Yuyu Yang, Shihan Liu, Wenfang Jin, Zengyi Qu, Baolei Fan
To isolate gastrodin (GAS), 4-hydroxybenzyl alcohol (4-HBA), and phenolic compounds from Chinese medicine Gastrodia elata Blume, and to explore the binding mode of fatty acid binding protein 4 (FABP4/aP2) that is closely related to macrophage inflammation, we study their anti-inflammatory targets. After the ultrasonic extraction of the main active components with 70% ethanol, three resins and three eluents were selected, and eight phenolic monomers with similar structures, such as gastrodin and 4-hydroxybenzyl alcohol, were isolated from Gastrodia elata by AB-8 macroporous resin and silica gel column chromatography and eluted with the CHCl3-MeOH gradient. Their structures were identified by HPLC and nuclear magnetic resonance (NMR). The FABP4 protein was added to GAS and 4-HBA, and the NMR experiment was performed to observe ligand binding. Finally, according to the spectral information of STD-NMR and molecular docking technology, the interaction between ligands and protein was studied. The fluorescence competition experiment confirmed that both GAS and 4-HBA were in the binding cavity of FABP4. Moreover, 3-phenoxy-2-phenylbenzoic acid (PPA) is a possible inhibitor of FABP4, reducing macrophage-related inflammation and endoplasmic reticulum stress. This work provides a new basis for the anti-inflammatory mechanism of Gastrodia elata, paving the way for the research and development of FABP4 inhibitor drugs.
{"title":"The Molecular Mechanism of FABP4 Inhibition Effects of GAS and 4-HBA in Gastrodia elata Blume Was Discussed Based on NMR and Molecular Docking","authors":"Yuyu Yang, Shihan Liu, Wenfang Jin, Zengyi Qu, Baolei Fan","doi":"10.1155/2024/6599029","DOIUrl":"https://doi.org/10.1155/2024/6599029","url":null,"abstract":"To isolate gastrodin (GAS), 4-hydroxybenzyl alcohol (4-HBA), and phenolic compounds from Chinese medicine <i>Gastrodia elata</i> Blume, and to explore the binding mode of fatty acid binding protein 4 (FABP4/aP2) that is closely related to macrophage inflammation, we study their anti-inflammatory targets. After the ultrasonic extraction of the main active components with 70% ethanol, three resins and three eluents were selected, and eight phenolic monomers with similar structures, such as gastrodin and 4-hydroxybenzyl alcohol, were isolated from <i>Gastrodia elata</i> by AB-8 macroporous resin and silica gel column chromatography and eluted with the CHCl<sub>3</sub>-MeOH gradient. Their structures were identified by HPLC and nuclear magnetic resonance (NMR). The FABP4 protein was added to GAS and 4-HBA, and the NMR experiment was performed to observe ligand binding. Finally, according to the spectral information of STD-NMR and molecular docking technology, the interaction between ligands and protein was studied. The fluorescence competition experiment confirmed that both GAS and 4-HBA were in the binding cavity of FABP4. Moreover, 3-phenoxy-2-phenylbenzoic acid (PPA) is a possible inhibitor of FABP4, reducing macrophage-related inflammation and endoplasmic reticulum stress. This work provides a new basis for the anti-inflammatory mechanism of <i>Gastrodia elata</i>, paving the way for the research and development of FABP4 inhibitor drugs.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"10 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140940449","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Fan Chen, Shunjun Ma, Runrun Wang, Dizhong Chen, Congcong Wen, Xianqin Wang, Tao Hu, Xiuwei Shen
SIPI6398 is a novel anti-schizophrenia agent with a new mechanism of action and demonstrates better target selectivity and safety compared to its competitors. However, few in vivo studies on the pharmacokinetics and bioavailability of SIPI6398 have been performed. A rapid and simple ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) approach was developed for accurate quantification of SIPI6398 in rat plasma. A simple protein precipitation of acetonitrile-methanol (9 : 1, v/v) was used to treat plasma. Chromatography was performed on a UPLC HSS T3 column (50 mm × 2.1 mm, 1.8 μm) at a flow rate of 0.4 ml/min. The mobile phase consisted of acetonitrile-water (with 0.1% formic acid) and gradient elution was used, and the elution time was 4 minutes. Quantitative analysis was performed using electrospray ionization (ESI) in positive ion detection mode with multiple reaction monitoring (MRM) mode. To evaluate the pharmacokinetics and bioavailability, SIPI6398 was administered to rats in two different ways: oral (4 mg/kg) and intravenous (2 mg/kg) administration. The calibration curve for the UPLC-MS/MS approach shows excellent linearity in the range of 1–2000 ng/mL with an r value above 0.99. The precision, accuracy, recovery, matrix effect, and stability results all meet the criteria established for biological analytical methods. The UPLC-MS/MS method was successfully applied it to pharmacokinetics study of SIPI6398. The bioavailability of SIPI6398 was calculated to be 13.2%. These studies have the potential to contribute towards a more comprehensive comprehension of the pharmacokinetics and bioavailability of SIPI6398.
