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1.
Chirality ; 35(9): 636-644, 2023 09.
Artigo em Inglês | MEDLINE | ID: mdl-36951148

RESUMO

This study presents the development of three new chiral stationary phases. They are based on silica modified with peptides containing phenylalanine and proline. Successful analyses and characterizations were conducted using Fourier transform infrared spectra, elemental analysis, and thermogravimetric analysis. After this, the enantioselective performance of the three chiral peptide-based columns was evaluated. The evaluation used 11 racemic compounds under normal-phase high performance liquid chromatography mode. Optimized enantiomeric separation conditions were established. Under these conditions, the enantiomers of flurbiprofen and naproxen were successfully separated on CSP-1 column: the separation factor of these was 1.27 and 1.21, respectively. In addition, the reproducibility of the CSP-1 column was also investigated. The results of the investigation illustrated that the stationary phases have good reproducibility (RSD = 0.73%, n = 5).


Assuntos
Flurbiprofeno , Naproxeno , Estereoisomerismo , Reprodutibilidade dos Testes , Cromatografia Líquida de Alta Pressão/métodos
2.
J Sep Sci ; 46(19): e2300314, 2023 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-37485594

RESUMO

Compound Chinese medicine preparation is a complex multi-component system. The traditional methods such as physicochemical identification and quantification of several main index components cannot provide adequate quality evaluation for Compound Banlangen Granules. The objective of this work was to establish a characteristic degradation fingerprint of Compound Banlangen Granules polysaccharides, and the reference fingerprint was obtained from the model samples prepared using prescription medicinal herbs from different origins. The partial degradation products of Compound Banlangen Granules polysaccharides were profiled by capillary zone electrophoresis, and the quality difference of polysaccharides of these preparations was compared by cluster analysis and principal component analysis. It was found that the contents and the characteristic degradation fingerprints of the polysaccharides from 25 batches of Compound Banlangen Granules of 17 manufacturers were significantly different. The quality of Compound Banlangen Granules polysaccharides was evaluated by the characteristic degradation fingerprint tool with satisfactory results. The present method provides a reference for the quality control strategy development of polysaccharides in other compound Chinese medicine preparations.

3.
Bioorg Med Chem Lett ; 72: 128873, 2022 09 15.
Artigo em Inglês | MEDLINE | ID: mdl-35779827

RESUMO

A novel series of 2-(2- oxoethyl)pyrimidine-5-carboxamide derivatives were designed, synthesized and evaluated as acetylcholinesterase inhibitors (AChEIs) for the treatment of Alzheimer's disease (AD). Biological activity results demonstrated that compound 10q showed the best inhibitory activity against AChE (IC50 = 0.88 ± 0.78 µM), which was better than that of Huperzine-A, and its inhibitory effect on BuChE was weak (IC50 = 10.0 ± 1.30 µM), which indicated that compound 10q was a dominant AChE inhibitor. In addition, the result of molecular docking study displayed that 10q could simultaneously bind to CAS and PAS sites of AChE, which was consistent with the mixed inhibition mode shown by the enzymatic kinetics study of 10q. Furthermore, the molecular properties of the target compounds were predicted online using the molinspiration server and pkCSM, The results exhibited that compound 10q had drug-like properties that satisfied the Lipinski's rule of five. Based on the bioactivity and molecular properties, compound 10q for further development was valuable.


Assuntos
Doença de Alzheimer , Inibidores da Colinesterase , Acetilcolinesterase/metabolismo , Doença de Alzheimer/tratamento farmacológico , Desenho de Fármacos , Humanos , Simulação de Acoplamento Molecular , Pirimidinas/farmacologia , Relação Estrutura-Atividade
4.
J Sep Sci ; 44(24): 4412-4421, 2021 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-34687475

