{"title":"Nanoparticle Assisted Fabric Phase Sorptive Extraction for Azo Dye Determination in the Industrial Sewage.","authors":"Nayereh Rahimian, Javad Feizy, Zarrin Es'haghi","doi":"10.1093/chromsci/bmae046","DOIUrl":"https://doi.org/10.1093/chromsci/bmae046","url":null,"abstract":"<p><p>Currently, one of the significant environmental problems is the presence of azo dye materials in water sources. In this study, for the first time, a fast and sensitive sample preparation approach using nanoparticle-assisted fabric phase sorptive extraction (NFPSE) followed by high-performance liquid chromatography was examined to remove some azo dyes such as methyl red and sunset yellow from aqueous solutions. Primarily, the significance of several parameters affecting NFPSE, such as fabric type, the kind of sorbent, the number of contacts with sol-gel and the time of contact, was investigated. In addition, experiments were performed to determine the effect of different adsorption parameters, such as sample volume, adsorption time, adsorbent value, desorption time, ionic strength and pH. It was found that the calibration curve was linear within two ranges of concentrations (0.05-0.1 and 0.5-15 ng/L for methyl red; 0.05-0.5 and 0.5-15 ng/L for sunset yellow) with correlation coefficients better than 0.9683. The limit of detection was 0.014 ng/L for methyl red and 0.015 ng/L for sunset yellow. Repeatability Relative Standard Deviation (RSD) with three replicated experiments was 1.5-10% for methyl red and 2.5-5.8% for sunset yellow. Relative recovery percentages of 88-96% for methyl red and 62-92% for sunset yellow were obtained in the samples. Moreover, the results have shown that acceptable accuracy, precision and linearity make the \"fabric phase sorptive extraction\" a proper method for the determination of dyes from industrial sewage samples.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141893545","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":"Chemical Profiling of Shen-Wu-Yi-Shen Tablets Using UPLC-Q-TOF-MS/MS and Its Quality Evaluation Based on UPLC-DAD Combined with Multivariate Statistical Analysis.","authors":"Yudan Mei, Yumei Hu, Xiaoqian Tao, Jing Shang, Mengyu Qian, Fengtai Suo, Jifeng Li, Liang Cao, Zhenzhong Wang, Wei Xiao","doi":"10.1093/chromsci/bmae001","DOIUrl":"10.1093/chromsci/bmae001","url":null,"abstract":"<p><p>Shen-Wu-Yi-Shen tablets (SWYST) is a traditional Chinese medicine prescription used for treating chronic kidney disease (CKD). This study aims to characterize the constituents in SWYST and evaluate the quality based on the quantification of multiple bioactive components. SWYST samples were analyzed with ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and a data-processing strategy. As a result, 215 compounds in SWYST were unambiguously identified or tentatively characterized, including 14 potential new compounds. Meanwhile, strategies based on characteristic fragments for rapid identification were summarized, indicating that the qualitative method is accurate and feasible. Notably, the glucose esters of laccaic acid D-type anthraquinone were first found and their fragmentation patterns were described by comparing that of O-glycoside isomers. Besides, based on comparisons of the cleavage ways of mono-acyl glucose with different acyl groups or acylation sites, differences in fragmentation pathways between 1,2-di-O-acyl glucose and 1,6-di-O-acyl glucose were proposed for the first time and verified by reference substances. In addition, a validated UPLC-DAD was established for the determination of 11 major bioactive components related to treatment of CKD (albiflorin, paeoniflorin, 2,3,5,4'-tetrahydroxy-stilbene-2-O-β-d-glucoside (TSG), 1-O-galloyl-2-O-cinnamoyl-β-d-glucose, emodin-8-O-β-d-glucoside, chrysophanol-O-β-d-glucoside, aloe-emodin, rhein, emodin, chrysophanol and physcion). Moreover, TSG and 1-O-galloyl-2-O-cinnamoyl-β-d-glucose were found as the quality markers related to the origins of SWYST based on multivariate statistical analysis. Conclusively, the findings in this work provide a feasible reference for further studies on quality research and mechanisms of action in treating CKD.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139512453","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: Isolation of Methoxyfuranocoumarins From Ammi majus by Centrifugal Partition Chromatography.","authors":"","doi":"10.1093/chromsci/bmae045","DOIUrl":"https://doi.org/10.1093/chromsci/bmae045","url":null,"abstract":"","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141468376","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}
Mi Jin Kim, Hwan Seong Choi, Hyunil Shin, Ji Hyun Lee, Nam Sook Kim, Hyungil Kim
