يعرض 1 - 10 نتائج من 1,104 نتيجة بحث عن '"structural identification"', وقت الاستعلام: 1.27s تنقيح النتائج
  1. 1
    دورية أكاديمية

    المؤلفون: Enfen LIU, Lin SUN, Ziye CHEN, Jun WANG

    المصدر: Shipin gongye ke-ji, Vol 45, Iss 13, Pp 257-264 (2024)

    الوصف: In order to study the effective method of the enrichment and purification of anthocyanin in black wolfberry and mulberry, and identify the structure of anthocyanin, the black wolfberry and mulberry extracts were purified by macroporous resins. The adsorption and desorption abilities of different types of the resins for anthocyanins were compared. LX-20SS was optimized as the resin for the purification of anthocyanins from black wolfberry. The purification conditions were as follows: The mass ratio of resin to crude anthocyanin powder of black wolfberry was at 10:1, and the elution concentration of ethanol was 70%, and the flow rate was 3 mL/min. After the purification, the content of anthocyanin reached 144.18±3.40 mg/g. DM-21 was optimized as the resin for the purification of mulberry anthocyanin. The purification conditions were as follows: The mass ratio of resin to crude anthocyanin powder of mulberry was at 20:3, and the elution concentration of ethanol was 30%, and the flow rate was 1 mL/min. The content of anthocyanin reached 112.44±2.24 mg/g after purification. High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis for anthocyanin structures in black wolfberry and mulberry showed that the main anthocyanin in black wolfberry was petunidin-3-O-rutinose (p-coumaroyl)-5-O-glucoside, which accounted for more than 95% of the total anthocyanin. In addition, there are two main types of anthocyanins in mulberry, corresponding to cyanidin-3-glucoside and cyanidin-3-rutinoside, which accounted for 63.58% and 36.42% of the total anthocyanins respectively. The results provided references for the development of black wolfberry and mulberry.

    وصف الملف: electronic resource

  2. 2
    دورية أكاديمية

    المصدر: Zhipu Xuebao, Vol 45, Iss 3, Pp 375-385 (2024)

    الوصف: Sugar esters in tobacco play an important role as precursors generating tobacco aroma species, and their presence significantly influence the quality of tobacco leaves. Typically present in trace amounts, sugar esters in tobacco exhibit a diverse range of isomers, making their separation and analysis a significant challenge. To address this challenge, mass spectrometry has been extensively applied for the identification and differentiation of various of sugar ester compounds in tobacco. However, there is no study regarding the separation and analysis of sugar esters specifically within Burley tobacco leaves. In this research, Burley tobacco leaf extracts were obtained using the solvent extraction technique, and underwent separation using silica gel column chromatography. Ultimately, the fractions comprising glucose esters and various sucrose esters were collected, respectively. The structural identification of these acquired sugar esters was achieved by liquid chromatography-tandem mass spectrometry (LC-MSn). According to the MS2 fragment ions of sucrose esters, the mass difference of 162.05 and 204.06 was mainly observed, implying an unbound fructose ring and a fructose ring acetylated in the sucrose ester, respectively. The composition information of fatty acids substituted to the glucose ring were further revealed based on the MS3 or MS2 fragment ions from sucrose esters or glucose esters. By combining the relative molecular weight, molecular formula, and the above mentioned fragment information, four types of sucrose esters from SE-I to SE-IV (referred to as compound 1-20) and two types of glucose esters GE-I to GE-II (referred to as compound 21-31) were finally identified. Among them, four sucrose esters of distinct molecular weights were newly discovered, and the structures of eight glucose esters were reported for the first time in cultivated tobacco. The sugar esters were analyzed by high-resolution mass spectrometry, which could effectively distinguish the number of fatty acids substituted on glucose and fructose, thus facilitating the differentiation of sugar ester types. Nevertheless, the identification of sugar esters in this study was limited to determine the characteristic skeleton and fatty acid composition. Detailed information on specific fatty acid types and substitution sites require further investigation using NMR technique. In conclusion, these results contribute to the current knowledge of sugar esters in Burley tobacco by expanding the range of identified types and providing high-resolution mass spectrometry data for various types of sugar esters for the first time. These findings hold significant reference value for the analysis, identification, and metabolism of different sucrose and glucose esters in tobacco.

