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Acta Pharmaceutica Sinica ; (12): 557-564, 2021.
Article in Chinese | WPRIM | ID: wpr-873776


A quantitative analytical method based on HPLC coupled with the charged aerosol detector (CAD) for quantitative analysis of multi-components with a single marker (QAMS) was established for simultaneous determinations of astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-O-β-D-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan in Astragalus membranaceus. The separation was performed on an Agilent SB-C18 (150 mm×4.6 mm, 3.5 μm), with gradient elution using the mobile phase consisting of 0.05% formic acid solution and 0.05% formic acid acetonitrile at the flow rate of 1.0 mL·min-1. The column temperature was 35 ℃, and the injection volume was 20 μL. For CAD, the drift tube temperature was at 50 ℃. The contents of six components in A. membranaceus were determined by both external standard method (ESM) and QAMS, and then were compared. The results showed that chromatographic peaks were separated well and the linear ranges of astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan were 0.113-2.250 mg·mL-1, 0.012-0.240 mg·mL-1, 0.004-0.080 mg·mL-1, 0.065-1.300 mg·mL-1, 0.005-0.100 mg·mL-1 and 0.007-0.150 mg·mL-1, respectively. The content ranges of astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan were 0.306-0.922 mg·g-1, 0.053-0.183 mg·g-1, 0.015-0.092 mg·g-1, 0.069-0.823 mg·g-1, 0-0.098 mg·g-1 and 0.020-0.107 mg·g-1 in 20 batches of A. membranaceus, respectively. Using astragaloside Ⅱ as an internal reference, the relative correlation factors of astragaloside Ⅰ, astragaloside Ⅳ, calycosin-7-O-β-D-glucoside, formononetin, and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan were calculated as 0.561, 0.835, 0.299, 0.796, and 0.799, respectively. The results were compared with those obtained by the external standard method to verify the feasibility, rationality and repeatability of QAMS method, and there was no significant difference in assay results between the two methods. In conclusion, the QAMS method is accurate and feasible, and could be used to determine the contents such as astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan, and it can be used for quality control of A. membranaceus.

Chinese Traditional and Herbal Drugs ; (24): 3078-3089, 2020.
Article in Chinese | WPRIM | ID: wpr-846404


Flavonoid glycosides (FGs) are secondary metabolites of many plants widely found in nature, and exhibit significant biological activities, such as anticancer, antioxidant and antimicrobial. According to the glycosidic bonds, FGs are divided into flavonoid O-glycosides and flavonoid C-glycosides. The main metabolic processes of FGs in vivo were specific hydrolysis in the gastrointestinal tract and glucuronidation in liver. Glucose, xylose, rhamnose and other glycosyl groups were hydrolyzed to produce secondary glycosides or aglycones in the gastrointestinal tract that were absorbed into blood, and then further glucuronidation and methylation metabolites are mainly produced by phase II metabolism in liver. This article reviews the metabolism in vivo and biotransformation in vitro of some typical natural flavonoid glycosides exited in Chinese materia medica (CMMs), such as flavonoid O-glycosides in Epimedii Folium, Glycyrrhizae Radix et Rhizoma, Scutellariae Radix, Citri Reticulatae Pericarpium, and Cirsii Japonici Herba, and flavonoid C-glycosides in Anemarrhenae Rhizoma and Puerariae Lobatae Radix. The investigation of the metabolisms of FGs in vivo is helpful for the clarification of the effective ingredients in CMMs, which will provide the basis for new drugs development based on metabolites in vivo.

China Journal of Chinese Materia Medica ; (24): 1857-1861, 2019.
Article in Chinese | WPRIM | ID: wpr-773156


The change of icariin( ICA) content in thirty-three samples of five Epimedium species listed in the Chinese Pharmacopoeia( 2015 edition),including E. brevicornu,E. sagittatum,E. pubescens,E. koreanum,and E. wushanense has been investigated in this study. The results indicated that the optimized process procedure was baking at 150 ℃ for 30 min,and 3'''-carbonyl-2″-β-L-quinovosyl icariin( CQICA) could not be translated into ICA and ICA could be converted under this heating process condition. ICA increased remarkably after the heating process by 1-3 times in E. brevicornu,E. wushanense and E. koreanum,and increased lightly in E. brevicornum and E. pubescens,while ICA slightly increased or decreased in E. sagittatum and E. wushanense.