{"title":"Advanced UPLC-MS/MS Method for the Quantification of SIPI6398 in Rat Plasma and Its Pharmacokinetic Characterization","authors":"Fan Chen, Shunjun Ma, Runrun Wang, Dizhong Chen, Congcong Wen, Xianqin Wang, Tao Hu, Xiuwei Shen","doi":"10.1155/2024/9811466","DOIUrl":"https://doi.org/10.1155/2024/9811466","url":null,"abstract":"SIPI6398 is a novel anti-schizophrenia agent with a new mechanism of action and demonstrates better target selectivity and safety compared to its competitors. However, few in vivo studies on the pharmacokinetics and bioavailability of SIPI6398 have been performed. A rapid and simple ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) approach was developed for accurate quantification of SIPI6398 in rat plasma. A simple protein precipitation of acetonitrile-methanol (9 : 1, v/v) was used to treat plasma. Chromatography was performed on a UPLC HSS T3 column (50 mm × 2.1 mm, 1.8 <i>μ</i>m) at a flow rate of 0.4 ml/min. The mobile phase consisted of acetonitrile-water (with 0.1% formic acid) and gradient elution was used, and the elution time was 4 minutes. Quantitative analysis was performed using electrospray ionization (ESI) in positive ion detection mode with multiple reaction monitoring (MRM) mode. To evaluate the pharmacokinetics and bioavailability, SIPI6398 was administered to rats in two different ways: oral (4 mg/kg) and intravenous (2 mg/kg) administration. The calibration curve for the UPLC-MS/MS approach shows excellent linearity in the range of 1–2000 ng/mL with an <i>r</i> value above 0.99. The precision, accuracy, recovery, matrix effect, and stability results all meet the criteria established for biological analytical methods. The UPLC-MS/MS method was successfully applied it to pharmacokinetics study of SIPI6398. The bioavailability of SIPI6398 was calculated to be 13.2%. These studies have the potential to contribute towards a more comprehensive comprehension of the pharmacokinetics and bioavailability of SIPI6398.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"21 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140883433","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Li Li, Jing Wen, Yuyang Deng, Juan Yang, Yue Yuan, Yi Shen, Guoce Liu, Yonghong Tian, Dean Lei
The accurate determination of the free nicotine content in cigarette smoke is crucial for assessing cigarette quality, studying harm and addiction, and reducing tar levels. Currently, the determination of free nicotine in tobacco products primarily relies on methods such as pH calculation, nuclear magnetic resonance (NMR) spectroscopy, headspace solid-phase microextraction (HS-SPME), and traditional solvent extraction. However, these methods have limitations that restrict their widespread application. In this study, the free nicotine in cigarette smoke was directly extracted by using cyclohexane according to the traditional solvent extraction method and detected via gas chromatography-mass spectrometry. Compared with the traditional two-phase solvent extraction, our experimental method is easy to execute and eliminates the influence of aqueous solutions on the original distribution of nicotine in cigarette smoke particulate matter. Furthermore, the presence of protonated nicotine in tobacco does not affect the determination. Compared with HS-SPME and NMR spectroscopy, our approach, which involves solvent extraction followed by chromatographic separation and instrumental detection, offers simplicity, improved precision, better detection limits, and reduced interference during the instrumental detection stage. The standard addition recoveries in the conducted experiment ranged from 96.2% to 102.5%. The limit of detection was 2.8 μg/cig, and the correlation coefficient for the quadratic regression of the standard curve exceeded 0.999. The relative standard deviation for parallel samples was between 1.7% and 3.4% (n = 5), fully meeting the requirements for the determination of free nicotine in cigarette smoke. Analysis of cigarette samples from 38 commercially available brands revealed that the content of free nicotine ranged from 0.376 to 0.716 mg/cig, with an average of 0.540 mg/cig, and free nicotine accounted for 39.1%–88.8% of the total nicotine content.