    وصف الملف: electronic resource

  3. 3
    دورية أكاديمية

    المصدر: Shipin Kexue, Vol 45, Iss 4, Pp 42-49 (2024)

    الوصف: The transformation of tert-butylhydroquinone (TBHQ) added in lard, soybean and palm oil was investigated during storage. The results showed that when the storage time was extended, the sum of the remaining amount of TBHQ and the production of 2-tert-butyl-1,4-benzoquinone (TBBQ) in oil samples was less than the initial amount of TBHQ added. The same chromatographic peaks except for TBHQ and TBBQ were found in the gas chromatograms of the methanol extracts from different oil samples. The unknown chromatographic peaks were isolated and purified by preparative liquid chromatography (Prep-LC), and their structures were identified and characterized by ultra-high performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-Q-TOF-MS), nuclear magnetic resonance (NMR), ultraviolet (UV) spectroscopy, and Fourier transform infrared (FTIR) spectroscopy. These results showed that the conversion products of added TBHQ were the same in different oils and fats, including TBBQ and 2-methylallyl-hydroquinone (MAHQ).

    وصف الملف: electronic resource

  4. 4
    رسالة جامعية

    المؤلفون: Gago Ferrero, Pablo

    المساهمون: University/Department: Universitat de Barcelona. Departament de Química Analítica

    مرشدي الرسالة: pablo8084@hotmail.com, Díaz Cruz, Silvia, Barceló i Cullerés, Damià, Galcerán Huguet, M. Teresa

    المصدر: TDX (Tesis Doctorals en Xarxa)

    الوصف: La progresiva destrucción de la capa de ozono unida a los largos periodos de exposición solar, principalmente en actividades de ocio, ha contribuido a una mayor incidencia de las enfermedades causadas por la radiación solar, principalmente el cáncer de piel. Hoy en día, los compuestos orgánicos que actúan de pantalla frente a la radiación solar ultravioleta (filtros solares, UV-F) se utilizan cada vez con más frecuencia y en mayor cantidad dada la concienciación actual que existe con respecto a los efectos perjudiciales de la radiación solar. Aunque tradicionalmente se han usado en productos bronceadores con este fin, actualmente se están añadiendo a otros productos cosméticos para evitar que componentes sensibles a la radiación solar se descompongan, así como en otros productos como detergentes líquidos, plásticos, papel, pinturas, textiles, etc. Los UV-F acceden al medio acuático por vía directa, a través de actividades acuáticas (baño, natación) y principalmente por vía indirecta a través de las estaciones de tratamiento de aguas residuales urbanas (EDARs), después de haber sido transferidos del cuerpo a la vestimenta, por la excreción después de su absorción dérmica, y a través de las aguas residuales industriales. Dada la elevada proporción de estos aditivos que se utiliza en las formulaciones y su frecuente uso, la cantidad de UV-F que se descarga en el medio ambiente es importante. Actualmente, uno de los mayores retos en el estudio ambiental de los UV-F es disponer de métodos de análisis lo suficientemente sensibles para poder evaluar la presencia de tales compuestos, sus metabolitos y otros productos de transformación en el sistema agua/sedimento/biota, en conexión con su grado de eliminación en los tratamientos de aguas residuales. Esta Tesis Doctoral aporta herramientas y conocimiento para ampliar la información disponible sobre el impacto ambiental de los filtros solares orgánicos (presencia, destino y degradación). En esta memoria de Tesis se describe el desarrollo de nuevas metodologías analíticas basadas en la cromatografía líquida de alta resolución acoplada a espectrometría de masas en tándem (LC-MS/MS) para el análisis de UV-F y sus principales productos de transformación, compuestos hasta el momento escasamente investigados. Se incluye el desarrollo y validación de un método analítico completamente automatizado, basado en la extracción en fase sólida (SPE) on-line acoplada a LC-MS/MS, para el análisis de aguas, así como otras metodologías basadas en la extracción con líquidos presurizados (PLE) y posterior análisis mediante LC-MS/MS para diferentes matrices ambientales sólidas como lodos de EDAR, sedimentos o peces. Estas metodologías se han aplicado en diferentes estudios para investigar la presencia y distribución de UV-F en muestras reales de aguas naturales, aguas residuales, sedimentos y lodos de EDAR. También se aportan nuevos datos sobre la bioacumulación de estos compuestos; se han analizado diferentes especies de peces de diversas cuencas hidrográficas de régimen mediterráneo así como también muestras de mamíferos marinos (delfines) de la costa de Brasil. Teniendo en cuenta que se ha comprobado que los procesos biológicos convencionales que se aplican en las EDARs no son efectivos para la eliminación de los UV-F, se han estudiado nuevos tratamientos, eficientes y respetuosos con el medio ambiente, para su degradación en fase líquida y sólida. Concretamente se ha investigado la biodegradación mediante el hongo Trametes versicolor, obteniendo resultados muy satisfactorios. También, se ha estudiado la degradación de estos compuestos mediante procesos de oxidación avanzada, en concreto, la ozonización y su combinación con peróxido de hidrógeno obteniendo una gran eficacia en sus eliminaciones. En todos los estudios de degradación se hizo especial hincapié en la identificación de los productos de transformación formados en los procesos mediante la aplicación de la espectrometría de masas de alta resolución.

