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A high performance liquid chromatography with a diode array detector combined with electrospray ionization ion trap time-of-flight multistage mass spectrometry(HPLC-DAD-ESI-IT-TOF-MS~n, HPLC-MS~n) method was established for qualitative analysis of the chemical components of ethyl acetate extract from Sinopodophylli Fructus. The analysis was performed on a Kromasil 100-5 C_(18)(4.6 mm×250 mm, 5 μm) column, with a mobile phase consisted of 0.1% formic acid(A) and acetonitrile(B) for gradient at a flow rate of 1.0 mL·min~(-1). Electrospray ionization ion trap time-of-flight multistage mass spectrometry was applied for qualitative analysis under positive and negative ion modes. With use of reference substance, characteristic fragmentation and their HR-MS data, 102 components were identified, including 67 flavonoids and 35 lignans. Among them, 45 compounds were reported in Sinopodophylli Fructus for the first time and 19 compounds were identified as new compounds. PharmMapper was used to predict the bioactivity of compounds that were first reported in Sinopodophylli Fructus, and 20 compounds of them were identified to have potential anticancer activity. The results showed that there were many isomers in the ethyl acetate extract of Folium Nelumbinis, and a total of 19 groups of isomers were found. Among them, C_(21)H_(20)O_8 had the highest number of isomers(18 compounds), all of which were α-peltatin or its isomers; C_(21)H_(20)O_7 ranked second, with 10 compounds, all of which were 8-prenylquercetin-3-methyl ether or its isomers. In conclusion, an HPLC-MS~n method was established for qualitative analysis of the ethyl acetate extract(with anti-breast cancer activity) from Sinopodophylli Fructus in this study, which will provide the evidence for clarifying pharmacological active ingredients of the ethyl acetate extract from Sinopodophylli Fructus against breast cancer.
Subject(s)
Acetates , Chromatography, High Pressure Liquid , Fruit , Spectrometry, Mass, Electrospray IonizationABSTRACT
OBJECTIVE: To evaluate the effectiveness and safety of Asarum insigne Diels and develop a sensitive, accurate, and efficient ultra-fast liquid chromatography coupled with triple quadrupole mass spectrometer (UFLC-MS/MS) method for simultaneous quantification of five compounds. METHODS: Chromatographic separation was performed on a Shimadzu shim-pack XR-ODS III column(2.0 mm×75 mm,1.6 μm). The mobile phase was composed of 0.1% aqueous formic acid and methanol and the flow rate was 0.2 mL•min-1. Using the established method, all components could be easily separated within 14 min. All components were detected in multiple reaction monitor mode after positive atmospheric pressure chemical ionization. RESULTS: The method was validated, and had good precision, linearity, lower limit of detection, lower limit of quantification, recovery, and stability. This method was used to determine and compare the contents of five components in different medicinal parts of 11 samples, and the contents of 3,4,5-trimethoxytoluene, 3,5-dimethoxytoluene, methyleugenol in different medicinal parts of Asarum insigne were reported for the first time, which (in ng•mg-1) were as follows: 3,4,5-trimethoxytoluene: 1.5-16.71; 3,5-dimethoxytoluene: 28.59-177.20; methyleugenol: 2.46-22.48; AL-I: 46.39-324.04; 7-OCH3-AL-IV: 12.95-251.04. The content of 7-OCH3-AL-IV and total contents of two aristololactams in roots were lower than those in leaves or flower parts, and the contents of AL-I in flowers (171.9-324.0 ng•mg-1) were higher than those in roots (78.44-124.56 ng•mg-1). For methyleugenol, the contents in roots were lower than those in the other parts. CONCLUSION: It is recommended to remove the leaves, flowers, and rhizomes when using Asarum insigne and use it with extreme caution. The UFLC-MS/MS method established in this study can provide guidance for the quality evaluation and safe clinical use of traditional Chinese medicine derived from Asarum insigne.
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Objective To perform qualitative and quantitative analysis on the volatile components in roots, rhizomes, leaves, and flowers of Asari Radix et Rhizoma derived from Asarum insigne. Methods The volatile components were analyzed by HS-GC-MS, and the relative percentage content of each component was calculated with peak area normalization method. Results There were 58 components separated from four parts of A. insigne, including 27 common components in different parts. The principal constituents was trans-β-farnesene, safrole, and asaricin. Their contents were different in four parts. Especially the contents of safrole in rhizomes, leaves, and flowers were up to 34%, 22%, and 21%; The safrole in rhizomes was over twice higher than that in roots (12%). Because safrole was extremely poisonous, the rhizomes, leaves, and flowers should be used carefully. Conclusion The volatile components in A. insigne can be detected by HS-GC-MS simply and quickly. The research can be helpful for development and quality evaluation of A. insigne.
