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Objective:To optimize the extraction technology of Qige granule. Methods:An HPLC method was established to de-termine the contents of astragaloside IV and puerarin in the extract of Qige granules. Based on the orthogonal design of L9(34),three factors including the water amount,decocting duration and extracting times were evaluated. Results:The best extraction process was as follows:adding 12-fold amount of water and extracting 3 times with 30 min for each time. Conclusion:The extraction technology opti-mized by the components evaluation is reasonable and practicable.
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[ Objective ] To establish a method for the determination of serum strychnine concentration in rheumatoid arthritis patients treated with Tongbiling prescription and to monitor the serum strychnine concentration. [ Methods ] Serum strychnine was extracted with solid phase extraction column. Reversed-phase HPLC conditions were: Hypersil Division ODS C18 column (150 mm ?4.6 mm, 5?m), mobile phrase being methanol: water (70 : 30) with 0.6 g potassium dihydrogen phosphate and 1.0 g dodecyl sodium sulfonate added in 1000 mL mixture (adjust pH to 4.5 with acetic acid), detecting wavelength at 254nm and a flow rate of 1.0 mL/min at room temperature. [Results] Strychnine has a good linearity in the range of 0.031- 2.000?g?mL-1. The minimum detecting concentration was 0.01?g?mL-1 and the average recovery was over 90%. Intra-day RSD and inter-day RSD ranged from 1.53% to 5.32%. [Conclusion] This method is simple and efficient, and can be used for the determination of strychnine.
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OBJECTIVE:To study the quality standards for Shenchang injection.METHODS:TLC was applied to identify the properties of Borneol and volatile oil of Rhizoma Acori Tatarinowii in the formula.HPLC was adopted to determine the content of ?-asarone in Shenchang injection.RESULTS:?-asarone showed good linear relationship in the range of 0.632 3～ 1.264 6? g.The average recovery of ammonium ?-asarone was 99.92%(RSD=0.91%).CONCLUSION:The standard can be used for the quality control of Shenchang injection.
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Objective: To determine the contents of ?-Asarone and ?-Asarone in Xing Nao nasal drops. Methods: HPLC was used with ODS C18 column (150mm?4.6mm, 5?m). Methanol mixture : water being 6 : 4 and Patassium biphoepate 1.4 and Dodecyl Sulphonic acid sodium salt 1.2g in 1000mL mixture served as mobile phase, detection wavelength at 257nm and flow rate being 1.0mL/min. Results: The mean recovery was 99.38 %(RSD=2.25 %) for ?-Asarone and 96.59 %(RSD=2.16) for ?-Asarone. Conclusion: this method is simple,rapid and accurate.
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[Objective] To establish a method for the determination of brucine and strychnine contents in Tongbiling Tablet. [Methods] Reversed-phase HPLC conditions were: Nucleodur C18 Gravity column (125 mm ? 4.6 mm, 5?m), mobile phrase being methanol-water (60:40) with 0.5 g potassium dihydrogen phosphate and 1.0 g dodecyl sodium sulfouate and 0.5 mL triethylamine in 1 000 mL mixture (adjusting pH to 4.5 with acetic acid) , detecting wavelength at 254 run and a flow rate of 1.0 mL/min at room temperature. [ Results ] The average recovery of brucine was 97.69 % ( RSD = 2.03%) and that of strychnine 97.93% ( RSD = 2.61%). [Conclusion] This method is efficient and can be used for the quality control of Tongbiling Tablet.
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Objective To study the change of Hesperidin content in various combinations of medicine from Buzhong Yiqi Decoction(BYD) by RP-HPLC.Methods The hesperidin content was determined by HPLC and analyzed by L8(27) orthogonal design and statistic analysis(SPSS).Results Principal herbs and ministerial herbs of BYD had a significant effect on the hesperidin content of adjunctive herbs(P
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Objective To establish the fingerprint chromatogram of Buzhong Yiqi Decoction(BYD) by multiple wavelength method,and to analyze the substance of formulas as a whole.Methods HPLC-PDA method was adopted.The chromatographic conditions were as follows:Hypersil ODS2 analytical column,the mobile phase consisting of 0.05 %phosphate acid and acetonitrile with gradient elution,detecting wavelength at 254 and 280 nm,the flow rate being 1.0 mL/min and the temperature of the column at 30 ℃.Results The methodological results were good.The results of dual-wavelength fingerprint chromatogram showed the all-around information of the fingerprints at 254 and 280 nm.The similarity of 10 batches of BuzhongYiqi Decoction was over 0.98.Conclusion Dual-wavelength fingerprint chromatogram can realize the analysis of a formulas as a whole,which supplies references for improving the quality control of BuzhongYiqi Decoction.
