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Integrated methods for fingerprinting of monofloral honeys 单花蜂蜜指纹图谱的综合方法
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-06-22 DOI: 10.1080/10826076.2023.2224024
Alina Tarna, C. Cimpoiu, A. Hosu
Abstract Honey is an important functional food due to its content of polyphenolic compounds with beneficial effects on human body. The analysis of polyphenolic compound in honey is very promising in determination of floral origin and so for quality control. This study approaches a new methodology using integrated methods for the determination of honey authenticity. Polyphenolic compounds from seven different types of monofloral honey from two different sources were extracted and analyzed by thin layer chromatography (TLC) and UV-Vis spectroscopy. Chromatographic analysis was performed on TLC Silica gel 60 RP-18 F254 plates using a mobile phase consisting in a mixture of methanol: water: formic acid (5: 5: 0.1, v/v/v). The images from the TLC analysis were processed and the obtained chromatograms together with the UV-Vis deconvoluted spectra of honey were subjected to visual and statistical analysis. The obtained results showed notable differences between the honey samples, which can be used to establish their floral origin and for their authentication. The proposed methodology is easy to perform, cost-effective and offers complementary information, therefore it has the potential of being used for the honey authentication. GRAPHICAL ABSTRACT
摘要蜂蜜是一种重要的功能性食品,它含有对人体有益的多酚类化合物。蜂蜜中多酚类化合物的分析在花源鉴定及质量控制方面具有重要的应用前景。本研究探讨了一种新的方法,使用综合方法来确定蜂蜜的真实性。从两种不同来源的七种不同类型的单花蜂蜜中提取多酚化合物,并用薄层色谱法和紫外-可见光谱法进行分析。在TLC硅胶60上进行色谱分析 RP-18F254板,使用由甲醇:水:甲酸(5:5:0.1,v/v/v)的混合物组成的流动相。对来自TLC分析的图像进行处理,并对获得的色谱图以及蜂蜜的UV-Vis去卷积光谱进行视觉和统计分析。所得结果表明,蜂蜜样品之间存在显著差异,可用于确定其花的来源和鉴定。所提出的方法易于执行,具有成本效益,并提供了补充信息,因此具有用于蜂蜜认证的潜力。图形摘要
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引用次数: 0
Library-based UHPLC-Q-exactive-orbitrap-MS putative identification of isomeric and non-isomeric bioactives from Zibushengfa Tablet and pharmacopeia quality-marker chemistry 基于uhplc - q -轨道谱-质谱的子补生发片异构体和非异构体生物活性推定鉴定及药典质量标记化学
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-06-21 DOI: 10.1080/10826076.2023.2223640
Shaoman Chen, Xican Li, Jingyuan Zeng, Rongxin Cai, Chunhou Li, Chuanbing Chen
Abstract Zibushengfa Tablet is a widely consumed traditional Chinese medicine (TCM) prescription. However, its main bioactives remain unclear and its pharmacopeia quality-marker (Q-marker) is poorly characterized nowadays. The present study analyzed its lyophilized aqueous powder using ultra-high-performance liquid chromatography-quadrupole-orbitrap mass spectrometry. Through comparison with authentic standards in the library, 46 bioactives were putatively identified, including quinic acid, D-gluconic acid, gallic acid, protocatechuic acid, 5-caffeoylquinic acid, L-tryptophan, salidroside, (+)-catechin hydrate, caffeic acid, cryptochlorogenic acid, mangiferin, ferulic acid, myricetin-3-O-galactoside, 2,3,5,4’-tetrahydroxystilbene-2-O-glucoside, forsythoside B, myricitrin, rutin, hyperoside, acteoside, 3,4-dicaffeoylquinic acid, myricetin, senkyunolide A, isochlorogenic acid C, quercitrin, (+)-epipinoresinol, quercetin, biochanin A, calycosin, luteolin, wedelolactone, calycosin-7-O-glucoside, chrysoeriol, trans-cinnamic acid, formononetin, chrysin, 3,3’,4’,5,6,7,8-heptamethoxyflavone, Z-ligustilide, amentoflavone, tangeretin, hinokiflavone, emodin, physcion, linoleic acid, stearic acid, palmitic acid, and palmitic acid ethyl ester. Of these, four pairs of isomers were successfully differentiated using the newly established library-filtering strategy. On this basis, senkyunolide A, amentoflavone, quercetin, quercitrin, and wedelolactone are preliminarily suggested as additional quality-markers for the consideration by Pharmacopeia Committee, to prevent the possible adulterate. Graphical Abstract
