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Objective Traditional raw pangolin products are not used as medicine, which can only be used as medicine after processing. Therefore, the processing mechanism of high temperature sand-fried pangolin was studied. Methods The changes of liposolubility and protein composition of pangolin before and after processing were analyzed by TLC and Nano LC-Q Exactive Orbitrap MS. Meanwhile, the simulation processing of cyclic dipeptides, which were significantly increased during processing, was performed. The activity of L-serine-L-tyrosine cyclic dipeptide was screened. Results The results showed that there was no significant change in fat-soluble components, significant decrease in polypeptides and significant increase in cyclic dipeptides after the sand-fried processing of pangolin. The formation of cyclic dipeptides was mainly related to the heating of the processing. At low temperature, the N-terminal of the linear peptide could be cycled to form L-shaped cyclic dipeptides. At high temperature, the N-terminal and C-terminal of the linear peptide could be rapidly cycled to form cyclic dipeptides. L-serine-L-tyrosine cyclic dipeptide could prolong coagulation time and increase the proliferation rate of mammary epithelial cells and the expression of genes related to milk protein synthesis in dairy cows. It also had significant analgesic activity, which was consistent with the traditional efficacy of pangolin. Conclusion These results suggested that large amounts of L-serine-L-tyrosine cyclic dipeptide produced by the processing of pangolin may be one of the material bases for enhancing the processing efficiency of pangolin. It was of great significance for revealing the material basis of pharmacodynamics of pangolin, searching for alternative resources and protecting pangolin.
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OBJECTIVE:To establish GC-MS fingerprints of liposoluble constituents from Danqi soft capsule. METHODS:GC-MS method was adopted. GC chromatogram column was DB-5 ms capillary column with high purity helium (99.999%)as carrier gas at the flow rate of 1.0 mL/min,with temperature programming. The injector temperature was 250 ℃. The sample size was 1 μL. The shunt ratio was 1:40,with distributary injection. Ionization mode was as follows as electron bombardment ion source,ion source temperature of 280 ℃,injector temperature of 300 ℃,electronic energy of 70 eV, solvent delay time of 3 min,mass charge ratio(m/z)of 50-550. Using ethyl palmitate as reference,MS spectrums of 11 batches of samples were determined. Similarity evaluation was conducted by using TCM Fingerprint Chromatogram Similarity Evaluation System(2004 A edition)to determine common peak. The common peaks were determined by LC Solution 2 workstation standard mass spectrometry Library(NIST05.LIB or NIST05s.LIB). RESULTS:The similarity of 11 batches of samples was higher than 0.90. After validation,GC-MS chromatograms of 11 batches of samples were in good agreement with control fingerprint. There were 49 common peaks in GC-MS chromatogram,and 38 chemical constituents were identified, accounting for 94.94% of total peak areas. CONCLUSIONS:Established fingerprint can provide evidence for quality evaluation of Danqi soft capsule.
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The liposoluble constituents in Momordicae Semen were investigated in the present study. By silica gel, Sephadex LH-20 column chromatography, and semi-preparative HPLC, 22 compounds were isolated and purified from dichloromethane and ethyl acetate fraction. Based on NMR and MS spectra analyses, these compounds were identified as lupeol (1), 5-(1'-hydroxypentyl)-5H-furan-2-one (2), palmitic acid (3), viscumamide (4), clavatustide C (5), laxanol (6), threo-1-(4-hydroxyphenyl)-2-{4-[2-formyl-(E)-vinyl]-2-methoxyphenoxyl}-propane-1, 3-diol (7), α-spinasterol-3-O-β-D-glucoside (8), chushizisin F (9), ehletianol C (10), tanegool (11), (7R, 8R, 8'R)-4'-guaiacylglyceryl-evofolin B (12), ligballinone (13), (7R, 8S, 8'R)- 4, 4', 9-trihydroxy- 7, 9'-epoxy- 8, 8'-lignan (14), chushizisin I (15), chushizisin A (16), chushizisin G (17), p-coumaraldehyde (18), α-spinasterol (19), p-hydroxybenzoic acid (20), chushizisin E (21), and 3-[2-(4-hydroxyphenyl)-3-hydroxyphenyl-2, 3-dihydro-1-benzofuran-5-yl] propane-1-ol (22), respectively. Compounds 1-17 were isolated from Momordica cochinchinensis for the first time. Compound 2 was a new natural product while compounds 4 and 5 were first found in the terrestrial organism.
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AIM To study the effects of degreasing-frosting on reducing toxicity and enhancing efficacy of Periplaneta americana L..METHODS The 95％ ethanol extracts from P.americana raw powder and processed products were extracted by petroleum ether,ethyl acetate,n-butanol and water.TLC was applied to comparing the component changes in various fractions.GC-MS was used for analyzing the kinds and contents of liposoluble constituents before and after processing.Shaking flask method combined with UV spectrophotometry method was adopted in the determination of Papp values in octanol-water and different pH values (2.23,3.28,4.22,5.23,6.12,7.24,8.23,9.10,10.15 and pure water) of buffer solutions.RESULTS After the petroleum ether fraction was processed,the colors of TLC spots became much shallower,which changed more significantly with the prolonging of processing time and increase of pressure.The TLC spots in the n-butanol and water fractions were clear without obvious changes.And no TLC spots were found in the ethyl acetate fraction.The kinds of liposoluble constituents were the same before and after processing,whose absolute contents were decreased after processing.Compared with raw powder,the Papp values of minor polypeptides in various processed products at different pH values exhibited significant differences (P ＜0.05,P ＜0.01),which also showed certain differences at the same pH values.CONCLUSION Degreasing-frosting can affect the contents of liposoluble constituents in P.americana and Papp values of minor polypeptides,which may be the mechanism of reducing toxicity and enhancing efficacy.
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Objective:To investigate the liposoluble constituents in fruit of Cnidium monnieri. Methods:The liposoluble constitu-ents in fruit of C. monnieri were extracted by Soxet extraction. The extracted liposoluble constituents were methyl esterified and then analyzed by GC-MS for the first time. Results:Thirty-nine compounds (85. 33%) were identified from the liposoluble constituents in fruit of C. monnieri. Phytol (15. 98%), hexadecanoic acid (12. 73%), 9,12,15-octadecatrienoic acid (11. 02%), 9-octadecenoic acid (6. 33%) and 9,12-octadecadienoic acid (4. 77%) were the main constituents of the liposoluble constituents in fruit of C. mon-nieri. Conclusion:Phytol, hexadecanoic acid, 9,12,15-octadecatrienoic acid and 9-octadecenoic acid are the active ingredients in fruit of C. monnieri.
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OBJECTIVE:To analyze and identify the liposoluble constituents in Isatis indigotica.METHODS:The liposoluble constituents in Isatis indigotica were extracted with petroleum benzin,and the constituents in methyl ester products were sperated,identified and determined by GC/MS.RESULTS:A total of 42 liposoluble compounds were detected,with fatty acid methyl esters making up 36.72%(saturated fatty acid methyl esters 8.67% and unsaturated fatty acid methyl esters 28.05%),and of which,35 were reported for the first time in the study of Isatis indigotica.CONCLUSION:The liposoluble compounds in Isatis indigotica serve as reference for its comprehensive benefits and development of its antioxydant applilication.