{"title":"Direct Extraction and Determination of Free Nicotine in Cigarette Smoke","authors":"Li Li, Jing Wen, Yuyang Deng, Juan Yang, Yue Yuan, Yi Shen, Guoce Liu, Yonghong Tian, Dean Lei","doi":"10.1155/2024/9273705","DOIUrl":"https://doi.org/10.1155/2024/9273705","url":null,"abstract":"The accurate determination of the free nicotine content in cigarette smoke is crucial for assessing cigarette quality, studying harm and addiction, and reducing tar levels. Currently, the determination of free nicotine in tobacco products primarily relies on methods such as pH calculation, nuclear magnetic resonance (NMR) spectroscopy, headspace solid-phase microextraction (HS-SPME), and traditional solvent extraction. However, these methods have limitations that restrict their widespread application. In this study, the free nicotine in cigarette smoke was directly extracted by using cyclohexane according to the traditional solvent extraction method and detected via gas chromatography-mass spectrometry. Compared with the traditional two-phase solvent extraction, our experimental method is easy to execute and eliminates the influence of aqueous solutions on the original distribution of nicotine in cigarette smoke particulate matter. Furthermore, the presence of protonated nicotine in tobacco does not affect the determination. Compared with HS-SPME and NMR spectroscopy, our approach, which involves solvent extraction followed by chromatographic separation and instrumental detection, offers simplicity, improved precision, better detection limits, and reduced interference during the instrumental detection stage. The standard addition recoveries in the conducted experiment ranged from 96.2% to 102.5%. The limit of detection was 2.8 <i>μ</i>g/cig, and the correlation coefficient <svg height=\"13.8595pt\" style=\"vertical-align:-2.2681pt\" version=\"1.1\" viewbox=\"-0.0498162 -11.5914 22.2574 13.8595\" width=\"22.2574pt\" xmlns=\"http://www.w3.org/2000/svg\" xmlns:xlink=\"http://www.w3.org/1999/xlink\"><g transform=\"matrix(.013,0,0,-0.013,0,0)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,4.498,0)\"></path></g><g transform=\"matrix(.0091,0,0,-0.0091,12.649,-5.741)\"></path></g><g transform=\"matrix(.013,0,0,-0.013,17.596,0)\"></path></g></svg> for the quadratic regression of the standard curve exceeded 0.999. The relative standard deviation for parallel samples was between 1.7% and 3.4% (<i>n</i> = 5), fully meeting the requirements for the determination of free nicotine in cigarette smoke. Analysis of cigarette samples from 38 commercially available brands revealed that the content of free nicotine ranged from 0.376 to 0.716 mg/cig, with an average of 0.540 mg/cig, and free nicotine accounted for 39.1%–88.8% of the total nicotine content.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"4 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140835688","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A fast, simple, and sensitive method for the simultaneous determination of seven polyamines in Nephotettix cincticeps was developed based on ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-3Q-MS) together with liquid phase extraction. Polyamines in insect samples were extracted with HClO4 solution and then were separated and detected by UPLC-3Q-MS, which was equipped with a hydrophilic interaction liquid chromatography column, within 5 min without any derivatization procedure. The method has been successfully used to detect 7 polyamines in healthy and difluormethylornithine-treated adults of Nephotettix cincticeps with a method limit of detection and the method limit of quantitation of 24–139 pg/mg and 82–464 pg/mg, respectively, an intraday and interday relative standard deviation (RSD, n = 5) of 1.97–6.00% and 2.08–5.92% respectively, and a recovery of 86–115%. The success of this study provided a reliable method for the rapid and high-throughput detection of polyamines in the insect sample.