Drugs, Chinese Herbal , Chemistry , Epimedium , Chemistry , Flavonoids , Hot Temperature , Phytochemicals , Specimen Handling
China Journal of Chinese Materia Medica ; (24): 3530-3536, 2017.
Article in Chinese | WPRIM | ID: wpr-335823


Sulfur-containing Anemarrhenae Rhizoma decoction pieces were prepared by using sulfur-fumigating procedure. The difference components before and after sulfur fumigation in Anemarrhenae Rhizoma were analyzed and on-line identified by UPLC-Q-TOF-MSE combined with UNIFI informatics platform, principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) respectively. As a result, 16 major differences components were identified, and among them, 9 components were mainly from sulfur-fumigated samples. The main chemical markers in sulfur-fumigated Anemarrhenae Rhizoma were identified as the sulfite derivatives newly produced after sulfur-fumigating. Meanwhile, UPLC-Q-TOF-MSE was used to find the main chemical marker anemarrhena saponin BⅡ sulfite (m/z 983). By using this method, a rapid screening method for sulfur-fumigated Anemarrhenae Rhizoma was established. This was a convenient and accurate detection method for sulfur dioxide residue, and it can be used as an effective assistant method to control the quality of Anemarrhenae Rhizoma. At the same time, it was the first time to identify sulfited derivatives of steroidal saponins, and screen the sulfur-fumigated Anemarrhenae Rhizoma.

China Journal of Chinese Materia Medica ; (24): 1146-1151, 2017.
Article in Chinese | WPRIM | ID: wpr-350211


To compare the differences of main components between in rhizoma and fibrous root of Trillium tschonoskii and T. kamtschaticum, a simple, accurate and reliable high performance liquid chromatography coupled with the charged aerosol detector (HPLC-CAD) method was developed and then successfully applied for simultaneous quantitative analysis of three compounds, including polyphyllin Ⅶ (T1),pennogenin 3-O-α-L-rhamnopyranosyl-(1→2) [α-L-rhamnopyranosyl-(1→4)]-β-D-glucopyranoside (T2),polyphyllin Ⅵ (T3), in 16 batches of rhizome and 14 batches of fibrous root. The analytes were well separated from other constituents on TSK gel ODS (4.6 mm×250 mm, 5 μm) with acetonitrile-water (43∶57) at a flow rate of 1.0 mL•min⁻¹. The injection volume was 20 μL. The nitrogen inlet pressure for the CAD system was 35 psi and the nebulizer chamber temperature was 35 ℃.The method was validated for linearity (r>0.999 0), intra and inter-day precision (0.29%-3.0%), repeatability (0.45%-1.4%), stability (1.9%-2.6%), recovery (100.1%-100.2%, 1.2%-1.8%), limits of detection (0.002 g•L⁻¹), and limits of quantification (0.005 g•L⁻¹).The obtained datasets were processed by principal component analysis (PCA) and it showed that there was almost no difference in rhizoma of T. tschonoskii and T. kamtschaticum from different areas of China. However, the 3 major compounds existed in rhizoma were different from those in fibrous root of T. tschonoskii and T. kamtschaticum.

Acta Pharmaceutica Sinica ; (12): 456-461, 2017.
Article in Chinese | WPRIM | ID: wpr-779614


A new method was developed for the chromatographic fingerprint analysis of Toosendan Fructus by HPLC coupled with the charged aerosol detector (CAD) in the present study. Samples were well separated on an Agilent ZOBAX SB C18 column (4.6 mm×250 mm, 5 μm) by gradient elution using acetonitrile and water containing 0.1% formic acid (v/v) at the flow rate of 1.0 mL·min-1. The column temperature was 30℃ and the injection volume was 5 μL. The nitrogen inlet pressure of the charged aerosol detector (CAD) was 35 psi, and the nebulizer chamber temperature was 35℃. In addition, the method of the chromatographic fingerprints combined with multivariate statistical analysis was effective and reasonable lead to an accurate classification of 20 batches of samples from different locations. The results showed that 28 common peaks were observed in the fingerprint and the samples were classified into three clusters. The established method was well validated, and showed high precision, good repeatability, and satisfactory stability. It may serve in the quality control and evaluation of Toosendan Fructus.