1.Simultaneous Determination of Three Kinds of Components in Compound Xiaozhi Suppository by HPLC
Guangcai QI ; Jiangrui WU ; Mimi ZHANG ; Shengfei CUI ; Zhenye LIU
China Pharmacy 2016;27(15):2138-2140
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.
2.Extraction Optimization by Response Surface Method and Content Determination by HPLC of Four Effec-tive Components in Fuke Yangkun Pills
Guangcai QI ; Shengfei CUI ; Jiangrui WU ; Mimi ZHANG ; Zhenye LIU
China Pharmacist 2016;19(6):1048-1051,1063
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 .