To determine 13 flavonoids and glycyrrhizic acid in licorice(Glycyrrhiza spp.), several samples from different areas were examined by HPLC-DAD analysisT he analysis was performed on a Zorbax Extend-C18(250 mm × 4...To determine 13 flavonoids and glycyrrhizic acid in licorice(Glycyrrhiza spp.), several samples from different areas were examined by HPLC-DAD analysisT he analysis was performed on a Zorbax Extend-C18(250 mm × 4.6 mm, 5 μm) column connected with a Zorbax Extend guard column(20 mm × 4.6 mm, 5 μm). The mobile phase consisted of(A) acetonitrile and(B) 0.026% aqueous H3PO4(V/V) using a gradient elution of 20%-25% A at 0-20 min, 25%-33% A at 20-30 min, 33%-50% A at 30-55 min, 50%-60% A at 55-65 min, and 60% A between 65 min and 80 min, and peaks were detected at 280 nm. The fourteen compounds were assigned by HPLC-Orbitrap MS methods. The regression coefficient for the linear equations for the 14 compounds ranged between 0.9998 and 1. The limits of detection and quantification lay in the range of 0.032-2.461 and 0.154-8.202 μg·mL-1, respectively. The relative recovery rates for the 14 compounds were in the range of 93.90%-106.73% with RSDs being less than 5%. Coefficient variations for intra-day and inter-day precisions were in the range of 0.27%-2.38% and 0.31%-3.51%, respectively. In summary, the validated method was applied to the simultaneous determination of the 14 components in 29 different licorice samples and was proven to be suitable for quality evaluation of licorices and their active fractions.展开更多
Aconiti Lateralis Radix Praeparata(Fuzi) is a commonly used traditional Chinese medicine in clinic for its potency in restoring yang and rescuing from collapse. Aconiti alkaloids, mainly including monoester-diterpenoi...Aconiti Lateralis Radix Praeparata(Fuzi) is a commonly used traditional Chinese medicine in clinic for its potency in restoring yang and rescuing from collapse. Aconiti alkaloids, mainly including monoester-diterpenoidaconitines(MDAs) and diester-diterpenoidaconitines(DDAs), are considered to act as both bioactive and toxic constituents. In the present study, a feasible, economical, and accurate HPLC method for simultaneous determination of six alkaloid markers using the Single Standard for Determination of Multi-Components(SSDMC) method was developed and fully validated. Benzoylmesaconine was used as the unique reference standard. This method was proven as accurate(recovery varying between 97.5%-101.8%, RSD < 3%), precise(RSD 0.63%-2.05%), and linear(R > 0.999 9) over the concentration ranges, and subsequently applied to quantitative evaluation of 62 batches of samples, among which 45 batches were from good manufacturing practice(GMP) facilities and 17 batches from the drug market. The contents were then analyzed by principal component analysis(PCA) and homogeneity test. The present study provided valuable information for improving the quality standard of Aconiti Lateralis Radix Praeparata. The developed method also has the potential in analysis of other Aconitum species, such as Aconitum carmichaelii(prepared parent root) and Aconitum kusnezoffii(prepared root).展开更多
基金supported by the National Natural Science Foundation of China(No.81001630)Natural Science Foundation of Shanghai(No.10ZR1436400)+1 种基金Major Projects of Knowledge Innovation Program of the Chinese Academy of Sciences(No.KSCX2-YW-R-166)the Twelfth Five-Year National Science&Technology Support Program(No.2012BAI29B06)
文摘To determine 13 flavonoids and glycyrrhizic acid in licorice(Glycyrrhiza spp.), several samples from different areas were examined by HPLC-DAD analysisT he analysis was performed on a Zorbax Extend-C18(250 mm × 4.6 mm, 5 μm) column connected with a Zorbax Extend guard column(20 mm × 4.6 mm, 5 μm). The mobile phase consisted of(A) acetonitrile and(B) 0.026% aqueous H3PO4(V/V) using a gradient elution of 20%-25% A at 0-20 min, 25%-33% A at 20-30 min, 33%-50% A at 30-55 min, 50%-60% A at 55-65 min, and 60% A between 65 min and 80 min, and peaks were detected at 280 nm. The fourteen compounds were assigned by HPLC-Orbitrap MS methods. The regression coefficient for the linear equations for the 14 compounds ranged between 0.9998 and 1. The limits of detection and quantification lay in the range of 0.032-2.461 and 0.154-8.202 μg·mL-1, respectively. The relative recovery rates for the 14 compounds were in the range of 93.90%-106.73% with RSDs being less than 5%. Coefficient variations for intra-day and inter-day precisions were in the range of 0.27%-2.38% and 0.31%-3.51%, respectively. In summary, the validated method was applied to the simultaneous determination of the 14 components in 29 different licorice samples and was proven to be suitable for quality evaluation of licorices and their active fractions.
基金financially supported by the project of Standardization of Traditional Chinese Medicines/Indigenous Drugs sponsored by Chinese Academy of Sciences(No.KSZD-EW-Z-004-01)
文摘Aconiti Lateralis Radix Praeparata(Fuzi) is a commonly used traditional Chinese medicine in clinic for its potency in restoring yang and rescuing from collapse. Aconiti alkaloids, mainly including monoester-diterpenoidaconitines(MDAs) and diester-diterpenoidaconitines(DDAs), are considered to act as both bioactive and toxic constituents. In the present study, a feasible, economical, and accurate HPLC method for simultaneous determination of six alkaloid markers using the Single Standard for Determination of Multi-Components(SSDMC) method was developed and fully validated. Benzoylmesaconine was used as the unique reference standard. This method was proven as accurate(recovery varying between 97.5%-101.8%, RSD < 3%), precise(RSD 0.63%-2.05%), and linear(R > 0.999 9) over the concentration ranges, and subsequently applied to quantitative evaluation of 62 batches of samples, among which 45 batches were from good manufacturing practice(GMP) facilities and 17 batches from the drug market. The contents were then analyzed by principal component analysis(PCA) and homogeneity test. The present study provided valuable information for improving the quality standard of Aconiti Lateralis Radix Praeparata. The developed method also has the potential in analysis of other Aconitum species, such as Aconitum carmichaelii(prepared parent root) and Aconitum kusnezoffii(prepared root).