RESUMO

A solid-phase extraction cartridge was fabricated using diallyl isophthalate as the monomer with the addition of porous organic cage material via in situ free-radical polymerization in a stainless-steel column. The resulting monolithic adsorbent exhibited a relatively uniform porous structure, a high specific surface area of 113.98 m2 /g, and multiple functional chemical groups according to the characterization results. An online solid-phase extraction-high-performance liquid chromatography procedure was fabricated to extract and determine tussilagone from Farfarae Flos. The results show that the complex sample matrices can be removed in the solid-phase extraction procedure. Simultaneously, tussilagone can remain, which can be subsequently switched to an octadecylsilane bonded analytical column. The methodological validation showed that the correlation coefficient was 0.9999 with a linear range of 0.6-200.0 µg/mL, the limit of detection was 0.2 µg/mL, the limit of quantification was 0.6 µg/mL, accuracy was 100.3-100.6%, and relative standard deviation of precision was ≤1.9%. The present monolithic cartridge exhibits good reusability of not more than 100 times. The real sample of Farfarae Flos was determined with a tussilagone content of 0.74 mg/g.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Sesquiterpenos/análise , Extração em Fase Sólida/métodos , Limite de Detecção , Porosidade , Reprodutibilidade dos Testes , Sesquiterpenos/isolamento & purificação , Espectroscopia de Infravermelho com Transformada de Fourier
5.
Anal Biochem ; 591: 113555, 2020 02 15.
Artigo em Inglês | MEDLINE | ID: mdl-31874172

RESUMO

A cycloalkyl-based polymer monolithic column for solid-phase extraction was prepared via radical polymerization using cyclohexyl methacrylate as the monomer. The preparative conditions such as crosslinker/monomer ratio and the amount of the porogens were optimized and the resulting monoliths were characterized by scanning electron microscopy and nitrogen adsorption-desorption method. On-line solid-phase extraction-high-performance liquid chromatography was performed to quantitatively analyse polyphyllin I, II, VI and VII contained in herbal medicine of paridis rhizome in mouse plasma using the homemade optimized monolithic SPE column combined with a C18 column, in which water was used to remove the plasma matrix while the polyphyllins in the mouse plasma were eluted by acetonitrile-water (42:58, V/V). Results obtained from the method validation show that the present method is feasible for the quantitative analysis of the four polyphyllins in plasma. The developed method was further applied for the real mouse plasma sample. These results show that the homemade cycloalkyl-based polymer monolithic SPE column has good ability for clean-up of the interfering bio-matrix and simultaneously extracting the four polyphyllins from mouse plasma. Furthermore, the present method is a promising method for quantitative determination of saponins compounds from complex bio-samples with the advantages of simple and efficient.


Assuntos
Saponinas/sangue , Extração em Fase Sólida/métodos , Animais , Cicloparafinas/química , Diosgenina/análogos & derivados , Camundongos , Polímeros/química , Esteroides
6.
Bioorg Med Chem Lett ; 30(6): 126985, 2020 03 15.
Artigo em Inglês | MEDLINE | ID: mdl-32008906

RESUMO

A series of new 4-arylthiazole-2-amine derivatives as acetylcholinesterase inhibitors (AChEIs) were designed and synthesized, Furthermore, their inhibitory activities against acetylcholinesterase in vitro were tested by Ellman spectrophotometry, and the results of inhibitory activity test showed that most of them had a certain acetylcholinesterase inhibitory activity in vitro. Moreover, the IC50 value of compound 4f was to 0.66 µM, which was higher than that of Rivastigmine and Huperzine-A as reference compounds, and it had a weak inhibitory effect on butyrylcholinesterase. The potential binding mode of compound 4f with AChE was investigated by the molecular docking, and the results showed that 4f was strongly bound up with AChE with the optimal conformation, in addition, their binding energy reached -11.27 Kcal*mol-1. At last, in silico molecular property of the synthesized compounds were predicted by using Molinspiration online servers. It can be concluded that the lead AChEIs compound 4f presented satisfactory drug-like characteristics.


Assuntos
Acetilcolinesterase/metabolismo , Aminas/síntese química , Inibidores da Colinesterase/síntese química , Fármacos Neuroprotetores/síntese química , Tiazóis/química , Alcaloides/farmacologia , Alcaloides/normas , Aminas/farmacologia , Butirilcolinesterase/metabolismo , Inibidores da Colinesterase/farmacologia , Desenho de Fármacos , Humanos , Simulação de Acoplamento Molecular , Fármacos Neuroprotetores/farmacologia , Rivastigmina/farmacologia , Rivastigmina/normas , Sesquiterpenos/farmacologia , Sesquiterpenos/normas , Relação Estrutura-Atividade
7.
Anal Bioanal Chem ; 412(2): 473-480, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-31792597

