Development method of fingerprint of Compound Danshen Dripping Pills based on analytical quality by design (AQbD) / 中草药

ABSTRACT

Objective To study the development of analytical quality by design (AQbD) method for the identification of Compound Danshen Dripping Pills (CDDP) by UPLC-UV. Methods The number of peaks and the target peak content (notoginsenoside R1, ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1) were taken as the analytical target profile (ATP), Plackett-Burman design (PBD) method was used to select critical method parameters (CMPs) and critical method attributes (CMAs) on the basis of risk assessment, and then the response model between CMAs and CMPs was established by Box-Behnken design (BBD). The optimal conditions were obtained via multivariable regression analysis and verified. Results From the seven factors of risk assessment, the flow rate (A), sample weight (B), and C18 column weight (C) were selected as CMPs. And CMAs were the number of peaks (N), notoginsenoside R1 (CR1) and ginsenoside Re (CRe). The variation trends of each factor and model were analyzed by response surface analysis. The optimal conditions were as follows flow rate of 0.28 mL/min, sample weight of 0.30 g, and C18 column weight of 1.10 g. Under the conditions, N was 12, CR1 was 1.676 5 mg/g, and CRe was 0.669 6 mg/g, with differences of 1.34%, 1.33%, and 2.94% respectively from the predictive values. The final method was as follows chromatographic column was Acquity UPLC BEH C18 chromatographic column (50 mm × 2.1 mm, 1.7 μm), mobile phase was acetonitrile-water gradient elution, detection wavelength was 203 nm, column temperature was 30 ℃, flow rate was 0.28 mL/min, and injection volume was 2 μL. Conclusion The results prove that the method is reliable.