{"title":"Rapid Analysis of Seven Polyamines in Nephotettix cincticeps by Using Ultra-Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry","authors":"Mingwen Zhang, Yunqiang Zhao, Zongwen Wang, Jintian Cheng","doi":"10.1155/2024/3302455","DOIUrl":"https://doi.org/10.1155/2024/3302455","url":null,"abstract":"A fast, simple, and sensitive method for the simultaneous determination of seven polyamines in <i>Nephotettix cincticeps</i> was developed based on ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-3Q-MS) together with liquid phase extraction. Polyamines in insect samples were extracted with HClO<sub>4</sub> solution and then were separated and detected by UPLC-3Q-MS, which was equipped with a hydrophilic interaction liquid chromatography column, within 5 min without any derivatization procedure. The method has been successfully used to detect 7 polyamines in healthy and difluormethylornithine-treated adults of <i>Nephotettix cincticeps</i> with a method limit of detection and the method limit of quantitation of 24–139 pg/mg and 82–464 pg/mg, respectively, an intraday and interday relative standard deviation (RSD, <i>n</i> = 5) of 1.97–6.00% and 2.08–5.92% respectively, and a recovery of 86–115%. The success of this study provided a reliable method for the rapid and high-throughput detection of polyamines in the insect sample.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"31 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140575975","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Rosuvastatin calcium is a widely used 3-hydroxy-3-methylglutaryl coenzyme A-reductase inhibitor developed for the treatment of dyslipidemia. To establish a control strategy for the elemental impurities, a new digestion method combined with an inductively coupled plasma-mass spectrometer (ICP-MS) was developed and validated by our team to determine elements Cd, Pb, As, Hg, Co, V, and Ni in rosuvastatin calcium tablets, which digest the sample perfectly even in the presence of a large number of excipients, especially titanium dioxide. The measurement mode was collision cell mode with kinetic energy discrimination (KED). 209Bi+, 115In+, and 89Y+ were chosen as internal standard elements. The recoveries of the limit of quantitation (LOQ) ranged from 90.5% to 106.4%, concentrations of the abovementioned elements in LOQ were 0.25 µg·L−1, 0.25 µg·L−1, 0.75 µg·L−1, 1.5 µg·L−1, 2.5 µg·L−1, 5 µg·L−1, and 8 µg·L−1 , respectively, linear correlation coefficients were above 0.9997, the recoveries in accuracy item ranged from 91.8% to 103.6%, and relative standard deviations (RSDs) of recovery in precision were not more than 1.8%, reflecting a reliable method of high sensitivity, strong anti-interference capacity, and good precision, and that it was suitable for the determination of elemental impurities in drugs.
{"title":"Development and Validation of Analytical Procedure for Elemental Impurities in Rosuvastatin Calcium Tablets by ICP-MS and Microwave Digestion","authors":"Yajie Hao, Guang Yin, Xuemei Wang, Juan Fu, Qihui Cao, Qinyong Sun, Guimin Zhang, Zhong Feng","doi":"10.1155/2024/9952318","DOIUrl":"https://doi.org/10.1155/2024/9952318","url":null,"abstract":"Rosuvastatin calcium is a widely used 3-hydroxy-3-methylglutaryl coenzyme A-reductase inhibitor developed for the treatment of dyslipidemia. To establish a control strategy for the elemental impurities, a new digestion method combined with an inductively coupled plasma-mass spectrometer (ICP-MS) was developed and validated by our team to determine elements Cd, Pb, As, Hg, Co, V, and Ni in rosuvastatin calcium tablets, which digest the sample perfectly even in the presence of a large number of excipients, especially titanium dioxide. The measurement mode was collision cell mode with kinetic energy discrimination (KED). 209Bi<sup>+</sup>, 115In<sup>+</sup>, and 89Y<sup>+</sup> were chosen as internal standard elements. The recoveries of the limit of quantitation (LOQ) ranged from 90.5% to 106.4%, concentrations of the abovementioned elements in LOQ were 0.25 <i>µ</i>g·L<sup>−1</sup>, 0.25 <i>µ</i>g·L<sup>−1</sup>, 0.75 <i>µ</i>g·L<sup>−1</sup>, 1.5 <i>µ</i>g·L<sup>−1</sup>, 2.5 <i>µ</i>g·L<sup>−1</sup>, 5 <i>µ</i>g·L<sup>−1</sup>, and 8 <i>µ</i>g·L<sup>−1</sup> , respectively, linear correlation coefficients were above 0.9997, the recoveries in accuracy item ranged from 91.8% to 103.6%, and relative standard deviations (RSDs) of recovery in precision were not more than 1.8%, reflecting a reliable method of high sensitivity, strong anti-interference capacity, and good precision, and that it was suitable for the determination of elemental impurities in drugs.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"44 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-03-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140314274","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Quang Minh Bui, Quang Trung Nguyen, Thanh Thao Nguyen, Ha My Nguyen, Thi Tinh Phung, Viet Anh Le, Ngoc Minh Truong, The Vinh Mac, Tien Dat Nguyen, Le Tuan Anh Hoang, Ha Minh Duc Tran, Van Nhan Le, Minh Duc Nguyen