{"title":"Simultaneous Detection Method of 11 Respiratory Drug Substances Including Theobromine, Oxymetazoline, etc. in Adulterated Dietary Supplements Using Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry and Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry Analysis.","authors":"Mi Jin Kim, Hwan Seong Choi, Hyunil Shin, Ji Hyun Lee, Nam Sook Kim, Hyungil Kim","doi":"10.1093/chromsci/bmae044","DOIUrl":"https://doi.org/10.1093/chromsci/bmae044","url":null,"abstract":"<p><p>Recently, the demand for respiratory disease-related products has surged due to the influence of coronavirus disease 2019, prompting warnings about illegal dietary supplements containing unauthorized substances. Additionally, adulterated dietary supplements are continuously detected in open markets, posing significant public health safety problem. In this study, we developed and validated an analytical method for 11 respiratory drug substances using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) and proposed optimal conditions for LC-quadrupole time-of-flight MS (LC-QTOF-MS) to determine the fragmentation patterns of each substance. This method underwent thorough validation considering specificity, linearity, limits of detection and quantification, accuracy, precision, matrix effect, stability, etc. All results met international guidelines. These validated methods were applied to 52 dietary supplements advertised for treating respiratory diseases and enhancing respiratory function, among which one sample was found to contain 313.7 mg/g of theobromine. This determination was made by comparing the product ion ratios with the standards and subsequent quantification. To re-confirm the detected substances, their fragmentation patterns were compared with those of the standards using LC-QTOF-MS. In conclusion, the mass-based information, coupled with the LC-ESI-MS/MS method development, can be successfully applied to rapidly identify 11 respiratory drug substances in illegal dietary supplements used for respiratory disease treatment. The developed simultaneous detection method contributes to public health and safety improvements.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-06-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141468377","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":"https://doi.org/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":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-06-23","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":"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":"https://doi.org/10.1093/chromsci/bmae043","url":null,"abstract":"","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-06-14","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}
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":"https://doi.org/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":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-06-12","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":"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":"https://doi.org/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":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-06-08","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":"https://doi.org/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":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-06-05","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}
Zixu Wang, Yue Liu, Guoqing Sun, Liu Yang, Shuai Huang, Lin Chen, Xianli Zhou
{"title":"A Simple and Rapid High-Performance Liquid Chromatography Method for Preparation and Content Detection of the Mainly Numbing Taste Substances of Zanthoxylum bungeanum Maxim.","authors":"Zixu Wang, Yue Liu, Guoqing Sun, Liu Yang, Shuai Huang, Lin Chen, Xianli Zhou","doi":"10.1093/chromsci/bmad087","DOIUrl":"10.1093/chromsci/bmad087","url":null,"abstract":"<p><p>As the characteristic numbing taste substances, hydroxyl-α-sanshool (HAS) and hydroxyl-β-sanshool (HBS) were considered vital indicators to evaluate the quality of Zanthoxylum bungeanum Maxim. However, it is very difficult to obtain their high-purity monomers individually, as the only difference between HAS and HBS is that C-6 cis-trans isomerism. In our study, a simple and rapid Ag +-HPLC method was developed to pure the standard chemicals of Z. bungeanum with numbing taste, and 1H NMR and 13C NMR were employed to determine the purity and structure. Moreover, an HPLC method was established to determine the content of numbing taste components of 16 varieties of Z. bungeanum from different regions. The analytical methods were validated for accuracy, precision, and linearity, respectively. The validated method was accurate (spiked recoveries 0.94-1.10), precise in terms of peak area (intra-day RSDs <1.25% and inter-day RSDs <1.61%), and linear (r2 ≥ 0.999). It was found that there were significant differences in the content of HAS and HBS among different types of Z. bungeanum, with HAS content ranging from 60.06 ± 1.14 to 164.13 ± 3.28 mg/g and HBS ranging from 7.81 ± 0.36 to 21.11 ± 0.75 mg/g. The RSDs of HAS range were 1.73-3.80% and that of HBS range 2.03-4.73% (RSDs ≤5%), which indicated that the measurements of HAS and HBS were reliable.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-05-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136397610","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}