RESUMO

A phenyl-based polymer monolithic column was prepared via free radical polymerization in a stainless steel column with the size of 4.6 mm i.d. × 50 mm, using ethylene glycol phenyl ether acrylate as the monomer. The resulting monolithic column shows high porosity of 73.42% and relative uniform pore structure, as characterized by mercury porosimetry and scanning electron microscopy, respectively. The optimized polymer monolith column was used for on-line solid-phase extraction prior to the reversed phase mode HPLC-UV analysis for the determination of dioscin in human plasma, using a COSMOSIL C18 column (4.6 mm × 150 mm, 4.5 µm). Water was used to wash non-retained components from the SPE sorbent, and methanol water (80:20, V/V) was used as the mobile phase for isocratic elution of dioscin. The maximum adsorbed quantity of dioscin to the SPE column is 6.79 mg/g, which is high enough for the quantitative analysis of dioscin in plasma, due to the low content of dioscin in plasma. The method was validated by assessing the linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and repeatability. The developed method was applied for the analysis of dioscin in plasma from a volunteer who had orally administered an aqueous extract of dioscorea nipponica rhizome, showing the method capable of detecting dioscin in the plasma. These results show that the developed method is a rapid method for on-line solid-phase extraction and determination of dioscin from plasma, exhibiting good selectivity with hydrogen bond interaction and hydrophobic interaction, good clean-up ability, cost-saving, and time-saving. Graphical abstract.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Diosgenina/análogos & derivados , Extração em Fase Sólida/métodos , Diosgenina/sangue , Diosgenina/normas , Humanos , Limite de Detecção , Padrões de Referência , Reprodutibilidade dos Testes , Extração em Fase Sólida/instrumentação
8.
J Sep Sci ; 41(9): 1923-1929, 2018 May.
Artigo em Inglês | MEDLINE | ID: mdl-29368444

RESUMO

An ionic-liquid-based polymer monolithic column was synthesized by free radical polymerization within the confines of a stainless-steel column (50 mm × 4.6 mm id). In the processes, ionic liquid and stearyl methacrylate were used as dual monomers, ethylene glycol dimethacrylate as the cross-linking agent, and polyethylene glycol 200 and isopropanol as co-porogens. Effects of the prepolymerization solution components on the properties of the resulting monoliths were studied in detail. Scanning electron microscopy, nitrogen adsorption-desorption measurements, and mercury intrusion porosimetry were used to investigate the morphology and pore size distribution of the prepared monoliths, which showed that the homemade ionic-liquid-based monolith column possessed a relatively uniform macropore structure with a total macropore specific surface area of 44.72 m2 /g. Compared to a non-ionic-liquid-based monolith prepared under the same conditions, the ionic-liquid-based monolith exhibited excellent selectivity and high performance for separating proteins from complex biosamples, such as egg white, snailase, bovine serum albumin digest solution, human plasma, etc., indicating promising applications in the fractionation and analysis of proteins from the complex biosamples in proteomics research.


Assuntos
Líquidos Iônicos/química , Polímeros/química , Proteínas/química , 2-Propanol/química , Adsorção , Animais , Celulase/química , Fracionamento Químico , Clara de Ovo/química , Glucuronidase/química , Humanos , Metacrilatos , Microscopia Eletrônica de Varredura , Complexos Multienzimáticos/química , Nitrogênio/química , Permeabilidade , Plasma/química , Poligalacturonase/química , Polimerização , Porosidade , Proteoma , Proteômica , Reprodutibilidade dos Testes , Soroalbumina Bovina/química
9.
Analyst ; 143(1): 280-288, 2017 Dec 18.
Artigo em Inglês | MEDLINE | ID: mdl-29184931

RESUMO

A double-functionalized polymer monolithic column was fabricated within the confines of a stainless-steel column (50 mm × 4.6 mm i.d.) via a facile method using iron porphyrin, ionic liquid (1-allyl-3-methylimidazolium chloride) and 1,10-decanediol dimethacrylate as tri-monomers; ethylene dimethacrylate as a crosslinker; polyethylene glycol 400 and N,N-dimethylformamide as co-porogens; benzoyl peroxide and N,N-dimethyl aniline as the redox initiation system. Results obtained from scanning electron microscopy, nitrogen adsorption-desorption, and mercury intrusion porosimetry confirmed the uniform pore structure and the pore size distribution of macro-pores. The home-made monolith was further characterized by elemental analysis to investigate the elemental composition of Fe supplied by iron porphyrin, confirming the synthetic process. The resulting optimized monolithic column was used as the stationary phase in high performance liquid chromatography for separating proteins, such as mixture of standard proteins, egg white, and human plasma, exhibiting good selectivity and high performance. It is worth noting that the home-made double-functionalized polymer monolithic column shows excellent selectivity for fractionation separation of human plasma proteins, and it is a promising separation tool for complex bio-samples in proteomic research.


