ABSTRACT
OBJECTIVE:To establish a method for the simultaneous determination of gallic acid,rhein and emodin in Com-pound xiaozhi suppository. METHODS:HPLC was performed on the column of Kromasil C18 with mobile phase of 0.5% phosphor-ic acid-Acetonitrile solution(gradient elution)at a flow rate of 1.0 ml/min,the detection wavelength was 273 nm for gallic acid and 254 nm for rhein and emodin,the column temperature was 28 ℃,and the injection volume was 20 μl. RESULTS:The linear range was 0.296 4-14.82 μg/ml for gallic acid(r=0.999 6),0.215 0-10.75 μg/ml for rhein(r=0.999 9)and 0.307 2-15.36 μg/ml for emo-din(r=0.999 9);RSDs of precision,stability and reroducibility tests were lower than 3.0%;recoveries were 95.1%-97.2%(RSD=0.64%,n=6),95.4%-97.2%(RSD=0.42%,n=6) and 96.5%-99.4%(RSD=1.10%,n=6),respectively. CONCLU-SIONS:The method is simple and accurate,and can be used for the contents determination of gallic acid,rhein and emodin in Compound xiaozhi suppository.
ABSTRACT
Objective: To develop an HPLC method for the simultaneous determination of paeoniflorin , liquiritin, baicalin and costunolide in Fuke Yangkun pills , and optimize the extraction technology by response surface methodology ( RSM).Methods: The separation of targeted compounds were performed on a Kromasil C 18 column (250 mm ×4.6 mm, 5 μm).The mobile phase consisted of acetonitrile (A) and 0.2%phosphoric acid (B) with gradient elution at a flow rate of 1.0 ml min-1.The detection wavelength was set at 230, 276, 280 and 225 nm, respectively.The column temperature was 28℃.Using the contents of the four components as the indices, the extraction process was optimized by a response surface method with methanol concentration , solid-liquid ratio and ex-traction time as the influencing factors .Results: The linear range of paeoniflorin , liquiritin, baicalin and costunolide was 1.616-161.600, 0.432-43.180, 2.045-204.500 and 0.518-51.840 μg ml-1, respectively.The average recovery (n=9) was 98.3%, 99.6%, 97.9%and 98.1%, respectively.The optimum conditions of extraction process were as follows:the methanol concentration was 64%, the solid-liquid ratio was 1 ∶51, and the extraction time was 25 min.Conclusion: The response surface methodology is convenient and highly predictive in optimizing the extraction process of the four effective components in Fuke Yangkun pills .The devel-oped content determination method is simple and accurate , which can be used for the quality control of Fuke Yangkun pills .