ABSTRACT
OBJECTIVE：To study the spectrum-effect relationship of HPLC finger print of different polar parts of Ampelopsis grossedentata with its in vivo anti-inflammatory effect. METHODS ：A. grossedentata was reflux extracted with 70％ ethanol，then extracted with petroleum ether ，chloroform，ethyl acetate and water saturated n-butanol；or it was directly decocted with water and then concentrated to obtain different polar parts. The xylene-induced mice ear swelling model was established ；using dexamethasone as positive control ，anti-inflammatory activity of different polar parts of A. grossedentata was investigated. Fingerprints of different polar parts of A. grossedentata were established by HPLC. The determination was performed on Poroshell 120 EC-C18 column with mobile phase consisted of acetonitrile- 0.1％ phosphoric acid solution （gradient elution ）at the flow rate of 1 mL/min. The column temperature was 25 ℃. The detection wavelength was set at 365 nm，and sample size was 5 μL. The grey ralational analysis method was used to analyze the spectrum-effect relationship of HPLC fingerprint common peaks of different polar parts of A. grossedentata with its anti-inflammatory effect. The correlation coefficient and correlation degree were calculated and ranked. RESULTS：Anti-inflammatory experiment showed that the anti-inflammatory effects of 70％ ethanol extraction part ，ethyl acetate extraction part and water extraction part were the most significant （inhibitory rates of ear swelling were 54.07％，30.54％， 30.45％）. Five common peaks were determined in HPLC fingerprints of different polar parts from A. grossedentata . The spectrum-effect analysis results showed that the correlation of5 common peaks were higher than 0.6；among them ，peak 3 and peak 2 （dihydromyricetin） had the strongest anti- inflammatory effect ，and their correlation degrees were both mail：123745789@qq.com greater than 0.8. CONCLUSIONS ： The anti-inflammatory effect of A. grossedentata on xylene-induced ear swelling in mice is the result of multi-comp onent synergy ； unknown substance of peak 3 and dihydromyricetin may be the main active components of A. grossedentata .
ABSTRACT
OBJECTIVE：To establish a method for simultaneous determination of gallic acid ，protocatechuic acid ，mangiferin， homomangiferin，hyperoside and isoquercetin in Mangguo zhike tablets. METHODS ：HPLC was adopted. The determination was performed on Phenomenex Gemini C 18 column with mobile phase consisted of 0.1％ phosphoric acid water solution-acetonitrile （gradient elution ）at the flow rate of 1.0 mL/min. The detection wavelength was set at 258 nm. The column temperature was set at 30 ℃，and sample size was 5 μL. Gallic acid was used as the internal substance，and the correction factors of gallic acid ， protocatechuic acid ，mangiferin，homomangiferin，hyperoside and isoquercetin were calculated ；the results of quantitative analysis of multi-components by single marker method （QAMS） were compared with those of external standard method （ESM）. RESULTS：The linear range of gallic acid ，protocatechuic acid ，mangiferin，homomangiferin，hyperoside and isoquercetin were 45.75-183 0 μg/mL（r＝0.999 9），2.525-101.0 μg/mL（r＝0.999 9），65.33-261 3 μg/mL（r＝0.999 6），9.058-362.3 μg/mL（r＝ 0.999 9），3.885-155.4 μg/mL（r＝0.999 9），1.870-74.8 μg/mL（r＝0.999 9），respectively. The limits of quantification were 0.571， 0.643，1.053，0.854，0.830，1.500 μg/mL，respectively. The limits of detection were 0.171，0.193，0.316，0.256，0.249，0.450 μg/mL， respectively. RSDs of precision ，stability and reproducibility tests were all lower than 3％ . The average recoveries were 98.8％-101.9％（RSD＝1.3％ ，n＝6），94.3％-101.5％（RSD＝3.3％，n＝6），97.9％-100.5％（RSD＝0.9％，n＝6），98.2％- 101.6％ （RSD＝1.2％，n＝6），102.3％-106.1％（RSD＝1.3％，n＝6）， 96.6％ -99.3％（RSD＝1.0％ ，n＝6），respectively. RCFs of 73） protocate-chuic acid ， mangiferin， homomangiferin，hyperoside and isoquercetin were 0.568 3，0.500 3，0.687 6， 0.939 1 and 0.826 3，using gallic acid as internal substance . The content ranges of protocatechuic acid and other 4 com- ponents measured by QAMS were 0.197-0.440，3.262-11.250， 0.201-1.196，0.168-0.381，0.115-0.293 mg/tablet，respectively. The content ranges measured by ESM were 0.198-0.441，3.239-11.570，0.206-1.194，0.171-0.380，0.119-0.298 mg/tablet， respectively. By comparing the content determination results by QAMS and ESM ，the relative errors were －3.80％-0.74％，and there was no statistical significance （P＞0.05）. CONCLUSIONS ：The established QAMS method is accurate ，reliable and repeatable，and can be used for content determination of 6 medicinal components in Mangguo zhike tablets.