Assuntos
Proteínas Sanguíneas/isolamento & purificação , Proteínas do Ovo/isolamento & purificação , Proteômica , Adsorção , Cromatografia Líquida de Alta Pressão , Clara de Ovo/química , Humanos , Microscopia Eletrônica de Varredura , Polímeros
10.
J Sep Sci ; 38(12): 2101-8, 2015 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-25864707

RESUMO

An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography.

11.
Anal Sci ; 40(2): 319-333, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38085445

RESUMO

In present work, a method for enrichment, purification, and content determination of oleanolic acid (OA) in medicinal plants was established based on on-line solid phase extraction (SPE). A metal organic frameworks-porous organic polymer monolith (MOF-POPM) was prepared with functionalized UiO-66-(OH)2 as monomer and was used as SPE column for online enrichment and purification of OA. The ratio of adsorbent, enriching and eluting solvent, mobile phase pH, and flow rate had been systematically investigated. Under the optimum conditions, the linear range of OA was 0.59-2500 µg/mL with r = 0.9996. The limit of detection (LOD) was 0.18 µg/mL and the limit of quantification (LOQ) was 0.59 µg/mL. The intra-day relative standard deviations (RSDs) and inter-day RSDs of retention time and peak area were less than 0.3% and 1.3%, respectively. The average recoveries of OA in medicinal plants samples ranged from 87.7 to 104.6%. The results demonstrated that the online system was reliable and accurate for enrichment, purification, and content determination of OA in medicinal plants.


Assuntos
Ácido Oleanólico , Plantas Medicinais , Cromatografia Líquida de Alta Pressão/métodos , Extração em Fase Sólida/métodos , Polímeros/química
12.
J Chromatogr A ; 1714: 464564, 2024 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-38071875

RESUMO

A monolithic adsorbent was designed aiming to the structure of osthole and columbianadin, and fabricated using diallyl phthalate as the monomer and ethylene dimethacrylate as the crosslinker with the addition of bamboo biochar, via polymerization reaction in a stainless-steel tube. The prepared composite adsorbent packed in the tube was used as a solid-phase extraction column for the extraction and determination of two coumarins (osthole and columbianadin) in Angelicae Pubescentis Radix, combing with a C18 analytical column through an HPLC instrument, which show excellent matrix-removal ability and good selectivity to osthole and columbianadin. Furthermore, the present adsorbent shows good applicability, which was used for the extraction of osthole from Duhuo Jisheng Pill. Compared to the commercial C18 and phenyl adsorbent, the present adsorbent own better selectivity and higher resolution. These results attributed to the enhanced specific surface area (141 m2/g) and enriched interaction sites of the resulting composite adsorbent, due to the doping of bamboo biochar, which can produce hydrogen bond, dipole-dipole, π-π and hydrophobic force interactions with the osthole and columbianadin. The methodology validation indicated that the present method showed good precision and good accuracy, and the composite adsorbent showed good preparative repeatability, which can be reused for no less than 100 times with the relative standard deviation ≤4.6 % (n = 100). The present work provided a simple and efficient method for the extraction and determination osthole and columbianadin from Angelicae Pubescentis Radix.


