ABSTRACT
OBJECTIVE： To establish the method for content determination of 6 kinds of triterpene acids such as haw acid， corosolic acid， betula acid， betulonic acid， oleanolic acid and ursolic acid in Tibetan medicine Rubus biflorus. METHODS： Pre-column devrivatization HPLC-FLD-APCI/MS method was adopted. 2-（7H-dibenzo[a，g]carbazol-7-yl） ethyl-4-methylbenzene- sulfonate was used as the pre-column derivatization reagent．Hypersil C18 column was used with the mobile phase consisted of 5％ acetonitrile water solution-acetonitrile （gradient elution） at the flow rate of 1.0 mL/min. The excitation wavelength of fluorescence was 300 nm and the emission wavelength was 395 nm. The column temperature was 35 ℃， and sample size was 10 μL. Under atmospheric-pressure chemical ionization （APCI） source in positive-ion mode， pressure was 60 psi， the drying gas flow rate was 9 L/min， the dry gas temperature was 350 ℃， the gasification temperature was 450 ℃， and the capillary voltage was 3 500 V. RESULTS： The linear range of haw acid，corosolic acid，betula acid，betulonic acid，oleanolic acid and ursolic acid were 0.025-6.4 μg/mL（r≥0.999 6）. The quantitative limits were 5.11， 4.78， 4.42， 4.22， 4.29， 4.51 ng/mL； and detection limits were 1.42， 1.27， 1.30， 1.28， 1.16， 1.22 ng/mL， respectively. RSD of precision test was less than 5％， stability and repeatability tests were all less than 2％（no betulonic acid detected）. The recovery rates were 97.90％-100.55％（RSD＝1.00％，n＝6）， 97.95％-102.95％（RSD＝1.74％，n＝6）， 96.00％-101.20％（RSD＝2.00％，n＝6）， 93.25％-104.20％（RSD＝4.25％，n＝6）， 92.20％-103.30％（RSD＝3.58％，n＝6）， 97.80％-103.50％（RSD＝2.03％，n＝6）， respectively. CONCLUSIONS： The method is accurate， reliable and exclusive， and can be used for simultaneous determination of 6 kinds of triterpene acids in Tibetan medicine R. biflorus.
ABSTRACT
OBJECTIVE:To establish the quality standard of Tibetan medicine Rubus biflorus.METHODS:The qualitative identification was conducted from characters characteristics,microscopic characteristics,TLC.The contents of moisture,ash and extract were determined.HPLC method was adopted for content determination of rutin and hyperoside.The determination was performed on Diamonsil C18 column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid solution(18∶82,V/V) at the flow rate of 1.0 mL/min.The detection wavelength was set at 360 nm,column temperature was 30 ℃,and sample size was 10 μL.RESULTS:The surface of the medicinal material was grayish red to grey red brown,with longitudinal wrinkle grooves,and the peel was easy to peel off.The pith of the medicinal material was large,loose,sponge-like.The powder of the medicine was light yellow;wood fiber was bundle or scattered individually;bast fiber was thick.TLC spot of hyperoside was clear and well-separated.The contents of moisture,total ash,acid-insoluble ash,water-soluble extract and ethanol extract were 6.71％-7.55％,1.43％-1.67％,0.41％-0.48％,17.70％-19.31％ and 13.76％-16.99％.The linear range was 3.13-50 μg/mL for rutin (r=0.999 2)and hyperoside (r=0.999 5).The limits of quantitation were 0.5,1.8 μg/mL,and the limits of detection were 0.2,0.9 μg/mL.RSDsof precision,stability and reproducibility tests were all lower than 2.0 ％ (n =6).The recoveries were 92.8 ％-98.8 ％ (RSD =2.25 ％,n=9),94.0％-98.6％ (RSD=l.71％,n=9).CONCLUSIONS:The moisture content,total ash and acid insoluble ash content of medicinal materials is not more than 10.0％,3.0％ and 0.6％,respectively.The total amount of water extract,alcohol extract,rutin and hyperoside is not less than 15.0％,12.0％,1.0 mg/g,respectively.Established standard can be used for quality control of Tibetan medicine R.biflorus.
ABSTRACT
OBJECTIVE:To establish the quality standard of Tibetan medicine Myricaria germanica. METHODS:M. germani-ca was identified in respects of properties,microscopic characteristics and TLC. The contents of moisture,ash and extract were de-termined. HPLC method was adopted for content determination of gallic acid. The determination was performed on Diamonsil C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution(5:95,V/V)at the flow rate of 1.0 mL/min. The detection wavlengths were set at 270 nm. The column temperature was 30 ℃ and the sample size was 10 μL. RESULTS:M. ger-manica was cylindrical in shape,and there were many narrow strip alternate leaflets,which were brittle,easily broken,weak in smell,mild in flavor. Cork cell surface and lower epidermal cell surface showed polygon;most of xylon were bunched;there were many clusters of calcium oxalate. TLC spots were clear and well-separated. The contents of moisture,total ash,acid-insoluble ash, water-soluble extract and ethanol were 6.83%-8.12%,4.01%-5.01%,1.06%-1.98%,17.91%-22.65%,11.29%-15.51%. The linear range of gallic acid were 3.13-50 μg/mL(r=0.9997);RSDs of precision,stability and reproducibility tests were lower than 1.0%;the recoveries were 94.0%-100.8%(RSD=2.27%,n=9). CONCLUSIONS:Established standard can be used for quality evalua-tion of Tibetan medicine M. germanica.