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":"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":"https://doi.org/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}
{"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":"https://doi.org/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":"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":"https://doi.org/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}
Hae-Jee Yoon, Jin Hee Kim, Myung Sook Oh, Seon-Pyo Hong, Ha-Jeong Kwon
{"title":"Simultaneous Quantification of Biogenic Amines and their Metabolites in Mice Tissue by Combining Ultraviolet and Integrated Pulsed Amperometric Detectors.","authors":"Hae-Jee Yoon, Jin Hee Kim, Myung Sook Oh, Seon-Pyo Hong, Ha-Jeong Kwon","doi":"10.1093/chromsci/bmaf004","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf004","url":null,"abstract":"<p><p>We developed a reversed-phased high-performance liquid chromatographic method combining ultraviolet detection and integrated pulsed amperometric detection for the simultaneous quantification of dopamine, 5-hydroxyindolacetic acid, homovanillic acid, serotonin, 3,4-dihydroxyphenylacetic acid, norepinephrine and epinephrine. All target components were completely separated in a C18 column with isocratic elution of 5% acetonitrile solution containing 8 mM HClO4 and 0.20 mM 1-octanesulfonic acid as an ion pairing reagent. This method showed limits of detection of 0.03-0.1 ng and limits of quantification of 0.10-0.3 ng with linear regression coefficients of 0.9998-1.0000. All inter-day and intra-day precision values were below 9.58%, and the average recoveries were 93.71-109.82% for mouse striatum samples. The mean levels of the seven components in striatal brain tissue in a mouse model of Parkinson's disease decreased by 2-12 times compared to those of a control group. In particular, the decrease in dopamine, 5-hydroxyindolacetic acid and 3,4-dihydroxyphenylacetic acid was statistically significant (P < 0.05). Orthogonal partial least squares discriminant analysis confirmed that the seven components are useful biomarkers. The significance of the developed method lies in its ability to simultaneously analyze seven biogenic amines related to Parkinson's disease by combining two detectors, offering a simple and cost-effective approach for clinical and biological labs.</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":"143006235","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":"Optimization of Extraction of Four Components from Radix Scrophulariae with Natural Deep Eutectic Solvents and Evaluation of Extract's Antioxidant Activity.","authors":"Ping Huang, Yanxia Zhou, Fei Ruan, Jianyu Sun, Jinglin Shen, Hongmei Chen","doi":"10.1093/chromsci/bmae037","DOIUrl":"10.1093/chromsci/bmae037","url":null,"abstract":"<p><p>In this research, eight natural deep eutectic solvents (NaDESs) consisting of food-grade ingredients were screened for the extraction of four bioactive compounds (acteoside, cinnamic acid, angoroside C and harpagoside) from radix scrophulariae (RS). Among these NaDESs, Proline-Glycerol NaDES with higher comprehensive score was selected. The Criteria Importance Through Intercriteria Correlation (CRITIC) was applied to calculate the information entropy and the weight of indexes, and figured out a comprehensive score. The weights of acteoside, cinnamic acid, angoroside C and harpagoside were 0.369, 0.172, 0.241 and 0.218, respectively. Response surface methodology (RSM) mathematical model was used to optimize the extraction parameters. The optimal extraction parameters were as follows: extraction time with 42.21 min, NaDES concentration with 52.89%, solid-to-liquid ratio with 1 : 37.05 g/mL and the predicted value of comprehensive score was 0.885. Under the optimal condition, the comprehensive score was 0.903 ± 0.005. Finally, the antioxidant activity experiment revealed that the 1,1-Diphenyl-2-picrylhydrazyl · radical scavenging activity and hydroxyl radical scavenging activity of the extract at 2.0 mg/mL and 1.5 mg/mL were approximately equal to those of ascorbic acid, respectively. The results showed that the extraction condition optimized by RSM combined with CRITIC was reasonable and dependable, and the extract of radix scrophulariae exhibited good antioxidant activity.</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":"141293455","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}
Ashok H Akabari, Harsh Gajiwala, Sagarkumar K Patel, Jasmina Surati, Divya Solanki, Ketan V Shah, Tejas J Patel, Sagar P Patel