Assuntos
Carvão Vegetal , Sasa , Cumarínicos , Cromatografia Líquida de Alta Pressão/métodos
13.
Se Pu ; 42(5): 487-493, 2024 Apr 08.
Artigo em Zh | MEDLINE | ID: mdl-38736393

RESUMO

The pharmaceutical analysis course is a three-dimensional knowledge network that connects several courses to form a new comprehensive knowledge node involving a large knowledge system and flexible knowledge structure. In this course, the subject of chromatography covers a wide range of topics. However, because accurate content is challenging to present, the teaching effect of this subject is poor. In this work, we sought to achieve the educational purpose of establishing morality and cultivating talent, as well as the goal of training highly skilled professionals, by taking the teaching of chromatography in the pharmaceutical analysis course as an example of transforming scientific research results into teaching resources. The resources obtained are integrated into the teaching process to provide innovative and scientific research ideas to students with the aim of not only helping them understand and master technical knowledge but also exercise their ability to raise and solve problems. Furthermore, we expound on how to introduce scientific development frontiers and formulate scientific problems through curriculum design. We also describe how our strategy can promote the teaching effect and achieve teaching objectives. Based on the characteristics of rapid knowledge update and equal emphasis on theory and practice in pharmaceutical analysis, the course is designed by introducing new advances in scientific development, formulating scientific problems, and adopting question- and problem-based learning methods for teaching. The teaching effect is then evaluated through diversified assessment, student feedback, and self-evaluation. The results show that the transformation of scientific research results into teaching resources plays a significant role in stimulating students' interest in learning, improving students' ability to solve problems, and achieving curriculum objectives, all of which greatly improve the teaching effect.


Assuntos
Ensino , Cromatografia , Currículo , Humanos
14.
J Pharm Biomed Anal ; 240: 115947, 2024 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-38181557

RESUMO

Huangqi Liuyi Decoction, a famous classical Chinese prescription, shows significant curative effect on diabetes and its complications, in which calycosin-7-glucoside, liquiritin and glycyrrhizic acid are the main components that playing these mentioned pharmacological activity, under the synergistic action of various other ingredients in the decoction. However, there are significant differences in the content of active compounds in Chinese medicinal materials, which mainly due to origin, picking seasons, and processing methods. Hence, the accurate content of the glycosides is the prerequisite for ensuring the pharmacological efficacy. Aiming at establishing an efficient extraction and determination method for accurate quantitative analysis of calycosin-7-glucoside, liquiritin and glycyrrhizic acid in Huangqi Liuyi Decoction, an on line solid-phase extraction-high-performance liquid chromatography method was developed, using a homemade bio-based monolithic adsorbent. The bio-based adsorbent was prepared in a stainless steel tube, using bio-monomers of methyleugenol and S-allyl-L-cysteine, which effectively reduced the dependence of the polymer field on non-renewable fossil resources and reduced carbon emissions. Furthermore, the prepared adsorbent owned abundant chemical groups, which can produce interactions of hydrogen bond, dipole-dipole, π-π and hydrophobic force with the target glycosides, thus improving the specific recognition ability of the adsorbent. The experiments were carried out on an LC-3000 HPLC instrument with a six-way valve. Methodology validation indicates that the recovery is in the range of 97.0%-103.4% with the RSD in the range of 1.6%-4.0%, due to the specific selectivity of the bio-based monolithic adsorbent for these three glycosides, and good matrix-removal ability for Huangqi Liuyi decoction. The limit of detection is 0.17, 0.50 and 0.33 µg/mL for calycosin-7-glucoside, liquiritin and glycyrrhizic acid, respectively, and the limit of quantitation is 0.50, 1.50 and 1.00 µg/mL, respectively, with the linear range of 2-200 µg/mL for calycosin-7-glucoside, and 5-500 µg/mL for liquiritin and glycyrrhizic acid. The present work provided a simple and efficient method for the extraction and determination of glycosides in complex medicinal plants.


Assuntos
Astragalus propinquus , Medicamentos de Ervas Chinesas , Glicosídeos , Polímeros/análise , Ácido Glicirrízico , Medicamentos de Ervas Chinesas/química , Glucosídeos/análise , Cromatografia Líquida de Alta Pressão/métodos
15.
Artigo em Inglês | MEDLINE | ID: mdl-36863242