    الوصف (مترجم): UV filters (UV-F), have become very popular chemicals since they were shown to have a protective role against photoaging, photocarcinogenesis and photoimmunosupression promoted by UV sun radiation. UV-F are increasingly used in personal care products such as sunscreen products, beauty creams, lipsticks, hair sprays, shampoos, etc. Despite they are traditionally used in cosmetics last years they have been also widely added in formulations of other products to protect the components, for instance in paints, textiles, paper, plastics, etc. UV-F are recent emerging environmental pollutants for which there is currently a lack of knowledge about their occurrence, fate and effects on the ecosystems. UV-F enter the environment through two principal sources: direct inputs from recreational activities and indirect wastewater input. The presence of these compounds in the aquatic ecosystem raises environmental concern since most of them are known to display endocrine disruption activity. This Thesis focuses on the development of analytical methodology for the determination of organic UV-F in water, sediment, sewage sludge and biota based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The developed tools allowed the detection of these compounds in complex environmental matrices and contributed to have a broader view on the presence and distribution of these compounds in the aquatic ecosystem. These methods were successfully applied to investigate the occurrence of selected UV filters in groundwater, river water, wastewater, sediment, sewage sludge, fish and marine mammals (dolphins). Moreover, this Thesis focuses on the research of new processes, sustainable and environmentally friendly, for the degradation of UV-F in wastewater and sewage sludge. Specifically, photodegradation, fungal biodegradation and advanced oxidation processes (ozonation and peroxone oxidation) were investigated. The identification of new transformation products formed during these treatments using non-target analysis based on high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) has been other main aim of this research.

