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

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.

Recent advances in Scutellariae radix: A comprehensive review on ethnobotanical uses, processing, phytochemistry, pharmacological effects, quality control and influence factors of biosynthesis.

Background: Scutellariae radix (SR) is the dried root of Scutellaria baicalensis Georgi. It has a long history of ethnic medicinal use, traditionally recognized for its efficacy in clearing heat， drying dampness, eliminating fire， removing toxins , stopping bleeding and tranquilizing fetus to prevent miscarriage. Clinically, it is used to treat cold, fever, migraine, hand-foot-and-mouth diseases, liver cancer and inflammatory diseases. Purpose: The review aims to provide a comprehensive reference on the ethnobotanical uses, processing, phytochemistry, pharmacological effect, quality control and influence factors of biosynthesis for a deeper understanding of SR. Results and conclusion: A total of 210 isolated components have been reported in the literature, including flavonoids and their glycosides, phenylpropanoids, phenylethanoid glycosides, phenolic acids, volatile components, polysaccharides and others. The extract of SR and its main flavonoids such as baicalin, baicalein, wogonin, wogonoside, and scutellarin showed antioxidant, anti-inflammatory, anti-tumor, antiviral, hepatoprotective, and neuroprotective effects. However, further studies are required to elucidate its mechanisms of action and clinical applications. The pharmacodynamic evaluation based on traditional efficacy should be conducted. Although various analytical methods have been established for the quality control of SR, there are gaps in the research regarding efficacy-related quality markers and the development of quality control standards for its processed products. The regulatory mechanisms of flavonoids biosynthesis remain to be explored while the influence of environmental and transcription factors on the biosynthesis have been studied. In conclusion, SR is a promising herbal medicine with significant potential for future development.

Traditional uses, phytochemistry, pharmacology, quality control and clinical studies of Cimicifugae Rhizoma: a comprehensive review.

Cimicifugae Rhizoma, generally known as "Sheng Ma" in China, has great medicinal and dietary values. Cimicifugae Rhizoma is the dried rhizome of Cimicifuga foetida L., Cimicifuga dahurica (Turcz.) Maxim. and Cimicifuga heracleifolia Kom., which has been used to treat wind-heat headache, tooth pain, aphtha, sore throat, prolapse of anus and uterine prolapse in traditional Chinese medicine. This review systematically presents the traditional uses, phytochemistry, pharmacology, clinical studies, quality control and toxicity of Cimicifugae Rhizoma in order to propose scientific evidence for its rational utilization and product development. Herein, 348 compounds isolated or identified from the herb are summarized in this review, mainly including triterpenoid saponins, phenylpropanoids, chromones, alkaloids, terpenoids and flavonoids. The crude extracts and its constituents had various pharmacological properties such as anti-inflammatory, antitumor, antiviral, antioxidant, neuroprotective, anti-osteoporosis and relieving menopausal symptoms. The recent research progress of Cimicifugae Rhizoma in ethnopharmacology, phytochemistry and pharmacological effects demonstrates the effectiveness of its utilization and supplies valuable guidance for further research. This review will provide a basis for the future development and utilization of Cimicifugae Rhizoma.

Pharmacokinetic Study of Safrole and Methyl Eugenol after Oral Administration of the Essential Oil Extracts of Asarum in Rats by GC-MS.

Asarum is a traditional medicine and has been widely used as remedies for inflammatory diseases, toothache, headache, local anesthesia, and aphthous stomatitis in China, Japan, and Korea. Our previous research found that safrole and methyl eugenol were vital compounds that contribute to distinguish the different species and raw Asarum and its processed products apart. The pharmacokinetics of safrole and methyl eugenol after oral administration of Asarum extract has not been reported yet. In this study, a rapid and simple gas chromatography-mass spectroscopy (GC-MS) method that has a complete run time of only 4.5 min was developed and validated for the simultaneous determination and pharmacokinetic study of safrole and methyl eugenol in rat plasma after administration of Asarum extracts. The chromatographic separation was realized on a DB-17 column (30 m × 0.25 mm × 0.25 µm). And detection was carried out under selected ion monitoring (SIM) mode. Plasma samples were pretreated by n-hexane. The pharmacokinetic parameters provided by this study will be beneficial for further developments and clinical applications of Asarum.

Direct on-line analysis of neutral analytes by dual sweeping via complexation and organic solvent field enhancement in nonionic MEKC.

Conventionally, neutral compounds cannot be separated by nonionic micelle capillary electrophoresis. In this report, the development of a novel on-line preconcentration technique combining dual sweeping based on complexation and organic solvent field enhancement is applied to the sensitive and selective analysis of three neutral glucosides: ginsenoside Rf, ginsenoside Rg1, and ginsenoside Re. Nonionic micelle detectability by CE is demonstrated through effective focusing of large sample volumes (up to 38% capillary length) using a dual sweeping mode. This results in a 50- to 130-fold improvement in the LODs relative to conventional injection method. Neutral compounds sweeping is examined in terms of analyte mobility dependence on borate complexation, solvent viscosity difference, and Brij-35 interaction. Enhanced focusing performance by this hyphenated method was demonstrated by a greater than fourfold reduction in glucoside bandwidth, as compared with common sweeping (devoid of organic solvent-mediated sweeping method in the sample matrices). Moreover, separation efficiencies greater than a million theoretical plates can be achieved by sweeping large sample volumes into narrow zones. The designated method was also tested for its ability to determine the presence of glucosides in the crude extracts obtained from plant sample.

Non-ionic detergent Triton X-114 Based vortex- synchronized matrix solid-phase dispersion method for the simultaneous determination of six compounds with various polarities from Forsythiae Fructus by ultra high-performance liquid chromatography.

A simple nonionic detergent - based vortex- synchronized matrix solid-phase dispersion (ND-VSMSPD) method was developed to extract bioactive compounds in Forsythiae Fructus coupled with ultra high-performance liquid chromatography (UHPLC). Nonionic detergent Triton 114 was firstly used as a green elution reagent in vortex- synchronized MSPD procedure. The optimum parameters were investigated to attain the best results, including Florisil as sorbent, 2mL 10% (v/v) nonionic detergent Triton X-114 as the elution reagent, 1:1 of sample/sorbent ratio, grinding for 3min, and whirling for 2min. The recoveries of the six compounds in Forsythiae Fructus were in the range of 95-104% (RSD <4.6%) and the method displayed a good linearity within the range of 0.08-20µgmL-1 for caffeic acid, 0.6-150µgmL-1 for forsythoside A, 0.4-100µgmL-1 phillyrin, 0.2-50µgmL-1 for quercetin, isorhamnetin and arctigenin (r≥0.999). It was proved that the extraction yields of almost all compounds attained by the established vortex- synchronized MSPD, which required lower sample, reagent and time, were higher than the normal MSPD and the traditional ultrasonic-assisted extraction. Consequently, this developed vortex- synchronized MSPD coupled with simple UHPLC method could be efficiently applies to extract and analyze the target compounds in real Forsythiae Fructus samples.