RESUMO

A monolithic solid-phase extraction (SPE) cartridge packed with a composite adsorbent was fabricated via polymerization using dodecene as the monomer with the porous organic cage (POC) material doped, combing with an analytical column through a high-performance liquid chromatography (HPLC) instrument, which was used for the online extraction and separation of 23-acetyl alismol C, atractylodes lactone II and atractylodes lactone III from Zexie Decoction. The POC-doped adsorbent shows porous structure with a relatively high specific surface area of 85.50 m2/g, which was obtained from the characterizations of a scanning electron microscope and an automatic surface area and porosity analyser. Efficient extraction and separation of three target terpenoids was achieved by an online SPE-HPLC method based on the POC-doped cartridge, which exhibits strong matrix-removal ability and good terpenoids-retention ability with a high adsorption capacity, due to the interactions of hydrogen bond and hydrophobicity between the terpenoids and the POC-doped adsorbent. Method validation shows good linearity (r ≥ 0.9998) of the regression equation, and high accuracy with the spiked recovery in the range of 99.2 %-100.8 % of the proposed method. Compared to the generally disposable adsorbent, this work fabricated a reusable monolithic cartridge, which can be used for at least 100 times, with the RSD based on the peak area of the three terpenoids less than 6.6 %.


Assuntos
Terpenos , Porosidade , Adsorção , Cromatografia Líquida de Alta Pressão , Ligação de Hidrogênio
16.
J Chromatogr Sci ; 61(6): 579-584, 2023 Jul 09.
Artigo em Inglês | MEDLINE | ID: mdl-35870202

RESUMO

A phenyl-based monolithic adsorbent was prepared in a 50-mm-long stainless steel tube, which was initiated by the redox system, using ethylene glycol phenyl ether acrylate as the monomer and ethylene glycol dimethacrylate as the crosslinker. The effects of monomer/crosslinker ratio and the porogens on the permeability and morphology of the resulting adsorbents were investigated, and the optimal adsorbent shows relatively uniform pore structure according to the characterizations of scanning electron microscopy and nitrogen adsorption-desorption method. The column that filled with the adsorbent was used as the solid-phase extraction (SPE) cartridge, exhibiting unique selectivity for the extraction of evodiamine from Euodia fructus (the fruits of Euodia rutaecarpa (Juss.)Benth.), which attributes to the interactions of π-π and hydrogen bonding between the adsorbent and evodiamine. Combined with a C18 analytical column via high-performance liquid chromatography (HPLC) system, an online SPE-HPLC method was established for extraction, enrichment and determination of evodiamine from Euodia fructus. Method validation demonstrates that the relative standard deviation of the precision is less than 0.66%, and the spiked recovery is in the range of 93.11-98.06%. Furthermore, it is worth noting that the prepared SPE cartridge can be reused for no less than 100 times. These results show that the developed method is simple and efficient for online extraction and enrichment of evodiamine from Euodia fructus.


Assuntos
Evodia , Cromatografia Líquida de Alta Pressão/métodos , Frutas , Extração em Fase Sólida/métodos
17.
J Pharm Biomed Anal ; 234: 115508, 2023 Sep 20.
Artigo em Inglês | MEDLINE | ID: mdl-37295190

RESUMO

Natural glycosides widely distributed in medicinal plants are valuable sources of therapeutic agents, showing various pharmacological effects. The separation and purification of natural glycosides are meaningful for their pharmacological research, which face with great challenges due to the complex of medicinal plants samples. In this work, two kinds of functional monolithic separation mediums A and S were fabricated and fully applied in the online extraction, separation and purification of active glycoside components from medicinal plants with a simple-procedure closed-loop mode. Chrysophanol glucoside and physcion glucoside were detected and separated from Rhei Radix et Rhizoma using separation medium A as a solid-phase extraction adsorbent. Rhapontin was isolated and purified from Rheum hotaoense C. Y. Cheng et Kao using separation medium S as the stationary phase of high-performance liquid chromatography. Compared to the reported literatures, high yield of 5.68, 1.20 and 4.76 mg g-1 of these three products were obtained with high purity. These two online closed-loop mode methods were carried out using high-performance liquid chromatography system, in which the sample injection, isolation and purification procedures are all online mode, and reduced loss compared to offline extraction and purification procedures, thus achieving high recovery and high purity.