Sausage is a convenient food that is widely consumed in the world and in Vietnam. Due to the rapid development of this product, the authenticity of many famous brands has faded by the rise of adulteration. Therefore, in this study, principal component analysis (PCA) was combined with chemical analysis to identify 6 sausage brands. Sausage samples were dried and then ground to a fine powder for both instrumental analyses of attenuated total reflectance-Fourier transform infrared (ATR-FTIR) and inductively coupled plasma–mass spectrometry (ICP-MS). Dried measurements of ATR-FTIR was performed directly on the ZnSe crystal, while elemental data were obtained through microwave digestion before the ICP-MS analysis. Principal component analysis (PCA) within the framework software of XLSTAT and STATISTICA 12 was performed on the spectroscopy and elemental dataset of sausage samples. PCA visualized the distinction of 6 sausage brands on both datasets of ATR-FTIR and ICP-MS. The classification on the spectroscopy profile showed that although more than 90% variation of the dataset was explained on the first two PCs, the difference between several brands was not detected as the distribution of data overlapped with one another. The PCA observation of the elemental composition on PC1 and PC3 has separated the sausage brands into 6 distinctive groups. Besides, several key elements contributed to the brands’ identification have been detected, and the most distinctive elements are Na, K, Ca, and Ba. PCA visualization showed the feasibility of the classification of sausage samples from different brands when combined with the results of FT-IR and ICP-MS methods. The experiment was able to differentiate the sausages from the 5 brands using multivariate statistics.
{"title":"Multivariate Statistical Analysis for the Classification of Sausages Based on Physicochemical Attributes, Using Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)","authors":"Quang Minh Bui, Quang Trung Nguyen, Thanh Thao Nguyen, Ha My Nguyen, Thi Tinh Phung, Viet Anh Le, Ngoc Minh Truong, The Vinh Mac, Tien Dat Nguyen, Le Tuan Anh Hoang, Ha Minh Duc Tran, Van Nhan Le, Minh Duc Nguyen","doi":"10.1155/2024/1329212","DOIUrl":"https://doi.org/10.1155/2024/1329212","url":null,"abstract":"Sausage is a convenient food that is widely consumed in the world and in Vietnam. Due to the rapid development of this product, the authenticity of many famous brands has faded by the rise of adulteration. Therefore, in this study, principal component analysis (PCA) was combined with chemical analysis to identify 6 sausage brands. Sausage samples were dried and then ground to a fine powder for both instrumental analyses of attenuated total reflectance-Fourier transform infrared (ATR-FTIR) and inductively coupled plasma–mass spectrometry (ICP-MS). Dried measurements of ATR-FTIR was performed directly on the ZnSe crystal, while elemental data were obtained through microwave digestion before the ICP-MS analysis. Principal component analysis (PCA) within the framework software of XLSTAT and STATISTICA 12 was performed on the spectroscopy and elemental dataset of sausage samples. PCA visualized the distinction of 6 sausage brands on both datasets of ATR-FTIR and ICP-MS. The classification on the spectroscopy profile showed that although more than 90% variation of the dataset was explained on the first two PCs, the difference between several brands was not detected as the distribution of data overlapped with one another. The PCA observation of the elemental composition on PC1 and PC3 has separated the sausage brands into 6 distinctive groups. Besides, several key elements contributed to the brands’ identification have been detected, and the most distinctive elements are Na, K, Ca, and Ba. PCA visualization showed the feasibility of the classification of sausage samples from different brands when combined with the results of FT-IR and ICP-MS methods. The experiment was able to differentiate the sausages from the 5 brands using multivariate statistics.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"1 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-03-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140105851","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In this study, for the first time, the levels of thirteen micro- and macromineral nutrients in the leaves, seeds, and supportive soil of Moringa stenopetala (M. stenopetala) were simultaneously determined using microwave plasma atomic emission spectroscopy (MP-AES). The samples were collected during the arid season, in 2019 from the three main M. stenopetala growing areas in southern Ethiopia (Chano Mile Kebele, Nechisar Kebele, and Konso Special Woreda). A novel digestion method for leaf and seed samples was developed using an optimized acid mixture (2.5 : 0.75 : 0.5 of HNO3, HClO4, and H2O2) at 240°C for 2 hrs and 30 min, resulting in clear and colorless solutions. The method makes the digestion process more efficient by minimizing the reagent volume, reducing digestion temperature and time, and simplifying the overall procedure. The efficiency of the optimized procedure was validated by spiking experiments, and the percentage recovery ranged between 94 and 110%. Under optimized experimental conditions, higher concentrations of essential minerals (K, Na, Ca, and Mg) were observed in the plant leaf and seed samples from the three areas. In addition, significant amounts of trace elements (Fe, Mn, Zn, and Cu) were also found. Importantly, no traces of the toxic elements (Cd and Pb) were detected in any of the analyzed samples, suggesting that the leaves and seeds of M. stenopetala