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Objective: To determine the component of naphtha from Acorus tatarinowii Schott.which can pass through the blood-brain barrier. Methods: Naphtha in rat brain was analyzed by GC-MS after gastric infusion of naphtha. Results: The methylisoeugenol,elemicin, ?-asarone and ?-asarone were detected in rat brain. Conclusion: The resuscitative effect of naphtha is resulted from the comprehensive action of multiple components.
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Objective To establish the HPLC fingerprint of amino acids compounds from Buzhong Yiqi Pill.Methods A pre-column derivatization HPLC method was adopted with praline as a reference.Separation was performed on a AccQ? TagTM C18(3.9? 150 mm)analytical column with mobile phase consisting of 0.15 mol/L sodium acetate buffer solution and 60 % acetonitrile,gradient elution with the flow rate of 1.0 mL/min.The column temperature was at 37 ℃.The Fluorescence detecting wavelength was set at 250 nm(excitation wavelength)and 395 nm(emission wavelength),the analysis time was 35 min.Results Twelve common peaks on the HPLC fingerprints of Buzhong Yiqi Pill were presented.The similarity was determined by the correlation coefficient,included angle cosine coefficient and evaluation software of chromatogram fingerprint similarity.The results showed the similarity for 10 bathes of samples was in 0.97～ 1.00.Conclusion Good fingerprints were obtained,which can be used for the quality control of Buzhong Yiqi Pill.
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AIM: To establish an effective and convenient method for applying HPLC fingerprints to quality control in the production of Xiasangju Granules(Spica prunellae,Folium mori,Flos chrysanthemi). METHODS: Komasil Sunfrie C_(18)(150 mm?4.6 mm,5 ?m) analytical column was used and eluted with a gradient program consisted of phase A(1% acetic acid) and phase B(methanol) and detected at 290 nm.The fingerprints of aqueous extract,alcohol-precipitated extract,concentrate and finished product were compared with. RESULTS: The fingerprint method for Xiasangju Granules was established.The similarity among 10 batches of Xiasangju Granules was no less than 0.970.The difference between extracts and finished product of Xiasangju Granules was obvious. CONCLUSION: This validated method is available for quality evaluation and quality control in Xiasangju Granule's production.
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AIM:To establish the fingerprint chromatogram of amino acids compounds of Xiasangju Granules(Spica Prunellae,Flos Chrysanthemi indici,Folium mori.).METHODS:To apply 6-aminoqtiinoly-N-hydroxysuccinimdyl carbamate(AQC) pre-column derivatization HPLC method.Separation was performed on SYMMETRY C_(18)(150 mm?(4.6) mm,5 ?m) analytical column with mobile phase consisting of acetate(pH=(5.05)) and 60% acetonitrile with gradient elution with the flow rate(1.0) mL/min and the column temperature at 37 ℃.The Fluorescence wavelength used for detection was set at 250 nm(Excitation wavelength) and 395 nm(Emission wavelength) and the analysis time was 50 min.RESULTS:12 co-peaks on the HPLC fingerprints of Xiasangju Granules were indicated.The similarities were determined by the coefficients of cosine and correlation.The results of similarity analysis were(0.95)-(1.00).CONCLUSION:Perfect fingerprints were obtained which can be used for the quality control of Xiasangju Granules.
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Objective: To determine ? asarone and ? asarone in Rhizoma acori tatarinowii(RAT) . Methods: HPLC condition consists of ODS C 18 column(150mm?4.6mm, 5?m), methanol: water(6∶4) as mobile phase containing potassium dihydrogen phosphate 1.4g and sodium lauryl sulfate 1.2g per 1000mL, detective wavelength at 257nm, flow rate at 1.0mL?min -1 . Results: For RAT the mean recovery of 99.02%( RSD =1.03%) for ? asarone, 101.26%( RSD =3.57%) for ? asarone are obtained, respectively. Conclusion: The method is sensitive, rapid and accurate.
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OBJECTIVE:To establish a HPLC method for determination of paeonol and imperatorin in Cangzhi nose spray. METHODS:HPLC system consisted of ODS C 18 column(150mm?4.6mm,5?m)methanol-water(6∶4)mixture as mobile phase,with detection wavelength at310nm,flow rate1.0ml/min.RESULTS:The average recoveries of paeonol and imperatorin were99.4%(RSD=0.69%)and99.9%(RSD=2.66%)respectively.CONCLUSION:The method is sensitive,rapid and ac?curate.