scholarly journals Combined Use of Deep Eutectic Solvents, Macroporous Resins, and Preparative Liquid Chromatography for the Isolation and Purification of Flavonoids and 20-Hydroxyecdysone from Chenopodium quinoa Willd

Biomolecules ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 776 ◽  
Author(s):  
Jia Zeng ◽  
Xianchao Shang ◽  
Peng Zhang ◽  
Hongwei Wang ◽  
Yanlong Gu ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Choline Chloride ◽  
Chenopodium Quinoa ◽  
Deep Eutectic Solvents ◽  
Preparative Hplc ◽  
Spectroscopic Techniques ◽  
Preparative Scale ◽  
Isolation And Purification ◽  
Macroporous Resins

Deep eutectic solvents (DESs) were used in combination with macroporous resins to isolate and purify flavonoids and 20-hydroxyecdysone from Chenopodium quinoa Willd by preparative high-performance liquid chromatography (HPLC). The extraction performances of six DESs and the adsorption/desorption performances of five resins (AB-8, D101, HPD 400, HPD 600, and NKA-9) were investigated using the total flavonoid and 20-hydroxyecdysone extraction yields as the evaluation criteria, and the best-performing DES (choline chloride/urea, DES-6) and macroporous resin (D101) were further employed for phytochemical extraction and DES removal, respectively. The purified extract was subjected to preparative HPLC, and the five collected fractions were purified in a successive round of preparative HPLC to isolate three flavonoids and 20-hydroxyecdysone, which were identified by spectroscopic techniques. The use of a DES in this study significantly facilitated the preparative-scale isolation and purification of polar phytochemicals from complex plant systems.

scholarly journals Identification and Quantification of an Adulterant in a Dietary Supplement Marketed for Sexual Enhancement

2018 ◽  
Vol 1 (4) ◽  
pp. 25-33 ◽  
Author(s):  
Flavia Redko ◽  
Sabrina Flor ◽  
Silvia Lucangioli ◽  
Jerónimo Ulloa ◽  
Rafael Ricco ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Spectroscopic Techniques ◽  
Easy Method ◽  
Isolation And Purification ◽  
Chromatography Analysis ◽  
Pharmaceutical Ingredients ◽  
Emerging Risk ◽  
The Mean ◽  
Layer Chromatography

In recent years, the consumption of dietary supplements (DS) has increased worldwide. In Argentina, approximately 14 million DS units were sold between 2015 and 2017. The adulteration of DS with active pharmaceutical ingredients or their analogues has been reported. This represents an alarming emerging risk to public health. The aim of this work was to detect the possible adulteration of a DS marketed in Argentina for the treatment of erectile dysfunction. Initially, thin layer chromatography analysis of the DS capsules content suggested the presence of a major compound. For the isolation and purification of this compound, an easy method consisted of a liquid-liquid extraction (water/CH2Cl2) followed by re-crystallisation from ethanol, is reported. Spectroscopic techniques such as mono- and bidimensional nuclear magnetic resonance, Fourier transform infrared spectroscopy and mass spectrometry allowed its identification as tadalafil. A rapid and reliable method was developed for the quantification of tadalafil in this DS by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). The mean content of tadalafil per capsule was 21.2 mg which represents a slightly higher value than that found in approved products in Argentina (5 or 20 mg per tablet). In addition, an undeclared alga was identified in the DS by microscopic techniques.

scholarly journals Natural Deep Eutectic Solvents for Simultaneous Extraction of Multi-Bioactive Components from Jinqi Jiangtang Preparations

Pharmaceutics ◽  
2019 ◽  
Vol 11 (1) ◽  
pp. 18 ◽  
Author(s):  
Lele Yang ◽  
Ling Li ◽  
Hao Hu ◽  
Jianbo Wan ◽  
Peng Li
Keyword(s):  
High Performance ◽  
Choline Chloride ◽  
Deep Eutectic Solvents ◽  
Bioactive Components ◽  
Operational Parameters ◽  
Ultrasound Assisted Extraction ◽  
Assisted Extraction ◽  
Natural Deep Eutectic Solvents ◽  
Quantification Analysis ◽  
Chemical Profiles

Natural deep eutectic solvents (NADESs), composed of natural primary metabolites, are now widely used as green and sustainable extraction solvents of bioactive components. In the present study, various NADESs were prepared to extract multi-components from different preparations of an herbal formula (Chinese name: Jinqi Jiangtang, JQJT) using ultrasound-assisted extraction (UAE). Results showed that most prepared NADESs provided more effective extraction of phenolic acids and alkaloids from JQJT preparations than conventional solvents. Among the tested NADESs, the solvent formed by choline chloride and laevulinic acid was selected to optimize the operational parameters using response surface methodology. The optimized extraction method was successfully applied to extract six major components in four commercial JQJT products, and quantification analysis was performed by the validated high-performance liquid chromatography with ultraviolet detection (HPLC-UV) method. The quantitative results indicated that preparations from different manufacturers showed different chemical profiles. In conclusion, NADESs-based UAE shows considerable potential as an efficient and green method for extraction of multi-bioactive components from commercial herbal preparations.

