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Objective To study the chemical constituents from the leaves of Styrax japonicus. Methods Seventeen compounds including nine phenylpropanoids and seven other constituents were isolated from the chloroform fraction of the 70% ethanol extract of leaves of S. japonicus, using column chromatography over silica gel and Sephadex LH-20 as well as the method of recrystallization. Results On the basis of physical and chemical properties combined with spectral data analysis, their structures were elucidated as nectandrin B (1), stigmasterol (2), matteucinol (3), eupomatenoid-7 (4), β-stigmasterol (5), dehydrodiisoeugenol (6), 4-oxo- 4[(3β,22E)-stigmasta-5,22-dien-3-yloxy] butanoic acid (7), 4-(3-methory-4-hydroxy) pheny-3-methyl-3-buten-2-one (8), ursolic acid (9), vanillic acid (10), (+)-(7S,8R,8’R)-4,8’-dihydroxy-3-methoxy-1’,2’,3’,4’,5’,6’-hexanorligna-7,7’-lactone (11), (+)-(7S,8R)-4- hydroxy-3-methoxy-1’,2’,3’,4’,5’,6’,7’-heptanorlign 8’-one (12), (2S,3R’)-2,3-dihydro-2-(4-hydroxy-3-methoxyphenyl)-7-methoxy- 5-(2-propen-1-yl)-3-benzofuranmethanol (13), vanillin (14), (E)-p-coumaric acid (15), and dihydrokaempferol (16). Conclusion Compounds 1, 3-16 are isolated from this plant for the first time.
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AIM To establish a quantitative analysis of multi-components by single-marker (QAMS) method for the simultaneous content determination of five constituents in Roudoukou-8 Powder (Myristicae Semen,Auck landiae Radix,Lignum aquilariae Resinatum,etc.).METHODS The analysis of 75％ methanol extract of this drug was performed on a 30 ℃ thermostatic Apollo C18 column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of methanol-0.1％ phosphoric acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelengths were set at 225,254,273,281 nm.With eugenol as an internal standard,the relative correction factors of the other four constituents were calculated,after which the content determination was made.RESULTS Ellagic acid,eugenol,costunolide,dehydroroma lactone,dehydrodiisoeugenol showed good linear relationships within the ranges of 0.227 0-1.135 2,5.272 2-26.361 0,0.540 8-2.704 0,0.530 4-2.652 0,0.059 0-0.299 5 μg (r ＞0.999 0),whose average recoveries (RSDs) were 96.37％ (2.07％),102.19％ (2.78％),101.66％ (1.66％),103.46％ (1.17％),98.25％ (1.98％),respectively.The results obtained by QAMS approximated those obtained by external standard method.CONCLUSION This stable and reliable method can be used for the quality control of Roudoukou-8 Powder.
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Objective To establish the HPLC fingerprint of Ershen Pills extracted with petroleum ether, which contains Psoraleae Fructus (PF) before and after processing, and initially set up the pattern recognition technique of the extract, so as to provide reference for quality control. Methods HPLC was used, and the separation was performed at 30 ℃ on an Spolar Hplc Packed C18 column (250 mm × 4.6 mm, 5 μm). Gradient elution was performed with the mobile phases of methanol-acetonitrile (1:1) and water containing 0.1% formic acid. The flow rate was 1 mL/min, and sample size was 10 μL. The UV detection wavelength was set at 210 nm. Furthermore, the fingerprint was analyzed by similarity analysis, as well as pattern recognition technique, including hierarchical clustering analysis and principal component analysis. Results The fingerprints were established respectively consisting of 28 common peaks well separated. There into, six compounds were identified (psoralen, isopsoralen, methyleugenol, methylisoeugenol, dehydrodiisoeugenol, and backuchiol). Compared with the reference spectrum, the similarity degrees were greater than 0.9. When dealing with principal component analysis, the samples were well divided into two categories, which was consistent with the principal component analysis. Meanwhile, the results of principal component analysis prompted some chromatographic peaks which could be used to distinguish between two species. Conclusion The method is stable and reliable, which can be used for quality control of Ershen Pills extracted with petroleum ether. Meanwhile, it is contributing to the entire quality control and quality evaluation when combined with chemical pattern recognition.
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OBJECTIVE:To establish a method for the determining contents of 2 lignan components[dehydrodiisoeugenol and 2,3-dihydro-7-methoxy-2-(3,4-methylened ioxyphenyl)-3-methyl-5-(E)-propenyl-benzofuran(referred to“lignanoid 2”)]. METH-ODS:HPLC method was adopted. The column was Elite C18 with the mobile phase of water-methanol(gradient elution)at the flow rate of 1.0 ml/min;the detection wavelength was 225 nm and the column temperature was 30 ℃. The sample size was 20 μl. RE-SULTS:There was a good linear relationship between sample quantity and the peak area in the range of 0.202-2.02 μg(r=0.999 9) and 0.204-2.04 μg(r=0.999 9)for 2 lignan components. The RSD of precision,stability and repeatability tests were less than 2%with the average recovery of 101.54%(RSD=0.60%,n=6)and 99.43%(RSD=1.09%,n=6). CONCLUSIONS:The method is simple,sensitive and accurate,and can be used for the quantization determination of dehydrodiisoeugenol and lignanoid 2 in nut-meg-5.
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Objective To develope a high performance liquid chromatograph ( HPLC ) method for simultaneous determination of nutmeg lignan and dehydrodiisoeugenol before and after processing of nutmeg. Methods The column was Diamonsil C18(250 mmí 4. 6 mm, 5 μm). The mobile phase was methanol-water in a gradient elution mode. The UV detection wave length was 274 nm. The column temperature was 25℃ . The flow rate was 1. 0 mL·min-1 . Results Nutmeg lignan and dehydrodiisoeugenol had a good linear correlation in ranges of 10. 24-61. 44 μg·mL-1(r=0. 999 6) and 3. 0-18. 0 μg·mL-1 (r=0.999 8), respectively. The average recovery rates were 97. 94% (RSD=2. 17%) and 97. 11% (RSD=2. 17%). Conclusion The method is simple, accurate, reproducible, and can be used for the simultaneous determination of nutmeg lignan and dehydrodiisoeugenol before and after the processing of nutmeg.
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Objective: To optimize the ethanol extraction process of Psoraleae Fructus-Myristicae Semen (psoralen-nutmeg) drug pair. Methods: Using L9(34) orthogonal design, the effects of ethanol concentration, ethanol amount, extraction time, and extraction times on the extraction process were investigated. The contents of psoralen, isopsoralen, and dehydrodiisoeugenol, dry extract yield, and total area of HPLC fingerprint characteristic peaks were used as comprehensive evaluation indexes. Results: The optimum process conditions were as follows: 50% ethanol, six times of the ethanol volume, extracted for three times, each time for 2 h. Conclusion: The method provides the basis for the determination of ethanol extraction process of Psoraleae Fructus-Myristicae Semen drug pair.
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Objective To establish the fingerprints analysis of the methanol extracts of nutmeg,and study quality uniformity of nutmeg in different areas.Methods A ZORBAX EclipseXDB-C18 (4.6 mm?150 mm,5 ?m) column was used.The mobile phase consisted of methanol-acetonitrile-water (25∶35∶40),the flow rate was 1 mL/min,the column temperature was 30 ℃,the detective wavelength was 270 nm.Dehydrodiisoeugenol was used as reference compound.Results Fingerprint of nutmeg was established,consisted of l7 common peaks.The similarity of fingerprints was over 0.9.Conclusion The fingerprints of nutmeg in different areas have no differences.This method is accurate,reliable and provides a scientific basis for the quality control of nutmeg.