    وصف الملف: application/pdf

  5. 5
    دورية أكاديمية

    المصدر: Heliyon, Vol 10, Iss 9, Pp e29902- (2024)

    الوصف: Objective: This study is aimed to screen, identify and detect illegal additives from healthcare products which claim or imply to have weight-loss effects. Method: Ultra-high performance liquid chromatography-quadruple-time-of-flight mass spectroscopy (UPLC-Q-TOF/MS) was employed to perform non-targeted screening of illegal additives from a total of 26 batches of healthcare products with weight-loss effects. A novel oxyphenisatin dipropionate analog was discovered in a fruit-flavored jelly that was not clearly labeled as containing added drugs. After being separated and purified by silica gel column chromatography, the analog was unambiguously characterized by one-dimensional (1D) and two-dimensional (2D) nuclear magnetic resonance (NMR) spectroscopies. The molecular structure of the analog was finally identified by comparing the spectra of the analog with those of suspected candidates prepared by de novo synthesis strategy. Thereafter, a sensitive and precise reversed phase ultra performance liquid chromatography coupled with photodiode array (UPLC-PDA) detection method was developed and verified for the determination of the analog in 15 batches of real samples. Results: In the MS/MS spectra, the signal intensity of mass/charge ratios (m/z, 242 and 214) of the novel analog fragments was highly similar to that of mass/charge ratios (m/z, 224 and 196) of oxyphenisatin dipropionate fragments. Additionally, the 1D NMR spectrum of the analog was completely consistent with that of one of the suspected candidates prepared by the de novo synthesis strategy. Based on the above analysis, the structure of the analog was determined as 3,3-bis[4'-(propionyloxy)phenyl]-6-fluoro-2-oxoindoline, which was briefly named 6-F oxyphenisatin dipropionate. A developed quantitative method showed good linearity (R2 > 0.999) in a concentration range of 1.0–100 μg/mL. The limits of detection (LOD) and quantification (LOQ) for the analog was 3 mg/kg and 10 mg/kg, respectively. The average recoveries of the analog from spiked three different matrix samples in low (1 time of LOQ), medium (2 times of LOQ), and high (10 times of LOQ) concentrations were varied from 93.9 % to 107.8 % with a precision of 0.03–1.56 %. Results of quantitative analysis in 15 batches of healthcare products revealed that the content of 6-F oxyphenisatin dipropionate in a fruit-flavored jelly and a solid beverage was 118 mg/kg and 330 mg/kg, respectively. Conclusion: In terms of its structure, 6-F oxyphenisatin dipropionate replaces hydrogen atom by the fluorine atom at position 6 on the indolinone fragment in oxyphenisatin dipropionate. To our best knowledge, 6-F oxyphenisatin dipropionate has never been detected as an illegal additive in foods. Such illegal addition of the analog to foods is more concealing, thus the supervision and testing departments should attach great importance to its application in food markets.

    وصف الملف: electronic resource

  6. 6
    دورية أكاديمية

    المصدر: Digital Chinese Medicine, Vol 6, Iss 4, Pp 426-437 (2023)

    الوصف: [Abstract: Objective: To identify the main components in the extracts of different parts of Juandan Baihe (Lilium lancifolium) by ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) technology and investigate their hypoglycemic activities. Methods: The MS fragmentation pathways of the main types of compounds in Juandan Baihe (Lilium lancifolium) were studied, and the main components in the extracts were systematically identified using MS fragmentation pathways combined with MS mining technology. Based on the hyperglycemia male mouse model [specific pathogen free (SPF)-grade Kunming mice] induced by streptozotocin (intragastric administration of 80 mg/kg for 3 d), the hypoglycemic effects of extracts of Juandan Baihe (Lilium lancifolium) roots, stems, corms, leaves, and flowers were evaluated by measuring the changes of blood glucose, daily water consumption, daily food intake, and body weight. Results: The MS fragmentation pathways of regalosides, dioscins, phenylpropanoids, flavonoids, and chlorogenic acids in Juandan Baihe (Lilium lancifolium) were clarified, and a mining method for compounds in this plant was constructed. A total of 58 compounds, including 6 chlorogenic acids, 14 regalosides, 13 phenylpropanoids, 5 flavonoids, and 20 dioscins, were identified from the roots, stems, corms, leaves, and flowers of Juandan Baihe (Lilium lancifolium). Among them, 30 compounds were reported for the first time from this plant. The root and corm extracts demonstrated significant hypoglycemic activities by reducing blood glucose levels from 23.76 ± 1.21 and 24.29 ± 1.35 mmol/L to 17.21 ± 1.23 and 18.78 ± 1.49 mmol/L, respectively (P < 0.05). The roots and corms extracts could also attenuate the symptoms of polydipsia (P < 0.01), polyphagia (P < 0.05), and weight loss caused by diabetes. Conclusion: This study clarifies that the roots of Juandan Baihe (Lilium lancifolium) are rich in regalosides and dioscins for the first time, and have significant hypoglycemic activities, providing the foundation for the comprehensive utilization of this plant and the development of hypoglycemic drugs.