摘要紫蒲生发片是一种消费广泛的中药方剂。然而,其主要生物活性尚不清楚,其药典质量标志物(Q-marker)目前的特征也很差。本研究采用超高效液相色谱-四极环质谱法对其冻干水性粉末进行了分析。通过与文库中真实标准品的比较,推定鉴定出46种生物活性物质,包括奎宁酸、D-葡萄糖酸、没食子酸、原儿茶酸、5-咖啡基奎宁酸,L-色氨酸、红景天苷、(+)-儿茶素水合物、咖啡酸、隐绿原酸、芒果苷、阿魏酸、杨梅素-3-O-半乳糖苷、2,3,5,4’-四羟基二苯乙烯-2-O-葡萄糖苷,连翘苷B、肉豆蔻苷、芦丁、金丝桃苷、acteoside、3,4-二咖啡基奎宁酸、杨梅素、仙子内酯A、异绿原酸C、槲皮素、(+,黄酮、大黄素、大黄素,亚油酸、硬脂酸、棕榈酸和棕榈酸乙酯。其中,使用新建立的文库过滤策略成功区分了四对异构体。在此基础上,为了防止可能的掺假,初步建议将人参内酯A、核黄素、槲皮素、槲皮素和韦氏内酯作为额外的质量标志物,供药典委员会考虑。图形摘要
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引用次数: 2
Advances on analysis methods of ginkgo biloba leaf extract 银杏叶提取物分析方法研究进展
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-06-21 DOI: 10.1080/10826076.2023.2223618
Jinhao Li, Jing Lan, Shufang Wang, Jianbiao Yao, Fangfang Wang, Xingchu Gong
Abstract Ginkgo biloba leaf extract (EGBL) is a valuable herbal extract. The main active ingredients are flavonoids, terpene lactones, organic acids and proanthocyanidins. In recent years, there have been many reports on the detection of the above active ingredients. In this paper, the analysis methods of chemical components in EGBL were reviewed, such as ultraviolet spectrophotometry, high-performance liquid chromatography, and quantitative nuclear magnetic resonance. The analysis methods of ginkgolic acids are also reviewed. Based on the current research progress, three suggestions are provided. Firstly, the quality marker research of EGBL needs to be strengthened. Secondly, more bioassay methods for EGBL quality control should be developed. Thirdly, it is necessary to strengthen the detection of proanthocyanidins in EGBL. GRAPHICAL ABSTRACT
摘要银杏叶提取物(EGBL)是一种很有价值的中草药提取物。主要活性成分为黄酮类化合物、萜烯内酯、有机酸和原花青素。近年来,关于检测上述活性成分的报道很多。本文综述了EGBL中化学成分的分析方法,如紫外分光光度法、高效液相色谱法和定量核磁共振法。综述了银杏酸的分析方法。根据目前的研究进展,提出了三点建议。首先,EGBL的质量标志物研究有待加强。其次,应开发更多用于EGBL质量控制的生物测定方法。第三,有必要加强EGBL中原花青素的检测。图形摘要
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引用次数: 0
Development of UPLC-MS/MS methods for quantitation of glutathione, cysteine, 14,15-epoxyeicosatrienoic acid, and 15-hydroxyeicosatetraenoic acid and application in paraquat poisoning cells 谷胱甘肽、半胱氨酸、14,15-环氧二十碳三烯酸和15-羟基二十碳四烯酸的UPLC-MS/MS定量方法的建立及其在百草枯中毒细胞中的应用
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-06-15 DOI: 10.1080/10826076.2023.2223634
Cong-Rong Tang, Xingjie Zhu, Zheng Yu, Xiaofan Ke, Jianhui Yang, Zhongqiu Lu, Lufeng Hu
Abstract Glutathione (GSH) and cysteine are important antioxidants in maintaining the oxidation-reduction balance. 14,15-epoxyeicosatrienoic acid (14,15-EET) and 15-hydroxyeicosatetraenoic acid (15-HETE) are biological active compounds metabolized from arachidonic acid. To dynamically monitor GSH, cysteine, 14,15-EET, and 15-HETE, an ultra-high-performance liquid chromatography-mass spectrometry (UPLC-MS/MS) method was developed. The derivative GSH, cysteine, and underivatized 14,15-EET, 15-HETE were determined by electrospray ionization source with multiple reaction monitoring. The developed method was well validated and applied to monitor the extracellular concentration of GSH, cysteine, 14,15-EET, and 15-HETE in paraquat (PQ) poisoning LO2 cells. It was shown that the derivation of GSH and cysteine is complete and specific. There was a good linear relationship among GSH, cysteine, 