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Article in Chinese | WPRIM | ID: wpr-801717


Objective: To analysis and identify the chemical components in Trichosanthis Fructus by UPLC-LTQ-Orbitrap-MS. Method: Samples of Trichosanthis Fructus were extracted by ultrasonic with 70% methanol after smashing and sifting by 40 mesh sieve. Thermo ScientificTM DionexTM UltiMateTM 3000 Rapid Separation LC system performed UPLC separations with Waters HSS T3-C18(2.1 mm×100 mm,1.8 μm) column. The mobile phase was 0.1% formic acid water(A)-methanol(B) with a gradient elution. The volume flow was 0.3 mL ·min-1. A Thermo ScientificTM LTQ-Orbitrap mass spectrometer equipped with a ESI probe was employed. The samples were respectively scanned in MS1 and MS2 mode of positive and negative ions. According to the chromatographic peak separation,mass signal intensity,and the number of molecular ions in MS1 model,the extraction condition,chromatogram and mass spectrum parameters were optimized. The chemical compounds were identified by the accurate mass measurement of molecular ions and fragment ion and comparation with reference substance. Result: 91 chemical compositions in Trichosanthis Fructus were totally identified,including 14 amino acids,5 monoterpenoids,5 tetracyclic triterpenoids,1 pentacyclic triterpene,14 flavonoids, 17 organic acids,3 polysaccharides,7 nucleotides,7 alkaloids and nitrogen compounds,2 volatile components,1 phytosterol,5 other compositions. Conclusion: The established UPLC-LTQ-Orbitrap-MS method can be used to quickly analyze and identify the main chemical constituents of Trichosanthis Fructus. The chemical information concerning the constituents in Trichosanthis Fructus could be helpful to the quality control and further studies of Trichosanthis Fructus.

Article in Chinese | WPRIM | ID: wpr-337927


To investigate cytotoxic secondary metabolites of Micrococcus sp. R21, an actinomycete isolated from a deep-sea sediment (-6 310 m; 142 degrees 19. 9' E, 10 degrees 54. 6' N) of the Western Pacific Ocean, column chromatography was introduced over silica gel, ODS, and Sephadex LH-20. As a result, eight compounds were obtained. By mainly detailed analysis of the NMR data, their structures were elucidated as cyclo(4-hydroxy-L-Pro-L-leu) (1), cyclo(L-Pro-L-Gly) (2), cyclo( L-Pro-L-Ala) (3), cyclo( D-Pro-L-Leu) (4), N-β-acetyltryptamine (5), 2-hydroxybenzoic acid (6), and phenylacetic acid (7). Compound 1 exhibited weak cytotoxic activity against RAW264. 7 cells with IC50 value of 9.1 μmol x L(-1).

Animals , Biological Factors , Chemistry , Metabolism , Pharmacology , Cell Survival , Macrophages , Cell Biology , Magnetic Resonance Spectroscopy , Mass Spectrometry , Mice , Micrococcus , Chemistry , Genetics , Metabolism , Molecular Structure , Phylogeny , Seawater , Microbiology , Secondary Metabolism
Acta Pharmaceutica Sinica ; (12): 930-933, 2012.
Article in Chinese | WPRIM | ID: wpr-276220


The aim of the study is to establish a new method of quality evaluation and validate its feasibilities by the simultaneous quantitative assay of four lignanoids in Schisandra chinensis. A new quality evaluation method, quantitative analysis of multi-components by single marker (QAMS), was established and validated with Schisandra chinensis. Four main lignanoids, schisandrin, schisantherin A, deoxyschizandrin and gamma-schizandrin, were selected as analytes and schisandrin as internal reference substance to evaluate the quality. Their contents in 13 different batches of samples, collected from different bathes, were determined by both external standard method and QAMS. The method was evaluated by comparison of the quantitative results between external standard method and QAMS. No significant differences were found in the quantitative results of four lignanoids in 13 batches of S. chinensis determined by external standard method and QAMS. QAMS is feasible for determination of four lignanoids simultaneously when some authentic standard substances were unavailable, and the developed method can be used for quality control of S. chinensis.

Chromatography, High Pressure Liquid , Methods , Cyclooctanes , Dioxoles , Drugs, Chinese Herbal , Chemistry , Fruit , Chemistry , Lignans , Plants, Medicinal , Chemistry , Polycyclic Compounds , Quality Control , Schisandra , Chemistry
Article in Chinese | WPRIM | ID: wpr-271857


<p><b>OBJECTIVE</b>To evaluate the affection of crushing technology on quality. The dissolution of Pills of Six Herbs with Rehmunnia prepared by different crushing technology was determined by taking the dissolution of Paeonol as test marker.</p><p><b>METHOD</b>The Pills was prepared with the fine powder which was crushed by normal crusher or super fine crusher. The rotatory-basket method was used, and the cumulative dissolution percentage was determined by UV.</p><p><b>RESULT</b>Statistics indicated there was a significant difference in dissolution parameter (T50) between super fine crushing powder Pills and normal fine-crushing powder Pills (P < 0.01), and there was a difference in dissolution of different batches of Pills of Six Herbs with Rehmunnia prepared by the normal crush technique (P < 0.05).</p><p><b>CONCLUSION</b>The determination of dissolution of Pills of Six Herbs with Rehmunnia is necessary. In order to improve the quality of drugs, we should adopt the technique of super fine crushing in the preparation procedure.</p>

Acetophenones , Chemistry , Drug Combinations , Drugs, Chinese Herbal , Particle Size , Plants, Medicinal , Chemistry , Quality Control , Rehmannia , Chemistry , Solubility , Technology, Pharmaceutical , Methods