    وصف الملف: electronic resource

  7. 7
    دورية أكاديمية

    المصدر: International Journal of Fruit Science, Vol 23, Iss 1, Pp 51-61 (2023)

    الوصف: ABSTRACTThe aim of this study was to isolate and purify flavonoids from Jujube (Zizipus jujuba Mill.) fruit and further evaluate antibacterial activities. Semi-preparative high-performance liquid chromatography (HPLC) was used to isolate and purify the flavonoids, while nuclear magnetic resonance spectroscopy (NMR) was employed for structural identification. Five flavonoids, including epicatechin, quercetin, rutin, isoquercitrin, and hyperin were identified. Antibacterial activity assays showed quercetin had the greatest inhibitory effect on Escherichia coli, Shigella, and Pseudomonas aeruginosa, and the minimum inhibitory concentration (MIC) against Escherichia coli or Pseudomonas aeruginosa was 250 μg/mL and against Shigella was 125 μg/mL. Rutin had the greatest inhibitory effect on Staphylococcus aureus, the MIC of which was 62.5 μg/mL. Hyperin had the greatest inhibitory effect on Bacillus subtilis, the MIC of which against Bacillus subtilis was 250 μg/mL, whereas that against Staphylococcus aureus was 62.5 μg/mL. We found that the antibacterial effects of the flavonoids were strong at a pH less than 6 and that they dropped sharply with increasing pH. Furthermore, the five metal ions Na+, Ca2+, K+, Fe2+, and Mg2+ generally increased the antibacterial activity of quercetin against Escherichia coli, Shigella, and Pseudomonas aeruginosa, and that of rutin against Staphylococcus aureus. For hyperin, Ca2+ and K+ had the strongest antibacterial effects. The present study suggests that the flavonoids extracted from Jujube (Zizipus jujuba Mill.) fruit were considered a promising candidate for natural and healthy antibacterial agents for the pharmaceutical and food industries.

    وصف الملف: electronic resource

  8. 8
    دورية أكاديمية

    المصدر: Guangxi Zhiwu, Vol 43, Iss 11, Pp 2106-2112 (2023)

    الوصف: To study the alkaloids in the rhizomes of Stephania macrantha. The total alkaloids of S. macrantha were extracted by acid extraction and alkali precipitation method. Eleven alkaloids have been isolated and purified by silica gel column chromatography and preparative high performance liquid chromatography (HPLC). The structures of compounds were identified by spectroscopic methods (NMR and MS). The results were as follows: (1) Eleven compounds were designated as sinomenine (1), sinoactine (2), stepharine (3), reticuline (4), isocorydine (5), corydalmine (6), asimilobine (7), sukhodianine (8), dicentrine (9), 7-oxocrebanine (10) and palmatine (11). (2) The total alkaloids of S. macrantha and sinomenine had inhibitory activities on human lung cancer cells (A549), with IC50 values of 7.5×10-4 g·mL-1 and 6.59×10-9 g·mL-1, respectively. Compounds 2, 3, 4, 7, 8, 9 and 10 were isolated for the first time from S. macrantha. The chemical constituents from S. macrantha belong to five types of alkaloids such as morphanes, proaporphines, aporphines, benzyltetrahydroi soquinolines and protoberberines.