14,15-EET, and 15-HETE. The relative standard deviations of precision and accuracy were all within 15%. After PQ poisoning, the extracellular concentrations of GSH and cysteine were increased at 72 h. 14,15-EET and 15-HETE started to increase at 24 h, earlier than GSH and cysteine. Irreversible pathological alterations appeared at 48 h. In conclusion, a fast and specific UPLC-MS/MS method for the determination of GSH, cysteine, 14,15-EET, and 15-HETE has been developed and validated. PQ induced the increase of 14,15-EET and 15-HETE earlier than that of GSH and cysteine in LO2 cells culture medium. Graphical Abstract
谷胱甘肽(GSH)和半胱氨酸是维持氧化还原平衡的重要抗氧化剂。14,15-环氧二碳四烯酸(14,15- eet)和15-羟基二碳四烯酸(15-HETE)是花生四烯酸代谢的生物活性化合物。为了动态监测GSH、半胱氨酸、14、15-EET和15-HETE,建立了超高效液相色谱-质谱(UPLC-MS/MS)方法。采用多反应监测的电喷雾电离源法测定衍生物GSH、半胱氨酸和未激活的14,15- eet、15-HETE。所建立的方法得到了很好的验证,并用于监测百草枯(PQ)中毒LO2细胞中GSH、半胱氨酸、14、15-EET和15-HETE的细胞外浓度。结果表明,谷胱甘肽和半胱氨酸的衍生是完整和特异性的。GSH、半胱氨酸、14、15-EET和15-HETE之间存在良好的线性关系。精密度和准确度的相对标准偏差均在15%以内。PQ中毒后72h细胞外谷胱甘肽和半胱氨酸浓度升高。14、15-EET和15-HETE在24 h开始升高,早于GSH和半胱氨酸。48 h出现不可逆的病理改变。综上所述,建立了一种快速、特异的UPLC-MS/MS测定GSH、半胱氨酸、14、15-EET和15-HETE的方法并进行了验证。PQ诱导LO2细胞培养液中14、15-EET和15-HETE的升高早于GSH和半胱氨酸的升高。图形抽象
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引用次数: 0
Comparative evaluation of solid-phase extraction and in-tube liquid-liquid extraction for the determination of Organophosphorus pesticides in the surface water from Medjerda River, Tunisia 固相萃取法和管内液-液萃取法测定突尼斯Medjerda河地表水中有机磷农药的比较评价
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-06-10 DOI: 10.1080/10826076.2023.2222301
Mouna Necibi, N. Mzoughi
Abstract In the present work, we develop, validate, and compare two extraction procedures (in-tube liquid-liquid extraction (ITLLE) and solid-phase extraction (SPE)). The parameters that influence extraction efficiency, the nature and volume of the extraction solvent, as well as the pH nature, were improved and a standard solution of Organophosphorus pesticides (OPPs) was used. Results indicated that SPE is clearly more successful than ITLLE extraction under optimum conditions. The validated method showed that this approach had good linearity, with correlation coefficients ranging from 0.991 to 0.998 and low detection and quantification limits of 0.01–0.03 ng L−1 and 0.03–0.9 ng L−1, respectively. Relative standard deviations were in the range of 0.2 and 1.2%, while extraction recoveries varied from 79 to 97%. The SPE was selected and, optimum recoveries for OPPs were obtained at pH 7, with 10 mL of ethyl acetate. The suggested approach was effectively applied to the analysis of water samples collected from the Medjerda River in two seasons. The average OPPs concentrations ranged from not detected (ND) to 17.5 ng L−1 during the dry season and from not detected ND to 13.1 ng L−1 during the wet season. The results demonstrate that none of the OPPs concentrations measured exceeded the regulatory limits. Graphical Abstract
摘要在本工作中,我们开发、验证并比较了两种提取方法(管内液-液萃取(ITLLE)和固相萃取(SPE))。改进了影响萃取效率的参数、萃取溶剂的性质和体积以及pH性质,并使用了有机磷农药的标准溶液。结果表明,在最佳条件下,SPE的提取效果明显优于ITLLE。经验证的方法表明,该方法具有良好的线性,相关系数在0.991至0.998之间,检测和定量限在0.01至0.03之间 ng L−1和0.03–0.9 ng L−1。相对标准偏差在0.2%至1.2%之间,而提取回收率在79%至97%之间。选择SPE,并在pH为7时获得OPP的最佳回收率,10 mL乙酸乙酯。所提出的方法有效地应用于两个季节从Medjerda河采集的水样的分析。OPPs的平均浓度范围从未检测到(ND)到17.5 ng L−1在旱季,从未检测到的ND到13.1 ng L−1。结果表明,所测得的OPP浓度均未超过监管限值。图形摘要
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引用次数: 0
Uncovering the Q-marker and potential mechanisms of Qishan Formula for lung cancer based on multi-technology 基于多技术的肺癌芪山方q标记物及其潜在机制研究