High Performance Liquid Chromatography Coupled with Radioactivity Detection: A Powerful Tool for Determining Drug Metabolite Profiles in Biological Fluids

1986 ◽  
Vol 41 (1-2) ◽  
pp. 115-125 ◽  
Author(s):  
K.-O. Vollmer ◽  
W. Klemisch ◽  
A. von Hodenberg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Isolation And Purification ◽  
Carbon 14 ◽  
Tracer Techniques ◽  
Metabolite Profiles

Abstract High performance liquid chromatography coupled with continuous radioactivity detection rep­resents an advancement in drug metabolism research. Using radioactive substances labelled in biologically stable positions, all metabolites can be specifically detected by radioactivity measure­ment. Thus no clean-up of biological fluids is required prior to HPLC. This can prevent artefact formation from unstable metabolites, reduces recovery problems and facilitates quantitation. Separation of highly polar and unpolar metabolites is possible in a single chromatographic run using gradient elution and reversed phase materials. This technique is also well-suited for prepara­tive isolation and purification of metabolites for subsequent structure elucidation. Various metabolite profiles of drugs labelled with carbon-14 or tritium are shown. Metabolites of the following drugs are presented: norfenefrine, etozolin, thymoxamine, naloxone, and levobunolol. We review the general methodology and report our experience with this technique. In principle, this technique may be useful for all biological systems in which tracer techniques are applied.

scholarly journals Separation and Enrichment of Three Coumarins from Angelicae Pubescentis Radix by Macroporous Resin with Preparative HPLC and Evaluation of Their Anti-Inflammatory Activity

Molecules ◽  
2019 ◽  
Vol 24 (14) ◽  
pp. 2664 ◽  
Author(s):  
Yuqiao Yang ◽  
Ruichao Zhu ◽  
Jin Li ◽  
Xuejing Yang ◽  
Jun He ◽  
...  
Keyword(s):  
High Performance ◽  
Pharmaceutical Products ◽  
Raw 264.7 Cells ◽  
Preparative Hplc ◽  
Scale Separation ◽  
Adsorption Dynamics ◽  
Adsorption And Desorption ◽  
Macroporous Resins ◽  
Pseudo Second Order ◽  
Anti Inflammatory

In order to enrich and separate three coumarins (columbianetin acetate, osthole and columbianadin) from Angelicae Pubescentis Radix (APR), an efficient method was established by combining macroporous resins (MARs) with preparative high-performance liquid chromatography (PHPLC). Five different macroporous resins (D101, AB-8, DA-201, HP-20 and GDX-201) were used to assess the adsorption and desorption characteristics of three coumarins. The result demonstrated that HP-20 resin possessed the best adsorption and desorption capacities for these three coumarins. Moreover, the adsorption dynamics profiles of three coumarins were well fitted to the pseudo second order equation (R2 > 0.99) for the HP-20 resin. The adsorption process was described by the three isotherms models including Langmuir (R2 > 0.98, 0.046 ≤ RL ≤ 0.103), Freundlich (R2 > 0.99, 0.2748 ≤ 1/n ≤ 0.3103) and Dubinin Radushkevich (R2 > 0.97). The contents of columbianetin acetate, osthole and columbianadin in the product were increased 10.69-fold, 19.98-fold and 19.68-fold after enrichment, respectively. Three coumarins were further purified by PHPLC and the purities of them reached above 98%. Additionally, the anti-inflammatory effects of these three coumarins were assessed by Lipopolysaccharide (LPS)-induced RAW 264.7 cells. It was found that the production of NO and MCP-1 was obviously inhibited by three coumarins. Columbianetin acetate, osthole and columbianadin could be used as potentially natural anti-inflammatory ingredients in pharmaceutical products. It was concluded that the new method combining MARs with PHPLC was efficient and economical for enlarging scale separation and enrichment of columbianetin acetate, osthole and columbianadin with anti-inflammatory effect from the APR extract.

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