are valuable sources of both micro- and macromineral nutrients and are safe from toxic metals. From a dietary perspective, the seed contains almost comparable concentrations of minerals as the leaves. As a result, the seeds of M. stenopetala can serve as an alternative source of minerals and play a role in overcoming the current global food crisis, particularly in the dry season. Analysis of variance at a 95% confidence level revealed significant differences in the levels of all mineral nutrients between the three sample means except K, Ca, Co, and Cu. Generally, the developed method includes an innovative digestion procedure that minimizes reagent consumption, operates at lower temperatures, and requires shorter digestion times, thereby optimizing resource utilization and maintaining analytical accuracy. Notably, the absence of toxic elements in the MP-AES procedure highlights the safety and reliability of M. stenopetala leaves and seeds as valuable, contamination-free sources of essential nutrients.
{"title":"Simultaneous Determination of Mineral Nutrients and Toxic Metals in M. stenopetala from Southern Ethiopia: A Comparative Study of Three Cultivating Areas Using MP-AES","authors":"Ashenafi Shemnsa, Wondimeneh Dubale Adane, Merid Tessema, Endale Tesfaye, Gizaw Tesfaye","doi":"10.1155/2024/8981995","DOIUrl":"https://doi.org/10.1155/2024/8981995","url":null,"abstract":"In this study, for the first time, the levels of thirteen micro- and macromineral nutrients in the leaves, seeds, and supportive soil of <i>Moringa stenopetala</i> (<i>M. stenopetala</i>) were simultaneously determined using microwave plasma atomic emission spectroscopy (MP-AES). The samples were collected during the arid season, in 2019 from the three main <i>M. stenopetala</i> growing areas in southern Ethiopia (Chano Mile Kebele, Nechisar Kebele, and Konso Special Woreda). A novel digestion method for leaf and seed samples was developed using an optimized acid mixture (2.5 : 0.75 : 0.5 of HNO<sub>3</sub>, HClO<sub>4</sub>, and H<sub>2</sub>O<sub>2</sub>) at 240°C for 2 hrs and 30 min, resulting in clear and colorless solutions. The method makes the digestion process more efficient by minimizing the reagent volume, reducing digestion temperature and time, and simplifying the overall procedure. The efficiency of the optimized procedure was validated by spiking experiments, and the percentage recovery ranged between 94 and 110%. Under optimized experimental conditions, higher concentrations of essential minerals (K, Na, Ca, and Mg) were observed in the plant leaf and seed samples from the three areas. In addition, significant amounts of trace elements (Fe, Mn, Zn, and Cu) were also found. Importantly, no traces of the toxic elements (Cd and Pb) were detected in any of the analyzed samples, suggesting that the leaves and seeds of <i>M. stenopetala</i> are valuable sources of both micro- and macromineral nutrients and are safe from toxic metals. From a dietary perspective, the seed contains almost comparable concentrations of minerals as the leaves. As a result, the seeds of <i>M. stenopetala</i> can serve as an alternative source of minerals and play a role in overcoming the current global food crisis, particularly in the dry season. Analysis of variance at a 95% confidence level revealed significant differences in the levels of all mineral nutrients between the three sample means except K, Ca, Co, and Cu. Generally, the developed method includes an innovative digestion procedure that minimizes reagent consumption, operates at lower temperatures, and requires shorter digestion times, thereby optimizing resource utilization and maintaining analytical accuracy. Notably, the absence of toxic elements in the MP-AES procedure highlights the safety and reliability of <i>M. stenopetala</i> leaves and seeds as valuable, contamination-free sources of essential nutrients.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"52 1","pages":""},"PeriodicalIF":2.6,"publicationDate":"2024-01-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139103046","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The aim of the current investigation is the development of a green, quick, easy, and accurate method for simultaneous preconcentration of fast green FCF (FG) and rhodamine B (Rh B) using a deep eutectic solvent (DES). Then, the high-performance thin layer chromatography (HPTLC) technique was used for the determination of analytes. Decanoic acid and tetrabutylammonium bromide were chosen as the components of DES. HPTLC analysis was performed on an aluminum plate silica gel 60 F254. Methanol-ammonia and ethyl acetate were selected as the mobile phase. Scanning of the plates was accomplished by scanner 3. Effective parameters on the preconcentration process such as concentration of salt, volume of DES, stirrer time, and pH were investigated via central composite design (CCD). Data validation demonstrated good repeatability. The limit of detection for FG and Rh B was obtained as 0.08 and 0.01 µg·mL−1, respectively. The enrichment factor for FG and Rh B was achieved as 7.43 and 10.77, respectively. The linear ranges for FG and Rh B were acquired as 0.10–1.20 and 0.05–1.20 µg·mL−1, respectively. The preconcentration factor for both analytes was 21.66. Finally, the proposed method was successfully used for the quantitation of FG and Rh B in pastille and lipstick.