Assuntos
Medicamentos de Ervas Chinesas , Plantas Medicinais , Rheum , Plantas Medicinais/química , Glicosídeos/análise , Medicamentos de Ervas Chinesas/química , Rizoma/química , Cromatografia Líquida de Alta Pressão/métodos , Glucosídeos/análise , Rheum/química
18.
J Pharm Biomed Anal ; 211: 114633, 2022 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-35124450

RESUMO

A composite monolithic column was prepared via polymerization in a 10-mm-long tube, using a porphyrin-based covalent organic framework (COF) as the co-monomer. The fabricated monolith exhibit good permeability, relatively uniform porous structure and high specific surface area, which was used as a guard column prior to an analytical column for the analysis of active components in medicinal plants with HPLC. Ten kinds of medicinal plants were used as the samples, in which sixteen target components were separated and analyzed, as well as the fingerprints of herb and herb couple. Compared to a generally used commercial VAST silica gel-C18 guard column, the homemade guard column shows good permeability with fast mass transfer, short analytical time and strong reusability with more than 100 injections, thus indicating the present monolith is an outstanding guard column prior to the C18 analytical column for the analysis of multiple active components in various medicinal plants.


Assuntos
Estruturas Metalorgânicas , Plantas Medicinais , Cromatografia Líquida de Alta Pressão/métodos , Estruturas Metalorgânicas/química , Plantas Medicinais/química , Polimerização , Porosidade
19.
Anal Methods ; 14(4): 401-409, 2022 01 27.
Artigo em Inglês | MEDLINE | ID: mdl-35006229

RESUMO

Herein, a poly(ionic liquid@MOF) composite monolithic column was prepared via in situ radical polymerization using ionic liquid (1-allyl-3-methylimidazolium hexafluorophosphate) and MOF (derivatized UIO66-2COOH) as copolymer monomers. The composite monolithic column was characterized via scanning electron microscopy (SEM), nitrogen adsorption-desorption isotherms and mercury intrusion porosimetry. Subsequently, the composite monolithic column combined with high performance liquid chromatography (HPLC) was used as a solid-phase extraction (SPE) absorbent for online purification and enrichment of tectochrysin in medicinal plants. The results indicated that the addition of the ionic liquid and MOF not only increased the surface area but also increased the adsorption capacity of the monolith for tectochrysin. The method showed good linearity in the concentration range of 0.01-500 µg mL-1. The calibration equation was y = 2154.6x - 8.3785 and the limit of detection (LOD, S/N = 3) and the limit of quantification (LOQ, S/N = 10) were 3.33 ng mL-1 and 10 ng mL-1, respectively. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.62%, the RSD of inter-column was less than 3.16%, and the recoveries ranged from 100.58% to 105.00%. Thus, results showed that this method is simple, accurate and convenient for the online enrichment and purification of tectochrysin from medicinal plants.


Assuntos
Líquidos Iônicos , Plantas Medicinais , Cromatografia Líquida de Alta Pressão/métodos , Flavonoides , Líquidos Iônicos/química , Extração em Fase Sólida/métodos
20.
J Pharm Anal ; 12(1): 96-103, 2022 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-35573883

RESUMO

In this study, a functionalized covalent-organic framework (COF) was first synthesized using porphyrin as the fabrication unit and showed an edge-curled, petal-like and well-ordered structure. The synthesized COF was then introduced to prepare porous organic polymer monolithic materials (POPMs). Two composite POPM/COF monolithic materials with rod shapes, referred to as sorbent A and sorbent B, were prepared in stainless steel tubes using different monomers. Sorbents A and B exhibited relatively uniform porous structures and enhanced specific surface areas of 153.14 m2/g and 80.01 m2/g, respectively. The prepared composite monoliths were used as in-tube solid-phase extraction (SPE) sorbents combined with HPLC for the on-line extraction and quantitative analytical systems. Indole alkaloids (from Catharanthus roseus G. Don and Uncaria rhynchophylla (Miq.) Miq. Ex Havil.) contained in mouse plasma were extracted and quantitatively analyzed using the online system. The two composite multifunctional monoliths showed excellent clean-up ability for complex biological matrices, as well as superior selectivity for target indole alkaloids. Method validation showed that the RSD values of the repeatability (n=6) were ≤ 3.46%, and the accuracy expressed by the spiked recoveries was in the ranges of 99.38%-100.91% and 96.39%-103.50% for vinca alkaloids and Uncaria alkaloids, respectively. Furthermore, sorbents A and B exhibited strong reusability, with RSD values ≤ 5.32%, which were based on the peak area of the corresponding alkaloids with more than 100 injections. These results indicate that the composite POPM/COF rod-shaped monoliths are promising media as SPE sorbents for extracting trace compounds in complex biological samples.

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