ABSTRACT
OBJECTIVE:To establish a method for the simultaneous determination of syringinand and pedunculoside in Zhuang medicine Yuyang powder. METHODS:HPLC was performed on the column of Agilent ODS with mobile phase of acetonitrile-water (gradient elution)at a flow rate of 1 ml/min,the detection wavelength was 210 nm,the column temperature was 30℃,and the in-jection volume was 5μl. RESULTS:The linear range was 0.71-3.55μg for syringin(r=0.999 7)and 1.62-8.10μg for pedunculoside (r=0.999 8), respectively;RSDs of precision, stability and reproducibility tests were lower than 3%;recoveries were 100.8%-104.9%(RSD=1.7%,n=6) and 96.0%-100.8%(RSD=2.2%,n=6). CONCLUSIONS:The method is simple,stable and reproducible,and can be used for the simultaneous determination of syringinand and pedunculoside in Zhuang medicine Yuyang powder.
ABSTRACT
<p><b>OBJECTIVE</b>To develop a method for the simultaneous determination of aflatoxin B1, B2, G1, G2 and ochratoxin A in Glycyrrhiza uralensis by HPLC-FLD after immunoaffinity column with online post-column photochemical derivatization.</p><p><b>METHOD</b>Sample was extracted with MeOH: H2O (80:20) and cleaned up by immunoaffinity column. The toxins were separated by reversed-phase HPLC and the mobile phase was consisted of methanol and 0.5% acetic acid solution with gradient elution. The determination was carried out by fluorescence detector after photochemical derivatization.</p><p><b>RESULT</b>The detection limits of aflatoxin G2, G1, B2, B1 and ochratoxin A were 0.02, 0.06, 0.015, 0.03 and 0.25 microg x kg(-1), respectively. The recoveries of analytes were from 76.0% to 103% and the relative standard deviations (RSDs) were below 13%.</p><p><b>CONCLUSION</b>The method is a simple, accurate and can be used to determine the contents of aflatoxin B1, B2, G1, G2 and ochratoxin A in G. uralensis simultaneously.</p>
Subject(s)
Aflatoxins , Chemistry , Chromatography, Affinity , Methods , Chromatography, High Pressure Liquid , Methods , Glycyrrhiza uralensis , Chemistry , Ochratoxins , Chemistry , Photochemical ProcessesABSTRACT
<p><b>OBJECTIVE</b>To establish a rapid determination method of pinoresinol diglucoside in Eucommiae unloads by near-infrared reflectance spectroscopy (NIRS).</p><p><b>METHOD</b>Forty-one samples of E. unloads were collected from three different producing areas and their main component, namely pinoresinol diglucoside, was determined by HPLC. Corresponding data of samples were collected from 12 000 to 4 000 cm(-1) by near-infrared reflectance spectroscopy. The spectral pretreatment was optimized by OPUS software and the calibration equations between the content of pinoresinol diglucoside and spectrum data were constructed by partial least squares regression.</p><p><b>RESULT</b>Available information could be extracted from spectra in the range from 7 502 to 4 597.6 cm(-1) after corrected by applying second derivative transformation and subtract a linear correction. Cross validation was used to prevent over-fitting. Good correlation existed between pinoresinol diglucoside content and NIR spectra ( R2 = 0.926 4, SEC = 0.029 and SEP = 0.066 2).</p><p><b>CONCLUSION</b>NIRS calibration equations developed in this study could be applied to the rapid analysis of the pinoresinol diglucoside content.</p>
Subject(s)
Eucommiaceae , Chemistry , Lignans , Spectrophotometry, Infrared , Methods , Time FactorsABSTRACT
Object To develop a method for the determination of flavonoids from the tender stem and leaf of Ampelosis grossedentata (Hand. Mazz.) W. T. Wang, and for its quality control. Methods Differential spectrophotometry was used at the wavelength of (318?1) nm, while taking dihydromyricetin as index. Results The regression equation, within the range of the control concentration in 4 576～22 88 ?g/mL, was A=29 56 C+0 005 5, with a good linearity (r=0 999 8) between the absorbance and concentration. The average recovery rate was 100 8% and RSD was 1 9% (n=5). Conclusion The method is simple, reliable and easy to operate and suitable for the quality control of Chinese medicinal materials with a better reproducibility.