{"title":"Simultaneous Preconcentration of Fast Green FCF and Rhodamine B Using Deep Eutectic Solvent and Determination via High-Performance Thin Layer Chromatography","authors":"Forough Karami, Ardeshir Shokrollahi","doi":"10.1155/2023/8797355","DOIUrl":"https://doi.org/10.1155/2023/8797355","url":null,"abstract":"The aim of the current investigation is the development of a green, quick, easy, and accurate method for simultaneous preconcentration of fast green FCF (FG) and rhodamine B (Rh B) using a deep eutectic solvent (DES). Then, the high-performance thin layer chromatography (HPTLC) technique was used for the determination of analytes. Decanoic acid and tetrabutylammonium bromide were chosen as the components of DES. HPTLC analysis was performed on an aluminum plate silica gel 60 F<sub>254</sub>. Methanol-ammonia and ethyl acetate were selected as the mobile phase. Scanning of the plates was accomplished by scanner 3. Effective parameters on the preconcentration process such as concentration of salt, volume of DES, stirrer time, and pH were investigated <i>via</i> central composite design (CCD). Data validation demonstrated good repeatability. The limit of detection for FG and Rh B was obtained as 0.08 and 0.01 <i>µ</i>g·mL<sup>−1</sup>, respectively. The enrichment factor for FG and Rh B was achieved as 7.43 and 10.77, respectively. The linear ranges for FG and Rh B were acquired as 0.10–1.20 and 0.05–1.20 <i>µ</i>g·mL<sup>−1</sup>, respectively. The preconcentration factor for both analytes was 21.66. Finally, the proposed method was successfully used for the quantitation of FG and Rh B in pastille and lipstick.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":" 21","pages":""},"PeriodicalIF":2.6,"publicationDate":"2023-12-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138514433","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The Dahuoluo pill (DHLP) is a classic Chinese patent medicine used to treat rheumatoid arthritis and other conditions. However, there has been no research on the chemical components of DHLP and the mechanisms by which it ameliorates rheumatoid arthritis. Hence, we analysed the chemical components of DHLP and the DHLP components absorbed in blood by using ultraperformance liquid chromatography-Q-exactive-orbitrap-mass spectrometry. We then used network pharmacology to predict the underlying mechanisms by which DHLP ameliorates rheumatoid arthritis. We identified 153 chemical compounds from DHLP, together with 27 prototype components absorbed in blood. We selected 48 of these compounds as potential active ingredients to explore the mechanism. These compounds are related to 88 significant pathways, which are linked to 18 core targets. This study preliminarily reveals the potential mechanisms by which DHLP ameliorates rheumatoid arthritis and provides a basis for further evaluation of the drug’s efficacy.