    وصف الملف: electronic resource

  9. 9
    دورية أكاديمية

    المصدر: Guangxi Zhiwu, Vol 43, Iss 11, Pp 2024-2032 (2023)

    الوصف: Bruguiera gymnorhiza hypocotyl is a common marine herbal medicine of the Jing people used in the treatment of hepatitis B. Firstly, MTT and real-time fluorescence quantitative PCR methods were used to determine the anti-HBV activity of different extracted parts of B. gymnorhiza hypocotyl, the chemical constituents of the active extraction parts were isolated and identified using modern chromatographic techniques and spectroscopic methods, and in vitro screening model was employed to test the anti-HBV activity of obtained compounds. The results were as follows: (1) The n-butanol phase of the hypocotyl exhibited anti-HBV activity; (2) A total of 11 compounds were isolated and structurally identified, namely uridine (1), thymidine (2), adenosine (3), oryzalactam (4), n-butyl-O-D-fructopyranoside (5), nortetillapyrone (6), (4R,6S)-4-methoxyl-2,3-dihydroaquilegiolide (7), (4R,6S)-2-dihydromenisdaurilide (8), gallcatechin (9), 1-(4-hydroxy-3-methoxy)-phenyl-2-[4-(1,2,3-trihydroxypropyl)-2-methoxy]-phenoxy-1,3-propandiol(10), and (-)-lyoniresinol-9-O-β-D-xylopyrano-side (11), among them, compounds 4, 5, 7 and 8 were firstly obtained from B. gymnorhiza, and Compound 4 showed anti-HBV activity with an inhibition rate of 23.59%. The study clarify the chemical composition of the anti-HBV of B. gymnorhiza hypocotyl.

    وصف الملف: electronic resource

  10. 10
    دورية أكاديمية

    المصدر: Guangxi Zhiwu, Vol 43, Iss 11, Pp 2149-2158 (2023)

    الوصف: The purpose of this paper was to investigate the chemical constituents of Potentilla kleiniana and their anti-inflammatory activities. The 60% ethanol extract of P. kleiniana were isolated by D-101 macroporous adsorptive resins, silica gel, Toyopearl HW-40F and other methods, and their chemical structures were elucidated on the spectral data of NMR and HR-ESI-MS analysis. Meanwhile, the anti-inflammatory activities of compounds were evaluated by mouse macrophage (RAW 264.7) inflammatory model induced by lipopolysaccharide (LPS) in vitro. The results were as follows: (1) Fifteen compounds were isolated and identified from P. kleiniana as 2-(heptadecanoyloxy)propane-1,3-diyl distearate (1), 9,12,13-trihydroxy-10,15-octadecadienoic acid (2), methyl-9,12,13-trihydroxy-10,15-octadecadienoic acid (3), 2,2′-oxybis(1,4-di-tert-butylbenzene) (4), emodin (5), chrysophanol (6), (6R,9R)-3-oxo-α-ionol-9-O-β-D-glucopyranoside (7), neo-andrographolide (8), methyl-α-D-fructofuranosides (9), 1-O-β-D-fructofuranosyl-α-D-allopyranos (10), p-coumaric acid (11), cesternosides A (12), koaburaside (13), orientin (14), isoorientin (15). Compounds 1-15 were obtained from Potentilla genus for the first time. (2) The anti-inflammatory test results showed that compounds 1-3, 8, and 11-15 had moderate inhibitory activities on NO production, and the inhibition rate of compound 8 was 72.5% at the concentrations of 25 μmol·L-1. In conclusion, the study enriches the phytochemical information of P. kleiniana, and clarifies that fatty acid derivatives, phenolic components and diterpenoids are anti-inflammatory active components, which provides a theoretical basis for further exploitation of P. kleiniana.

    وصف الملف: electronic resource