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To a certain extent, the drug effect is determined by its blood concentration. It is generally accepted that the blood concentrations of constituents of Chinese medicines are very low. There is no sufficient experimental bases and references on its degree and the possibility of taking effect. In this study, 69 papers were collected and analyzed by searching the database of Scifinder, Pubmed, CNKI. The minimum effective blood concentrations of 73 common Western medicines and the maximum blood concentrations of 211 in vivo constituents of 40 Chinese medicines (single herb or compound Chinese medicine) were summarized. It was found that the maximum blood concentrations of the most in vivo constituents of Chinese medicines were much less than the minimum effective blood concentrations of the Western medicines. Specifically, the minimum effective blood concentrations of 17 Western medicines (23% of total) and the maximum blood concentrations of the 143 in vivo constituents of Chinese medicines (68% of total) were less than 100 ng ·mL-1; the minimum effective blood concentrations of 31 Western medicines (42% of total) and the maximum blood concentrations of the 20 in vivo constituents of Chinese medicines (9% of total) were more than 1 000 ng·mL-1. In this paper, a systematic summary and comparison of the blood concentrations in traditional Chinese medicines and Western medicines were conducted, which could provide a new ideas and references for the study of the pharmacodynamical material basis and its mechanism in traditional Chinese medicine.
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OBJECTIVE: To study the HPLC fingerprint of Swertia patens, the most commonly used substitute of Swertiae Mileensis Herba recorded in Chinese Pharmacopoeia, compare the major chemical constituents between the two kinds of herbs, and provide scientific evidence for their identification and quality control. METHODS: HPLC fingerprint method was used to analyze 12 batches of S. patens and 5 batches of Swertiae Mileensis Herba. Similarity evaluation method and clustering analysis method were introduced to compare the HPLC chromatograms of them. RESULTS: The repetition, stability, and precision of the fingerprint method were good. A total of 13 common peaks were confirmed. The similarities of the chromatograms of 17 batches of Swertia were greater than 0.94. CONCLUSION: Different batches of S. patens and Swertiae Mileensis Herba have high similarity. It is possible for S. patens to take place of Swertiae Mileensis Herba.
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<p><b>OBJECTIVE</b>To explore the character of inorganic elements in Asari Radix et Rhizoma (Xixin).</p><p><b>METHOD</b>The contents of 53 inorganic elements in Xixin samples from different localities and species were determined by ICP-AES and ICP-MS. The statistical data were made using SAS.</p><p><b>RESULT</b>The result demonstrated that Xixin has the high contents of Fe, Cr, Li. It has been observed that the content of Cu and Pb of the samples are much higher than the standard level. The results of hierarchical cluster analysis revealed two groups which correspond with the species of the samples. No correlations between the contents of the inorganic elements and the localities of the samples were found. Some characteristic elements were displayed in some specific areas. The difference of the contents of the 53 inorganic elements between root and rhizome of Xixin was reported for the first time. The primary form of inorganic elements in Xixin has been studied for the first time. The result demonstrated that the extraction rate between different elements varied, with the average extraction rate of (22.25 +/- 24.96)%.</p><p><b>CONCLUSION</b>The inorganic elements analysis of Xixin can provide evidence of its identification, cultivation and application.</p>
Subject(s)
Asarum , Chemistry , Classification , China , Drugs, Chinese Herbal , Rhizome , Chemistry , Trace ElementsABSTRACT
<p><b>OBJECTIVE</b>To develop an HPLC method for simultaneous determination of swertiamarin, gentiopicroside, sweroside, mangiferin, erythrocentaurin, and to detect these five constituents in eight Qingyedans derived from Swertia mileensis, S. cincta, S. patens, S. punicea, S. delavayi, S. nervosa, S. macrosperma and S. yunnanensis.</p><p><b>METHOD</b>The separation was carried out on a Thermo BDS Hypersil C18 (4. 6 mm x 250 mm, 5 microm) column eluted with mobile phase of water containing 0. 1% phosphoric acid and methanol (B) in gradient program (0-10 min, 18%-20% B; 10-30 min, 20%-35% B; 30-35 min, 35%-60% B). The column temperature was 32 degrees C , and the detection wavelength was set at 250, 260, 225 nm. The flow rate was 0. 7 mL . min-1 from 0 to 30 min, and be increased to 1. 0 mL . min-1 in 35 min.</p><p><b>RESULT</b>The five compounds were well separated. The linear response ranges of swertiamarin, gentiopicroside, sweroside, mangiferin, erythrocentaurin were 0. 072-13. 39, 0. 1204. 518, 0. 060-5. 050, 0. 025-1. 518, and 0. 031-0. 210 microg, respectively. The mean recoveries of five compounds were 97.03% -102. 7% (RSD 1. 8% -6.2% ). There are swertiamarin, gentiopicroside and sweroside in most samples, and mangiferin in half samples. But erythrocentaurin was only detected in a few samples. The contents of five compounds were different in different samples. The contents of swertiamarin in S. mileensis, S. patens, S. yunnanensis and S. delavayi are up to 34. 47-118.05 mg . g-1, the contents of gentiopicroside are up to 25. 91 mg . g-1 in S. cincta. In S. puncea all contents of swertiamarin, gentiopicroside, sweroside and mangiferin are higher, especially the content of sweroside. There are Xiao-Qingyedans and Da-Qingyedans called in markets, and they can be identified by the contents of swertiamarin, gentiopicroside and sweroside. S. punicea can be identified by the content of sweroside, and the ratio gentiopicroside/total content can be used for identification of S. cincta from other seven Qingyedan species.</p><p><b>CONCLUSION</b>The method was certified to be accurate and reliable and can be used for identification and quality evaluation of traditional Chinese medicine Qingyedan derived from Swertia species.</p>