{"title":"Characterization of the Active Ingredient and Prediction of the Potential Mechanism of Dahuoluo Pill via Mass Spectrometry with the Network Pharmacology Method","authors":"Haoran Xu, Yuelin Bi, Xin Feng, Jiaqi Wang, Gengyuan Yu, Tonghua Zhang, Tianyi Li, Xuhua Gao, Runhua Liu, Yu Sun, Hao Wu, Linlin Fang, Chenning Zhang, Yikun Sun","doi":"10.1155/2023/8819534","DOIUrl":"https://doi.org/10.1155/2023/8819534","url":null,"abstract":"The Dahuoluo pill (DHLP) is a classic Chinese patent medicine used to treat rheumatoid arthritis and other conditions. However, there has been no research on the chemical components of DHLP and the mechanisms by which it ameliorates rheumatoid arthritis. Hence, we analysed the chemical components of DHLP and the DHLP components absorbed in blood by using ultraperformance liquid chromatography-Q-exactive-orbitrap-mass spectrometry. We then used network pharmacology to predict the underlying mechanisms by which DHLP ameliorates rheumatoid arthritis. We identified 153 chemical compounds from DHLP, together with 27 prototype components absorbed in blood. We selected 48 of these compounds as potential active ingredients to explore the mechanism. These compounds are related to 88 significant pathways, which are linked to 18 core targets. This study preliminarily reveals the potential mechanisms by which DHLP ameliorates rheumatoid arthritis and provides a basis for further evaluation of the drug’s efficacy.","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"14 2","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135539637","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-10-30eCollection Date: 2023-01-01DOI: 10.1155/2023/5561071
Eulogio J Llorent-Martínez, Julia Jiménez-López, Antonio Ruiz-Medina
We propose a modification of terbium-sensitized luminescence (TSL) by means of the introduction of nanoparticles to improve the sensitivity and selectivity of the analytical methods. TSL detection is usually based on the complexation between fluorescent organic compounds (the analytes) and terbium. The organic compound is then excited, and, after an energy transfer towards terbium, the latter emits the luminescence signal. Here, the modification consists of the introduction of nanoparticles (carbon quantum dots, CQDs) into the system. The carboxylic groups of CQDs react with terbium, providing an interesting time-resolved luminescence probe. We applied this system for the determination of the neonicotinoid imidacloprid (IMID). When IMID was introduced in the terbium-CQDs system, the luminescent signal (λexc/λem of 256/545 nm) was quenched, proportionally to IMID concentration in the range of 100-2500 ng·mL-1, obtaining a limit of detection of 30 ng·mL-1. A method detection limit of 0.9 mg·kg-1 was reached in caneberries, thus complying with the maximum residue level of 5 mg·kg-1 established by Codex Alimentarius. We performed recovery experiments in caneberries (blackberries, blueberries, raspberries, and mulberries), obtaining recovery yields close to 100% in all cases. These results show that the use of terbium ions-nanoparticles luminescence probes can be useful for screening purposes in quality control laboratories.
{"title":"Luminescent Probe Based on Terbium-Carbon Quantum Dots for the Quantification of Imidacloprid in Caneberries.","authors":"Eulogio J Llorent-Martínez, Julia Jiménez-López, Antonio Ruiz-Medina","doi":"10.1155/2023/5561071","DOIUrl":"10.1155/2023/5561071","url":null,"abstract":"<p><p>We propose a modification of terbium-sensitized luminescence (TSL) by means of the introduction of nanoparticles to improve the sensitivity and selectivity of the analytical methods. TSL detection is usually based on the complexation between fluorescent organic compounds (the analytes) and terbium. The organic compound is then excited, and, after an energy transfer towards terbium, the latter emits the luminescence signal. Here, the modification consists of the introduction of nanoparticles (carbon quantum dots, CQDs) into the system. The carboxylic groups of CQDs react with terbium, providing an interesting time-resolved luminescence probe. We applied this system for the determination of the neonicotinoid imidacloprid (IMID). When IMID was introduced in the terbium-CQDs system, the luminescent signal (<i>λ</i><sub>exc</sub>/<i>λ</i><sub>em</sub> of 256/545 nm) was quenched, proportionally to IMID concentration in the range of 100-2500 ng·mL<sup>-1</sup>, obtaining a limit of detection of 30 ng·mL<sup>-1</sup>. A method detection limit of 0.9 mg·kg<sup>-1</sup> was reached in caneberries, thus complying with the maximum residue level of 5 mg·kg<sup>-1</sup> established by Codex Alimentarius. We performed recovery experiments in caneberries (blackberries, blueberries, raspberries, and mulberries), obtaining recovery yields close to 100% in all cases. These results show that the use of terbium ions-nanoparticles luminescence probes can be useful for screening purposes in quality control laboratories.</p>","PeriodicalId":14974,"journal":{"name":"Journal of Analytical Methods in Chemistry","volume":"2023 ","pages":"5561071"},"PeriodicalIF":2.6,"publicationDate":"2023-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10627717/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"71481827","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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