{"title":"Stability-Indicating TLC-Densitometric and HPLC Methods for Simultaneous Determination of Teneligliptin and Pioglitazone in Pharmaceutical Dosage Forms with Eco-Friendly Assessment.","authors":"Ashok H Akabari, Harsh Gajiwala, Sagarkumar K Patel, Jasmina Surati, Divya Solanki, Ketan V Shah, Tejas J Patel, Sagar P Patel","doi":"10.1093/chromsci/bmae038","DOIUrl":"10.1093/chromsci/bmae038","url":null,"abstract":"<p><p>The combination of teneligliptin hydrobromide hydrate and pioglitazone hydrochloride in pharmaceutical formulations has improved type 2 diabetes management. Two chromatographic methods TLC-densitometry and RP-HPLC were developed for simultaneous quantification of teneligliptin hydrobromide hydrate and pioglitazone hydrochloride in pharmaceutical formulations, ensuring accuracy and stability assessment. The TLC method uses a mobile phase of methanol, toluene, ethyl acetate and triethylamine (1:7:2:0.1, v/v/v/v) on TLC silica gel plates, scanned at 268 nm. The RP-HPLC method employs isocratic elution with acetonitrile and sodium acetate buffer (adjust pH 3.6 with glacial acetic acid, 60:40 v/v) on a shimpack C18 column (250 × 4.6 mm i.d., 5 μm), detected at 235 nm. Both methods offer high accuracy and reliability, making them valuable for pharmaceutical quality control. Additionally, an environmental impact assessment was conducted using eco-scale, Analytical Greenness Metric Approach, Green Analytical Procedure Index, and national environmental method index to evaluate solvent consumption, waste generation and energy usage. Statistical comparisons (t-tests and F-tests) validate the outcomes of both methods, ensuring their effectiveness in drug formulation analysis. These methods can enhance pharmaceutical quality control while fulfilling environmental responsibilities.</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":"141247813","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}
Azra Takhvar, Somaye Akbari, Effat Souri, Reza Ahmadkhaniha, Ali Morsali, Mohammad Reza Khoshayand, Mohsen Amini, Alireza Taheri
{"title":"Metal-Organic Frameworks MIL-101(Fe) and MIL-53(Al) as Efficient Adsorbents for Dispersive Micro-Solid-Phase Extraction of Sorafenib in Plasma and Wastewater, Coupled with HPLC-UV Analysis.","authors":"Azra Takhvar, Somaye Akbari, Effat Souri, Reza Ahmadkhaniha, Ali Morsali, Mohammad Reza Khoshayand, Mohsen Amini, Alireza Taheri","doi":"10.1093/chromsci/bmaf003","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf003","url":null,"abstract":"<p><p>In the present study, metal-organic frameworks, MIL-101(Fe) and MIL-53(Al), were synthesized under solvothermal conditions and were characterized by Fourier transform infrared spectroscopy, X-ray energy diffraction spectroscopy and scanning electron microscopy. The synthesized metal-organic frameworks were utilized for the purpose of dispersive micro-solid phase extraction of sorafenib in both human plasma and wastewater, which was subsequently followed by high performance liquid chromatography with ultraviolet determination. Parameters affecting extraction efficacy including adsorbent amount, ionic strength, pH, type of elution solvent, adsorption and desorption time were optimized. Under optimal experimental conditions, the linearity in human plasma and wastewater was achieved in the range of 0.25-5.00 and 0.01-0.20 μg/mL, respectively. The extraction recovery for MIL-101(Fe) and MIL-53(Al), respectively, was calculated in human plasma and wastewater and found to be in the range of 86.27-99.47%.</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":"143006146","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}
Marwa A Wahab Mubarak, M Abdul-Azim Mohammad, Ramzia I El-Bagary, Ehab Elkady, Nisreen F Abo-Talib
{"title":"A Simple Validated LC-UV Method for the Simultaneous Determination of Brimonidine and Brinzolamide in the Presence of Brinzolamide's Degradation Product (Major Metabolite) in Rabbit Aqueous Humor.","authors":"Marwa A Wahab Mubarak, M Abdul-Azim Mohammad, Ramzia I El-Bagary, Ehab Elkady, Nisreen F Abo-Talib","doi":"10.1093/chromsci/bmae040","DOIUrl":"10.1093/chromsci/bmae040","url":null,"abstract":"<p><p>A sensitive, specific, reliable and low-cost LC-UV method has been developed and validated for simultaneous quantification of brimonidine tartrate (BM) and brinzolamide (BZ) in rabbit aqueous humor (AH) in the presence of N-desethyl-brinzolamide (NDBZ); BZ is a major degradation product, and it is also considered to be its major metabolite. Dorzolamide hydrochloride (DZ) was used as an internal standard (IS). The analytes were extracted from rabbit AH samples by a simple pre-treatment utilizing ZnSO4.7H2O as a deproteinizing agent. The analytes were separated on a cyanopropyl Waters column (4.6 × 200 mm, 5 μm) with an isocratic mobile phase consisting of 25 mM ammonium acetate pH 4.5 (adjusted with 85% phosphoric acid):methanol:acetonitrile (94:4.5:1.5, v/v) at a flow rate of 1.0 mL min-1. The detection was done at 254 nm. The lower limit of quantification in rabbit AH was 100.0 ng mL-1. The method was validated according to EMA guidelines. The method was confirmed to be accurate, precise and linear over a range of 100.0-1000.0 ng mL-1 for BM and BZ. The method developed herein is simple, safe, eco-friendly, rapid and accurately applied for the quantification of BM and BZ, along with the successful separation of NDBZ, which is considered as a potential irritant degradation product of BZ.</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":"141306046","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":"Correction to: 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":"","doi":"10.1093/chromsci/bmae043","DOIUrl":"10.1093/chromsci/bmae043","url":null,"abstract":"","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":"141317457","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}