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-05-31 DOI: 10.1080/10826076.2023.2216765
Yutong Sui, Yanqun Yang, Jing Zhang, Ziwei Wang, Xue Geng, Jiakang Jiang
Abstract Qishan Formula (QSF) is mainly used to treat lung cancer and its side effects of radiotherapy and chemotherapy. Although the clinical efficacy of QSF has been recognized, its mechanism of action and active ingredients are still unclear. This study aims to explore the potential Q-Marker of QSF and reveal its anti-lung cancer mechanism. Firstly, the fingerprints of 10 batches of QSF were established, and the potential Q-markers were screened by chemometrics, then network pharmacology and molecular docking methods were used to explore its anti-lung cancer mechanism. Finally, the potential Q-markers were quantitatively by UPLC-QDA. The results showed that 48 common peaks were identified by the established fingerprint, and calycosin, ginsenoside Rg1, atractylenolide III, atractylenolide I and ginsenoside Rb1 were screened as potential Q-Markers of QSF by chemometrics. Network pharmacology and molecular docking found that the potential Q-Markers may regulate various signaling pathways through targets such as FOS, IL6, EGFR, ESR1, MAPK1, and MAPK3, and play a therapeutic role in lung cancer. Besides, the established UPLC-QDA can also perform quality control for Q-Markers of QSF. This study can provide academic ideas and lay a foundation for the comprehensive quality control and mechanism research of QSF and other compound preparation. Graphical Abstract
摘要岐山方主要用于治疗癌症及其放化疗副作用。尽管QSF的临床疗效已得到认可,但其作用机制和有效成分尚不清楚。本研究旨在探索QSF潜在的Q标记物,揭示其抗癌症的机制。首先建立了10批QSF的指纹图谱,通过化学计术筛选潜在的Q标志物,然后运用网络药理学和分子对接方法探讨其抗癌症的机制。最后,通过UPLC-QDA对潜在的Q标记物进行了定量分析。结果表明,所建立的指纹图谱共鉴定出48个共有峰,并通过化学计学筛选出calycosin、人参皂苷Rg1、苍术内酯III、苍术皂苷I和人参皂苷Rb1作为QSF的潜在Q标记。网络药理学和分子对接发现,潜在的Q标记物可以通过FOS、IL6、EGFR、ESR1、MAPK1和MAPK3等靶点调节各种信号通路,并在癌症中发挥治疗作用。此外,建立的UPLC-QDA还可以对QSF的Q标记进行质量控制。本研究可为QSF等复方制剂的综合质量控制和机理研究提供学术思路,奠定基础。图形摘要
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引用次数: 0
Holistic chemical characterization of Zaoren Anshen preparations based on HPLC fingerprint and multi-components quantification 基于高效液相色谱指纹图谱和多组分定量的皂仁安神制剂整体化学表征
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-03-16 DOI: 10.1080/10826076.2023.2206667
Man-Jiang Xie, Jie Wang, Chenguang Dong, P. Tu, Qingying Zhang
Abstract Based on HPLC fingerprint analysis and multi-components quantification, a simple, sensible, and reliable HPLC-UV method, capable of qualitatively and quantitatively characterizing the main chemical markers of all medicinal herbs of Zaoren Anshen (ZRAS) prescription by one injection, was firstly developed. Then, three different dosage forms of ZRAS preparations, i.e., capsule, granule, and oral liquid, were analyzed and compared systematically, indicating the similarity and difference in chemical markers of the three ZRAS preparations. The strategy of combining HPLC chemical fingerprint and multi-components quantification in one injection was rather practical, powerful and useful in characterizing the main chemical markers of ZRAS preparations, which was a benefit for holistic quality evaluation and control of ZRAS preparations. Moreover, the present results provide sound scientific data for further studies on the effective constituents and quality control of ZRAS preparations. GRAPHICAL ABSTRACT
摘要在高效液相色谱指纹图谱分析和多组分定量的基础上,首次建立了一种简便、灵敏、可靠的HPLC-UV方法,能够一次注射定性、定量地表征枣仁安神方所有药材的主要化学标志物。然后,对三种不同剂型的ZRAS制剂,即胶囊、颗粒剂和口服液进行了系统的分析和比较,表明三种ZRAS制剂在化学标志物上的相似性和差异性。将高效液相色谱化学指纹图谱和多组分定量相结合的策略在表征ZRAS制剂的主要化学标志物方面相当实用、有力和有用,有利于对ZRAS制剂进行全面质量评价和控制。此外,本研究结果为进一步研究ZRAS制剂的有效成分和质量控制提供了可靠的科学依据。图形摘要
