter paper tests could be useful for farmers, traders and industries to check the authenticity of S. lappa and I. racemosa. Chemical fingerprints and UPLC-PDA method were found sufficient to define quality of both the species.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143032374","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}
Shu-Tong Yang, Yi-Wen Cao, Zi-Ying Zeng, Zheng Gang, Min Chen, Bing-Yan Du, Miao-Miao Su, Zhong-Hua Yang, Zhu-Hua Tang, Yun-Liu Zeng
{"title":"Determination of Azole Fungicide Residues in Fresh Juice by Magnetic Solid Phase Extraction Based on Fe3O4@ZnAl-LDH@MIL-53(Al) Sorbent in Combination with High-Performance Liquid Chromatograph.","authors":"Shu-Tong Yang, Yi-Wen Cao, Zi-Ying Zeng, Zheng Gang, Min Chen, Bing-Yan Du, Miao-Miao Su, Zhong-Hua Yang, Zhu-Hua Tang, Yun-Liu Zeng","doi":"10.1093/chromsci/bmae029","DOIUrl":"10.1093/chromsci/bmae029","url":null,"abstract":"<p><p>In this work, a magnetic adsorption material based on metal-organic framework (Fe3O4@ZnAl-LDH@MIL-53(Al)) was synthesized and used as an adsorbent in the process of magnetic solid phase extraction. Then, a high-performance liquid chromatograph was used to quantitatively detect triazole fungicides in samples. In order to verify the successful preparation of the material, a series of characterization analyses were carried out. Besides, the key parameters that may affect the extraction efficiency have been optimized, and under optimal conditions the three triazole fungicides showed good linearity in the range of 10-1000 μg/L (R2 ≥ 0.9796); Limit of detections were ranged from 0.013 to 0.030 μg/mL. Finally, the established method was applied to the detection of triazole fungicides in four fresh juice samples. The results showed that the target analyte was not detected in all the test samples. By detecting the recoveries (73.3-104.3%) and coefficient variation (RSD ≤ 6.8%) of triazole fungicides in fortified samples, it proved that this established method meets the requirements of pesticide residue analysis and showed excellent application potential.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140957570","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}
{"title":"Quality by Design-Steered Chromatographic Separation and Identification of the Geometric Isomers of Capsiate by Reversed-Phase HPLC and LC-MS.","authors":"Reena Gupta, Bhupinder Kapoor, Monica Gulati, Sumant Saini, Pooja Rani, Atanas G Atanasov, Stefano Dall'Acqua, Qushmua Alzahrani, Deepak Kapoor, Jesus Simal-Gandara","doi":"10.1093/chromsci/bmaf001","DOIUrl":"10.1093/chromsci/bmaf001","url":null,"abstract":"<p><p>An efficient reverse-phase high-performance liquid chromatographic method, based on the design of the experiment approach, was developed for the simultaneous determination of capsiate isomers. Critical method parameters, i.e., flow rate and mobile phase composition, demarcated during preliminary screening were optimized using central composite design. Chromatographic separation was achieved on a Nucleodur C18 column (250 × 4.6 mm, 5 μm), with the mobile phase consisting of water-acetonitrile (40:60), both acidified with 0.1% v/v formic acid, passed at a flow rate of 1 mL/min. E- and Z-capsiates were eluted from the column at the retention times of 18.56 ± 0.09 and 17.30 ± 0.08 min, respectively, with a resolution factor of 1.693 ± 0.046. The method was found to be linear within the concentration range of 1.054-5.270 and 8.623-43.115 μg/mL for Z- and E-isomers, respectively, with an R2 of >0.99. Recovery of the individual values was in range of 96.15-101.92%, with a relative standard deviation of <2%. The developed method was used to quantify capsiate isomers extracted from sweet pepper fruits. Therefore, the proposed method is presented for optimum isomeric resolution of these closely related E- and Z-isomers with convenient sample preparation, acceptable run-time, cost effectiveness and use of conventional instruments.</p><p><strong>Highlights: </strong></p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 2","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-01-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143006218","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}