ABSTRACT
Objective: To optimize the preparation process of Angelicae Sinensis Radix cellwall broken powder (ASR CBP) and evaluate the physical quality of powder. Methods: A HPLC method was established for the determination of five active constituents (ferulic acid, senkyunolide I, coniferyl ferulate, ligustilide and n-butylidenephthalide) of ASR. The Box-Behnken response surface design method was used. The pulverization time, pulverization temperature and sampling capacity in the pulverization process were investigated. The particle size distribution (D90) of the broken wall powder of ASR and the five active ingredients content were used as the response value to construct the response surface model. Under the premise of D90 < 45 μm, the maximum value of the five active ingredients was calculated to optimize the superfine grinding process parameters. A total of 13 physical indicators of D90, coefficient of nonuniformity, particle size distribution width, bulk density, tap density, interparticle porosity, Karl index, specific surface area, pore volume, Hausner ratio, angle of repose, loss on drying and hygroscopicity were used to establish the physical fingerprint of ASR CBP. The similarity evaluation method was used to evaluate the similarity of different batches of ASR CBP. Results: The methodological results of the HPLC method for the determination of the five active ingredients were in accordance with the guidelines. Results of response surface method showed the optimized preparing parameters of ASR CBP technology as follows: 35 min of pulverization time, -10 ℃ of pulverization temperature, and 580 g of sampling capacity. The RSD values between the content and the response surface fitting results of five active ingredients of three batches of cellwall broken powder prepared by the optimal process were all less than 3%. The similarity of the three batches of the optimal process of ASR CBP was above 99.4%. Conclusion: Box-Behnken optimized preparation method of ASR CBP has obvious advantages in retaining the content of active ingredients, especially volatile components. Physical fingerprinting has good practical effects as a tool to evaluate the consistency of physical properties of Chinese material medica powder. The combination of applications helps to achieve a higher quality control level of Chinese medicine cellwall broken powder production.