ABSTRACT
OBJECTIVE:To establish a method for simultaneous determination of gallic acid,chlorogenic acid,paeoniflorin and paeonol in Fule granules. METHODS:HPLC method was adopted. The determination was performed on Ultimate XB-C18 col-umn with mobile phase consisted of acetonitrile-0.05%phosphoric acid(gradient elution)at the flow rate of 1.0 mL/min. The detec-tion wavelengths were 270 nm(gallic acid,paeonol),325 nm(chlorogenic acid)and 230 nm(paeoniflorin). The column tempera-ture was 30 ℃,and sample size was 10 μL. RESULTS:The linear ranges of gallic acid,chlorogenic acid,paeoniflorin and pae-onol were 0.0762-1.524 μg(r=0.9997),0.0376-0.751 μg(r=0.9999),0.0303-0.606 μg(r=0.9997),0.0206-0.412 μg(r=0.9998),respectively. The limits of quantification were 0.353,0.276,0.421,0.540 μg/mL,and the limits of detection were 0.121,0.104,0.148,0.186μg/mL. RSDs of precision,stability and reproducibility tests were all no more than 2.04%. The recover-ies were 95.24%-100.47%(RSD=1.59%,n=9),99.49%-103.70%(RSD=2.27%,n=9),96.27%-101.09%(RSD=1.94%,n=9),95.05%-98.89%(RSD=1.22%,n=9), respectively. CONCLUSIONS:The method is simple,accurate and reproducible,and can be used for the simultaneous determination of gallic acid,chlorogenic acid,paeoniflorin and paeonol in Fule granules.
ABSTRACT
Objective To establish a method for fingerprint analysis of amino acids from honey by high performance liquid chromatography ( HPLC). Methods Amino acids of honey were concentrated by 732 cation exchange resin, and then were treated by pre-column derivatization with phenyl isothiocyanate, with praline as control peak. The chromatography was performed on a Waters Symmetry C18 ( 250 mm × 4.6 mm × 5 μm) column, with acetonitrile ∶ water (4∶1) as mobile phase A and 30 mmol/L sodium acetate ∶ acetonitrile (355∶15, acetic acid adjusting pH value to be 6.5) as mobile phase B by gradient elution. The detection wave length was set at 254 nm. The flow rate was 1.0 mL/min. The column temperature was 40℃, and the injection volume was 5μL. Results Sixteen common peaks were shown in the fingerprint of 15 batches of honey samples. The similarity for 15 batches of honey samples was in the range of 0.910 ~ 0.996 . Conclusion The fingerprint detection method is simple, practical, reproducible and specific, and can provide certain reference for quality control of honey.