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OBJECTIVE To optimize the molding process of Shuangye pipa granules based on the concept of quality by design （QbD） and analyze its physical fingerprint. METHODS The dry extract of Shuangye pipa granules was used as the main drug. The retention rate of total flavonoid， moisture absorption rate， dissolution rate， angle of repose and molding rate of the granules were selected as evaluation indexes. The single-factor test combined with the entropy weight method and Box-Behnken response surface design was used to optimize the molding process， and validation test was conducted. The physical fingerprints of 10 batches of Shuangye pipa granules prepared by the optimal process were comprehensively analyzed by eight secondary physical indexes （relative homogeneity， moisture， moisture absorption rate， Hausner ratio， angle of repose， bulk density， tap density and porosity）. RESULTS The optimal molding process of Shuangye pipa granules was as follows： soluble starch-maltodextrin-mannitol was 1∶1∶1 （m/m/m）， 95% ethanol was as wetting agent and the amount of it was 37%， the drug-assisted ratio was 1∶0.8 （m/m）， the drying temperature was 59 ℃， drying time was 28 min. The results of 3 validation tests showed that the average comprehensive score was 0.879 6， the RSD of which with prediction value （0.881 9 score） was 1.97%. The similarity between the physical fingerprints of 10 batches of Shuangye pipa granules and the control physical fingerprint was higher than 0.99. CONCLUSIONS The optimized molding process of Shuangye pipa granules is stable and feasible， and the physical property of Shuangye pipa granules is stable and controllable.
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Objective To establish a quantitative model to rapidly determine content of 3-butylphthalide in Angelicae Sinensis Radix based on near-infrared diffuse reflectance spectroscopy (NIR). Methods Totally 145 batches of samples of Angelicae Sinensis Radix from 14 areas of Gansu and Yunnan Provinces were collected and dried in the shade. With the content of 3-butylphthalide determined by RP-HPLC-DAD as reference, the NIR spectra of 145 batches of Angelicae Sinensis Radix were collected by integrating sphere diffuse reflectance, and the PLS (partial least squares) quantitative analysis model was established between 7415-4056 cm-1. Results The Rc (correlation coefficient between actual content and predicted content), RMSEC (the root-mean-square error of calibration), RMSEP (the root-mean-square error of prediction), Rcv (cross-validation correlation coefficient), RMSECV (the root-mean-square error of cross-validation), and average predicted recovery reached 0.976 7, 0.614 3, 0.706 5, 0.897 8, 1.155 4 and 102.08%, respectively. Conclusion This prediction model was accurate, reliable, and can be used to quantitatively determine the content of 3-butylphthalide in Angelicae Sinensis Radix.
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Objective To investigate the correlation between mineral elements in soil and quality of Angelica sinensis. Methods The contents of five index chemical compositions, volatile oil, ethanol soluble extractive in fifty-six batches of Angelica sinensis from twelve habitats, and fifteen kinds of mineral elements in corresponding soil were determined. Pearson correlation analysis, partial correlation analysis and stepwise regression analysis were used. Results The results showed that there were significant(P<0.05) or very significant correlation (P<0.01) between many kinds of mineral elements in soil and quality constituents of Angelica sinensis. Mg, Na, Cr and Hg were the dominant factor of ferulic acid; K, Zn, Ni, Mn, Na, Pb, Cu and Sb were the dominant factor of 3-butylphthalide;K, Zn, Ni, Na, Cd, Cr and Hg were the dominant factors of Z-butylidenephthalide; Fe, Ca, Zn, Ni, Mn, Pb and Cu were the dominant factor of Z-ligustilide; Zn, Mn, As and Cu were the dominant factors of linolic acid; Fe, K, Ca, Zn, Mn, Na, Pb, Cd, Cr, Cu, Sb and Hg were the dominant factors of volatile oil; Fe, K, Mg, Ni, Mn, Pb, As, Cu and Sb were the dominant factors of ethanol soluble extractive. Conclusion Mineral elements in soil have an important and stable influence on the quality formation of Angelica sinensis. K, Zn, Ni, Mn, Pb, Cu, Hg, Fe, Sb, Cr and Na are the dominant factors of several quality constituents of Angelica sinensis at the same time, which should be selectively examined during planting base selection and cultivation.