ABSTRACT
AIM: To establish quality standard for Myricetin Dispersible Tablets. METHODS: Myricetin Dispersible Tablets were identified by UV and IR,and the content of myricetin in the tablets was determined by HPLC. RESULTS: The UV and IR spectra of Myricetin Dispersible Tablets were similar with those of myricetin.The linear range of myricetin was within the range of 0.071-0.165 mg/mL(r=(1.000 0)).The average recovery was 98.55%(n=6),and the RSD was 1.92%. CONCLUSION: The quality standard developed can be used for the quality control of Myricetin Dispersible Tablets.
ABSTRACT
AIM:To establish an HPLC-ELSD method for determing dulcitol and astragaloside in Compound Fufangteng Capsules(Radix et Rhizoma Ginseng rubra,Radix Astragali,Herba Euonymi,etc).METHOD:Chro-matographic conditions included Lichrospher 5-NH_2 column(250 mm?4.6 mm,5 ?m)and the mobile phase consisting of a mixture of acetonitrile-water(91 ∶9).The flow rate of mobile phase was 1.0 mL/min.The column tempe-rature was at 28 ℃.Detector:PL-ELS2100 ELSD(Eva:65 ℃,Ned:50 ℃,gas flow:0.9 L/min).RESULTS:The linear ranges of dulcitol and astragaloside were 2.91-29.1 ?g(r= 0.999 8)and 1.03-10.3 ?g(r= 0.999 1),respectively.The average recoveries of dulcitol and astragaloside were 99.24% and 103.17% with corresponding RSD of 2.6 % and 1.8%(n=6),respectively.CONCLUSION:The method is steady and with good repeatability,and can be used to determine the content of dulcitol and astragaloside in Compound Fufangteng Capsules.
ABSTRACT
AIM: To analyze the chemical composition and their relative contents of Fuyinjie Compound Huangsong Lotion. METHODS: A capillary column HP-5 MS was used. The column temperature was controlled by a program and the MS analysis was performed with EI and quadrupole mass analyzer. The chemical composition was identified by NIST98 searching and mass spectra comparing, and their relative contents were determined by using normalization method of chromatographic peak areas. RESULTS: There were 39 components found and 31 composed of more than 90% separated components were identified. CONCLUSION: The GC-MS is a simple, rapid and sensitive method for the chemical composition analysis of Fuyinjie Compound Huangsong Lotion.
ABSTRACT
AIM: To establish a RP-HPLC method to determine the fingerprint of Compound Fufangteng Mixture (Radix Ginseng Rubra, Radix Astragel. etc). METHODS: Chromatographic conditions included Shim-pack CLC ODS column and the mobile phase composed of a mixture of acetonitrile-water (gradient elution), detection wavelength at 203nm. The mobile phase flow rate was 1.0mL?min -1. RESULTS: 19 peaks existed on the HPLC fingerprint of Compound Fufangteng Mixture. CONCLUSION: The method can provide more information for the quality control of Compound Fufangteng Mixture.