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引用次数: 0
Differential compounds of licorice before and after honey roasted and anti-arrhythmia mechanism via LC-MS/MS and network pharmacology analysis LC-MS/MS和网络药理学分析蜂蜜烘烤前后甘草的差异化合物及其抗心律失常机制
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-03-16 DOI: 10.1080/10826076.2023.2202238
Lujie Lu, Wen-xin Wang, Peijun Sun, Shuwei Yan, Hui Chen, Xiao Liu, Jiajia Dong, Lihong Chen, T. Lu
Abstract Licorice is mainly used to treat cough in clinics. After being roasted with honey, licorice has a cardiac protective effect. Due to its different sources, the chemical components in licorice are also diverse. To distinguish the different compounds between three sources of raw licorice (RL) and between three sources of honey-roasted licorice (HRL), a UPLC-QTOF-MS/MS method was established. Eighteen batches of samples were analyzed which were derived from Glycyrrhiza uralensis Fisch., Glycyrrhiza inflata Bat., and Glycyrrhiza glabra L. In addition, the potential key pathways of HRL to anti-arrhythmia were explored by network pharmacology. Among the three sources of RL, 77 differential compounds were detected in the positive ion mode; and 62 differential compounds were detected in the negative ion mode, of which 21 differential compounds were detected in both ion modes. Twenty-nine differential compounds were identified before and after honey-roasted of G. uralensis Fisch., 51 and 17 differential compounds were identified in G. glabra L. and G. inflata Bat., receptively. The network pharmacological analysis predicted that Rap1, Ras, PI3K-Akt, and cAMP signaling pathway might be closely related to the anti-arrhythmia mechanism of HRL. This study provides a theoretical reference for the quality improvement and clinical application of licorice. Graphical Abstract
摘要甘草在临床上主要用于治疗咳嗽。甘草与蜂蜜一起烘烤后,具有心脏保护作用。由于来源不同,甘草中的化学成分也不同。为了区分三种原料甘草(RL)和三种蜂蜜炙甘草(HRL)之间的不同化合物,建立了UPLC-QTOF-MS/MS方法。对来自甘草的18批样品进行了分析。,甘草。,此外,通过网络药理学探讨了HRL抗心律失常的潜在关键途径。在RL的三种来源中,在正离子模式下检测到77种不同的化合物;在负离子模式下检测到62种差异化合物,其中在两种离子模式下都检测到21种差异化合物。在甘草蜜烤前后共鉴定出29个不同的化合物。,在G.glabra L.和G.inflata Bat.中鉴定出51个和17个不同的化合物。,接受。网络药理学分析预测Rap1、Ras、PI3K-Akt和cAMP信号通路可能与HRL的抗心律失常机制密切相关。本研究为甘草的质量改进和临床应用提供了理论参考。图形摘要
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引用次数: 0
A comprehensive review on QbD driven analytical procedures developed for the analysis of various drugs 全面回顾了QbD驱动的分析方法,用于分析各种药物
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-03-16 DOI: 10.1080/10826076.2023.2204238
Aggarapu Susmitha, G. Rajitha, Gireesh Kumar Eri
Abstract Quality has been a prime priority for the pharmaceutical sector with the development of recommendations by regulatory organizations like ICH. Concepts of ICH Q8 to Q10 are the foundation of the QbD methodology, a systematic approach to pharmaceutical development. Pharma industries have adopted the QbD approach to support product quality during manufacturing and to improve robust manufacturing processes. QbD adoption in analytical procedure development is AQbD, Analytical Quality by Design. It aids in reliable, economical analytical procedure development and also facilitates regulatory flexibility. This review illustrates the detailed aspects with relevant examples in each step of AQbD and DoE techniques applied to various analytical techniques for analytical procedure development for the determination of medicinal compounds. The overview of techniques created using AQbD contributes to the direction in this field of study. Visual Abstract
