RESUMO
OBJECTIVE:To establish the UPLC fingerprint for Qinghou liyan granule,and provide reference for its quality control by combining with principal component analysis (PCA). METHODS:UPLC was performed on the column of ACQUITY UPLC BEH C18 with mobile phase of acetonitrile(A)-0.1% aqueous phosphoric acid solution(B)(gradient elution)at a flow rate of 0.4 mL/min,the detection wavelength was 280 nm,column temperature was 30℃,and injection volume was 2μL. Using ellag-ic acid as a reference,12 batches of samples were analyzed,Similarity Evaluation Software for Chromatographic Fingerprint of Traditional Chinese Medicinewas used for the similarity analysis and identification of the common peaks,and the PCA was used for common peaks. RESULTS:There were 18 common peaks in the fingerprints of 12 batches of samples,and 6 principal peaks (gallic acid,ellagic acid,naringin,hesperidin,neohesperidin and baicalin) were identified;the similarity degree of 12 batches and reference fingerprints were no less than 0.984. According to PCA,the 18 peaks can be integrated into 3 principal components, with cumulative contribution rate of principal component of 78.277%;baicalin and 16 peaks were the discriminating factors of the fingerprint of Qinghou liyan granule. CONCLUSIONS:The method can provide reference for the quality control of Qinghou liyangranule.
RESUMO
OBJECTIVE:To establish a method for the contents determination of gallic acid,naringin,hesperidin,neohesperi-din and baicalin in Qinghou liyan granule. METHODS:UPLC was performed on the column of ACQUITY UPLC BEH C18 with mobile phase of acetonitrile- 0.1% phosphoric acid(gradient elution)at a flow rate of 0.40 ml/min,detection wavelength was 280 nm,column temperature was 30 ℃,and injection volume was 1 μl. RESULTS:The linear range was 0.048-0.480 μg for gallic ac-id(r=0.999 3),0.012-0.120 μg for naringin(r=0.999 9),0.016-0.160 μg for hesperidin(r=0.999 8),0.022-0.220 μg for neo-hesperidin(r=0.999 9)and 0.072-0.720 μg for baicalin(r=0.999 2);limit of quantitation was 2.4,1.6,1.8,1.8,1.6 ng,limit of detection was 7.5,5.0,5.6,5.6,5.0 ng;RSDs of precision,stability and reproducibility tests were no lower than 3.0%;recover-ies were 96.64%-102.02%(RSD=2.00%,n=6),95.86%-102.56%(RSD=2.86%,n=6),97.24%-102.54%(RSD=2.10%,n=6),97.44%-102.60%(RSD=2.40%,n=6)and 96.91%-103.13%(RSD=2.62%,n=6). CONCLUSIONS:The method is rapid and accurate,and can be used for the simultaneous determination of gallic acid,naringin,hesperidin,neohesperidin and baicalin in Qinghou liyan granule.