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Objective:To establish an HPLC gradient elution method for the determination of isoalantolactone,alantolactone,xan-thotoxol,oxypeucedanin,imperatorin and osthole in Kangfu ointment simultaneously. Methods:Isoalantolactone,alantolactone,xan-thotoxol,oxypeucedanin,imperatorin and osthole were determined by HPLC with a chromatographic column of Agilent TC-C18(250 mm ×4.6 mm,5 μm),the mobile phase was methanol-0.1% formic acid solution with gradient elution at a flow rate of 0.9 ml·min-1. The detection wavelengths were 220 nm and 300 nm. The column temperature was 35℃. Results: The linear range of isoalantolac-tone,alantolactone,xanthotoxol,oxypeucedanin,imperatorin and osthole was 6.16-123.20 μg·ml-1,3.78-75.60 μg·ml-1,1.87-37.40 μg·ml-1,4.06-81.20 μg·ml-1,9.27-185.40 μg·ml-1and 13.89-277.80 μg·ml-1,respectively. The correlation coef-ficient was 0.999 4,0.999 8,0.999 6,0.999 5,0.999 9 and 0.999 7, respectively. The average recovery was 98.04% (RSD=1.06%),97.10%(RSD = 1.53%), 96.73% (RSD = 0.90%), 98.92% (RSD = 1.36%), 99.12% (RSD = 0.83%) and 100.27%(RSD=0.58%),respectively. Conclusion:The method is simple and accurate,which can be used to improve the quality standard for Kangfu ointment.
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Objective:To compare the contents of notoginsenoside R1 , ginsenoside Rg1 and ginsenoside Rb1 between Notoginseng Radix et Rhizoma and its formula granules. Methods:An HPLC method was used with a SunFire C18 column (250mm × 4. 6 mm, 5μm),the flow rate was 1. 0 ml·min-1, the detection wavelength was set at 203 nm, and the column temperature was at 30 ℃. The mobile phase was acetonitrile( A)-water( B) with gradient elution. An HPLC was used to determine the contents of the three ingredi-ents between Notoginseng Radix et Rhizoma and its formula granules, and compare the differences. Results: The total content of the three ingredients in Notoginseng Radix et Rhizoma and its formula granules was 9. 214% and 8. 646%, respectively. The total content of the three ingredients was equivalent and the daily amount of the major components in the commercial formula granules was equivalent with that in the decoction of Notoginseng Radix et Rhizoma. Conclusion:The production process of the original formula granules is re-liable, and the quality of formula granules of Notoginseng Radix et Rhizoma is stable.
RESUMO
OBJECTIVE:To establish a method for the simultaneous determination of chlorogenic acid,paeoniflorin,ferulic ac-id,berberine hydrochloride and baicalin in Lianqiao baidu pill. METHODS:HPLC was performed on the column of Agilent Eclipse XDB-C18 with mobile phase of 0.5% phosphoric acid(triethylamine adjusted to pH 3.0)-methanol(gradient elution)at a flow rate of 1.0 ml/min,the column temperature was 30 ℃,the detection wavelength was 230 nm(for paeoniflorin and berberine hydrochlo-ride),324 nm(for chlorogenic acid and ferulic acid)and 278 nm(for baicalin),and the injection volume was 5 μl. RESULTS:The linear range was 1.884-30.144 μg/ml for chlorogenic acid(r=0.999 9),0.392-6.272 μg/ml for paeoniflorin(r=0.999 7), 0.102-1.632 μg/ml for ferulic acid(r=0.999 7),1.326-21.216 μg/ml for berberine hydrochloride(r=0.999 8) and 1.95-31.2 μg/ml for baicalin(r=0.999 9),respectively;RSDs of precision,stability and reproducibility tests were lower than 2.0%;recoveries were 99.58%-102.47%(RSD=0.93%,n=9),99.21%-102.18%(RSD=0.90%,n=9),98.28%-101.23%(RSD=0.86%,n=9), 99.66%-101.84%(RSD=0.82%,n=9)and 99.18%-101.05%(RSD=0.62%,n=9). CONCLUSIONS:The method is accurate,re-liable,simple and fast,and can be used for the simultaneous determination of chlorogenic acid,paeoniflorin,ferulic acid,berber-ine hydrochloride and baicalin Lianqiao baidu pill.
RESUMO
Objective:To establish a quantitative analysis method to determine the content of sulfurous anhydride in Rhizoma di-oscoreae by ion chromatography-direct extraction. Methods:Sulfurous anhydride was extracted by KOH solution (25 mmol·L-1). An IonPac? AS11-HC column(250 mm × 4 mm, 9. 0 μm) was used. The column temperature was 20℃, the eluent was KOH solution (20 mmol·L-1 ) at flow rate of 1. 00 ml·min-1 and the conductivity temperature was 20℃. Results:There was a good linear rela-tionship between the injection quantity (1.160-29.100 μg)and the peak area of sulfite(r =0.999 9). The average recovery was 98. 9%(RSD=0. 6%, n=9). The quantitation limit was 1. 38 ng·ml-1. Conclusion: The method is simple, accurate and rapid, which is appropriate for the quantitative analysis of sulfite anhydride in Rhizoma dioscoreae.