摘要随着ICH等监管组织制定建议,质量一直是制药行业的首要任务。ICH Q8至Q10的概念是QbD方法论的基础,这是一种系统的药物开发方法。制药行业采用了QbD方法来支持生产过程中的产品质量,并改进稳健的生产流程。分析程序开发中采用的QbD是AQbD,即设计分析质量。它有助于可靠、经济的分析程序开发,也有助于监管的灵活性。这篇综述阐述了AQbD和DoE技术应用于各种分析技术的各个步骤的详细方面和相关例子,用于药物化合物测定的分析程序开发。使用AQbD创建的技术概述有助于该研究领域的方向。视觉摘要
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引用次数: 0
Hydrophilic molecularly imprinted chitosan microspheres based on deep eutectic solvents for micro-solid phase extraction of catechin 基于深共晶溶剂的亲水分子印迹壳聚糖微球微固相萃取儿茶素
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2023-03-16 DOI: 10.1080/10826076.2023.2208201
Mengdi Yuan, Chenglin Zhong, K. Row, Guizhen Li
Abstract Hydrophilic molecularly imprinted chitosan microspheres (HMICS) were synthesized using deep eutectic solvents (DESs)-(3-aminopropyl) triethoxysilane (APTES) as co-functional monomer for the extraction of catechin from green tea with micro-solid phase extraction (micro-SPE). Various factors were studied to optimize the extraction condition during extraction process. The actual extraction amount under the optimal conditions (amount of adsorbent (20 mg), type and volume of washing (acetone, 1.2 mL) and eluting solvent (acetone/acetic acid, 1.0 mL), extraction time (30 min), extraction temperature (40 °C), and sample pH (4)) were obtained at 97.06 mg·g−1. The catechin recovery ranged with ranged with limit of detection (LOD) within 0.09–0.24 µg·mL−1, and limit of quantification (LOQ) within 0.18–0.28 µg·mL−1. From the experimental results in this system, the HMICS was proved to have higher extraction capacity, improving as a promising adsorbent for the extraction of catechin. GRAPHICAL ABSTRACT
摘要以深度共晶溶剂(DESs)-(3-氨基丙基)三乙氧基硅烷(APTES)为共官能单体,采用微固相萃取法(micro-SPE)从绿茶中提取儿茶素,合成了亲水性分子印迹壳聚糖微球(HMICS)。对提取过程中的各种因素进行了研究,优化了提取条件。最佳条件下的实际提取量(吸附剂(20 mg),洗涤的类型和体积(丙酮,1.2 mL)和洗脱溶剂(丙酮/乙酸,1.0 mL),提取时间(30 min),提取温度(40 °C),样品pH(4))在97.06时获得 儿茶素的回收率在0.09–0.24之间,检出限(LOD)在0.09至0.24之间 µg·mL−1,定量限(LOQ)在0.18–0.28之间 µg·mL−1。从该体系的实验结果来看,HMICS具有更高的萃取能力,是一种很有前途的儿茶素萃取吸附剂。图形摘要
{"title":"Hydrophilic molecularly imprinted chitosan microspheres based on deep eutectic solvents for micro-solid phase extraction of catechin","authors":"Mengdi Yuan, Chenglin Zhong, K. Row, Guizhen Li","doi":"10.1080/10826076.2023.2208201","DOIUrl":"https://doi.org/10.1080/10826076.2023.2208201","url":null,"abstract":"Abstract Hydrophilic molecularly imprinted chitosan microspheres (HMICS) were synthesized using deep eutectic solvents (DESs)-(3-aminopropyl) triethoxysilane (APTES) as co-functional monomer for the extraction of catechin from green tea with micro-solid phase extraction (micro-SPE). Various factors were studied to optimize the extraction condition during extraction process. The actual extraction amount under the optimal conditions (amount of adsorbent (20 mg), type and volume of washing (acetone, 1.2 mL) and eluting solvent (acetone/acetic acid, 1.0 mL), extraction time (30 min), extraction temperature (40 °C), and sample pH (4)) were obtained at 97.06 mg·g−1. The catechin recovery ranged with ranged with limit of detection (LOD) within 0.09–0.24 µg·mL−1, and limit of quantification (LOQ) within 0.18–0.28 µg·mL−1. From the experimental results in this system, the HMICS was proved to have higher extraction capacity, improving as a promising adsorbent for the extraction of catechin. GRAPHICAL ABSTRACT","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41786708","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}
引用次数: 0
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Journal of Liquid Chromatography & Related Technologies
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