[关键词]
[摘要]
目的 建立当归破壁饮片沸腾干燥动力学模型,测定其干燥动力学参数,比较不同温度沸腾干燥产品质量,为优化干燥工艺参数提供参考。方法 采用沸腾干燥对当归破壁饮片软材进行干燥,研究其在60、75、90 ℃条件下的干燥特性;应用Weibull函数对其干燥曲线进行拟合;根据Fick扩散定律和Arrhenius方程求算干燥过程水分有效扩散系数和活化能;运用HPLC测定不同干燥温度当归破壁饮片挥发成分含量,测定指纹图谱并计算相似度;测定物理属性指标,建立以15个物理指标(D90、粒度分布范围、粒度分布宽度、相对均齐度Iθ、松密度、振实密度、颗粒间孔隙率、压缩度、比表面积、孔体积、休止角、平板角、色度L*、a*、b*)来表征当归破壁饮片的物理质量属性和构建物理指纹图;从物理和化学属性多角度综合评价不同干燥温度对其质量的影响。结果 当归破壁饮片沸腾干燥属于降速干燥过程,温度越高,达到目标水分控制点的时间越短;沸腾干燥过程中水分比随时间变化服从Weibull函数分布(R2为0.991 1~0.999 0,χ2为9.380 5×10−5~6.030 0×10−4,RMSE为0.007 7~0.021 3);当归破壁饮片沸腾干燥的水分有效扩散系数(moisture effective diffusion coefficients,Deff)值(1.84×10−3~6.90×10−3 m2/s)和活化能(activation energy,Ea)值为39.70 kJ/mol。不同温度沸腾干燥的当归破壁饮片挥发性成分含量有一定差异,随温度升高,挥发性成分含量略有降低;HPLC指纹图谱及物理指纹图谱与对照图谱的相似度较高(相似度均>0.90)。结论 Weibull函数能较好预测当归破壁饮片沸腾干燥过程中的水分迁移规律,不同温度沸腾干燥的当归破壁饮片整体质量差异不大,指纹图谱相似度均符合要求;对指导产品生产过程中干燥工艺参数优化和提高品质具有重要意义。
[Key word]
[Abstract]
Objective To establish a kinetic drying model for the fluidized drying of ultrafine granular powder (UGP) of Danggui (Angelicae Sinensis Radix, ASR), determine their drying kinetic parameters, compare the quality of product dried at different temperatures, and provide reference for the optimization of drying process parameters. Methods Fluidized drying was used to dry the soft material of UGP of ASR, and its drying characteristics were studied under 60, 75, 90 ℃. Weibull function was used to fit the drying curve. The effective diffusivity and activation energy of water during drying were calculated according to Fick’s diffusion law and Arrhenius equation. HPLC was used to determine the content of volatile components in the UGP of ASR at different drying temperatures. The fingerprint of UGP of ASR was determined and the similarity was calculated. Determination the physical properties, which fifteen physical indexes (D90, particle size distribution range, particle size distribution width, relative homogeneity Iθ, bulk density, vibration density, porosity between particles, compression degree, specific surface area, pore volume, angle of reposition, angle of plate, color of L*, a*, b*) were established to characterize the physical quality of UGP of ASR and used to construct physical fingerprinting. The effects of different drying temperatures on its quality were comprehensively evaluated from the physical and chemical properties. Results The fluidized drying of UGP of ASR belongs to a slow drying process. The higher the temperature, the shorter the time to reach the target water control point. During fluidized drying process, water ratio over time followed Weibull function distribution (R2 = 0.991 1—0.999 0, χ2 = 9.380 5 × 10−5—6.030 0 × 10−4, RMSE = 0.007 7—0.021 3). The moisture effective diffusion coefficients (Deff) for fluidized drying of UGP of ASR values (1.84 × 10−3—6.90 × 10−3 m2/s) and activation energy (Ea) values were 39.70 kJ/mol. The volatile component content of UGP of ASR fluidized drying at different temperature has a certain difference, with the increase of temperature, the content of volatile components decreased slightly. Both HPLC and physical fingerprints showed high similarity to the control pattern and its similarity were all above 0.90. Conclusion Weibull function could better predict water migration rule during fluidized drying of UGP of ASR. There was no significant difference in the overall quality of UGP of ASR fluidized drying at different temperatures. The similarity of HPLC and physical fingerprints all conform to the requirements. It is of great significance to guide the optimization of fluidized drying process parameters and improve product quality in the production process.
[中图分类号]
R283.6
[基金项目]
国家企业技术中心(发改高技〔2020〕1918号);中药破壁饮片国家地方联合工程研究中心(发改办高技〔2019〕180号);广东省中药破壁饮片工程实验室(粤发改创新函[2018]3149号)