Optimization of the preparation process of Soft-shelled turtle blood lyophilized powder using Box-Behnken response surface methodology / 中国药房

OBJECTIVE To optimize the preparation process of Soft-shelled turtle blood lyophilized powder （STBLP）， and to provide a reference for improving the availability and quality stability of soft-shelled turtle blood （STB）. METHODS STBLP was prepared with vacuum freeze-drying. Taking the solubility as the index， the preparation process parameters of STBLP were optimized by single factor experiment and Box-Behnken response surface method. RESULTS The optimal freeze-drying process for STBLP was obtained： pre-freezing time of 4 h， total drying time of 13 h （before at 0 ℃）， and resolution drying temperature of 25 ℃. The average solubility of 3 batches of STBLP prepared according to the optimal process was 95.72% （RSD＝0.68%， n＝3）， the relative error of which was －0.97% to the theoretical solubility （96.66%）. CONCLUSIONS Optimized lyophilization process in this study are stable and feasible， the solubility of the prepared sample is high.

Effect of Different Drying Methods on Volatile Components in Pseudostellariae Radix Based on GC-IMS / 中国实验方剂学杂志

ObjectiveTo compare the effects of different drying methods on volatile components of Pseudostellariae Radix. MethodThe samples were dried by different methods， including air drying， sun drying， hot air drying （40， 60， 80 ℃） and vacuum freeze drying. Gas chromatography-ion mobility spectrometry （GC-IMS） was used to compare the changes of volatile components in the samples after different treatments. The samples were incubated at 80 ℃ and 500 r·min-1 for 15 min， the injection temperature was 85 ℃， the injection volume was 200 μL， the flow rate of carrier gas was from 2 mL to 150 mL during 20 min， and the temperature of IMS detector was 60 ℃. SE-54 capillary column （0.32 mm×30 m， 0.25 μm） was used， the column temperature was 60 ℃， and the analysis time was 35 min. The differential spectra of volatile components were constructed and analyzed by principal component analysis （PCA）. ResultA total of 37 volatile components were identified from dried Pseudostellariae Radix. The number of compounds in descending order was ketones， aldehydes and alcohols. There were some differences in the volatile components in samples dried by different methods. And the volatile components in samples with sun drying， air drying and hot air drying at 40 ℃ were similar， compared with other drying methods， vacuum freeze drying and hot air drying at 80 ℃ had great effects on the volatile components of Pseudostellariae Radix， and the compounds in the samples with vacuum freeze drying were the least. ConclusionIn this study， GC-IMS for the detection and analysis of volatile components in Pseudostellariae Radix is established， which has the characteristics of high efficiency， nondestructive inspection and simple sample processing. This method can be used for the distinction of Pseudostellariae Radix dried by different methods. And hot air drying at 40 ℃ can effectively retain the volatile components of Pseudostellariae Radix， and achieve similar flavor to samples with sun drying and air drying.

Effects of Different Drying Methods on the Main Components of Forsythia suspensa Flowers / 中国药房

OBJECTIVE：To establish the method for the content det ermination of 4 components in Forsythia suspensa flowers by drying in shade ，vacuum freeze-drying ，oven（30，50，70 ℃）and sun ，so as to evaluate the effects of different drying methods on the main components of F. suspensa flowers and screen the optimal drying method. METHODS ：UPLC method was adopted. The determination was performed on Waters ACQUITY UPLC BEH C 18 column with mobile phase consisted of acetonitrile- 0.1％ phosphoric acid aqueous solution （gradient elution ）at the flow rate of 0.3 mL/min. The detection wavelength was set at 230 nm， and column was 35 ℃. The sample size was 1 μL. Euclidean closeness（C）i of different drying methods was calculated by TOPSIS comprehensive analysis method ，and the optimal drying method was defined. RESULTS ：The linear range of forsythiaside A ， rutin，forsythin，（+）-pinoresinol-4-O-β-D-glucopyranoside were 0.007 5-0.037 7，0.027 4-0.137 2，0.001 9-0.009 5，0.005 6-0.028 8 µg（all r＞0.999）. RSDs of precision ，stability（32 h）and reproducibility tests were all lower than 2％. The recoveries were 97.27％-102.53％，100.53％-104.11％，98.45％-104.02％，98.66％-104.82％，respectively；and all RSDs ＜3％（n＝3）. The contents were 1.645 8-4.987 9，11.730 2-20.978 0，0.875 5-2.005 0，2.366 0-5.535 7 mg/g. The content of forsythiaside A was the highest after drying at 30 ℃，rutin and （+）-pinoresinol-4- O-β-D-glucopyranoside were the highest after vacuum freeze-drying，forsythiaside was the highest after drying at 50 ℃ . Results of TOPSIS analysis showed that Ci of F. suspensa flowers by drying in shade ，vacuum freeze-drying ，oven（30，50，70 ℃）and sun were 0.079 9，0.553 5，0.495 4， 0.503 8，0.157 9，0.217 2，respectively；the order of Ci was vacuum freeze-drying ＞ 50 ℃ oven drying ＞ 30 ℃ oven drying＞sun drying ＞70 ℃ oven drying ＞ shade drying. CONCLUSIONS：Established method is simple ，reproducible and can be used for the content determination of 4 components in F. suspensa flowers. The samples are preferably dried by vacuum freeze-drying，followed by 50 ℃ oven drying ，30 ℃ oven drying ， and then dried in the sun and oven at 70 ℃ and finally in the shade.

Effects of Different Drying Methods on Contents of 4 Active Ingredients in Leaves of Eucommia ulmoides / 中国药房

OBJECTIVE:To investigate the effects of different drying methods on contents of active ingredients in leaves of Eu-commia ulmoides,and provide reference for establishing its drying methods after habitat harvesting. METHODS:Different drying methods [natural drying in the shade for 72 h,natural drying in the sunlight for 36 h,drying beside or over a fire(60℃6 h,80℃2 h,100℃1 h,120 ℃ 0.5 h),microwave vacuum freeze drying for 12 h,vacuum freeze drying for 12 h] were used for process-ing. HPLC was conducted to determine the contents of aucubin,geniposidic acid,chlorogenic acid and geniposide in samples and compare with the untreated fresh products. RESULTS:Contents of 4 ingredients in samples after the 2 freeze drying were close to these in fresh samples,which were higher than samples after other drying. CONCLUSIONS:Drying methods show significant ef-fects on the effective ingredients in leaves of E. ulmoides. Compared with natural drying in the shade and natural drying sunlight and drying beside or over a fire,microwave vacuum freeze drying and vacuum freeze drying can make better retention of the active ingredients in fresh leaves of E. ulmoides.

Effects of Different Drying Methods on Contents of 4 Active Ingredients in Leaves of Eucommia ulmoides / 中国药房

OBJECTIVE:To investigate the effects of different drying methods on contents of active ingredients in leaves of Eu-commia ulmoides,and provide reference for establishing its drying methods after habitat harvesting. METHODS:Different drying methods [natural drying in the shade for 72 h,natural drying in the sunlight for 36 h,drying beside or over a fire(60℃6 h,80℃2 h,100℃1 h,120 ℃ 0.5 h),microwave vacuum freeze drying for 12 h,vacuum freeze drying for 12 h] were used for process-ing. HPLC was conducted to determine the contents of aucubin,geniposidic acid,chlorogenic acid and geniposide in samples and compare with the untreated fresh products. RESULTS:Contents of 4 ingredients in samples after the 2 freeze drying were close to these in fresh samples,which were higher than samples after other drying. CONCLUSIONS:Drying methods show significant ef-fects on the effective ingredients in leaves of E. ulmoides. Compared with natural drying in the shade and natural drying sunlight and drying beside or over a fire,microwave vacuum freeze drying and vacuum freeze drying can make better retention of the active ingredients in fresh leaves of E. ulmoides.

The effect of pre-freezing method on crystallinity of alanylglutamine / 中国药学杂志

OBJECTIVE: To research and regulate the crystal quality of alanylglutamine for improving their stability and pharmacodynamics as well as vacuum freeze-drying efficiency. METHODS: Scanning electron microscopy (SEM), X-ray powder diffractometer (XRD), differential scanning calorimetry (DSC), and thermogravimetric analyzer (TG) as well as lyophilized experiments were used to investigate the effect of pre-freeze method on crystallinity and uniformity of particle size of alanylglutamine. RESULTS: The result of SEM revealed that the lyophilized alanylglutamine with accelerated pre-freeze method is small-size particle with low crystallinity. Then the lyophilized alanylglutamine with multi-step annealing pre-freeze method become uniformly large particle with high crystallinity. The RESULTS of XRD and DSC indicted that, comparing with the lyophilized alanylglutamine with accelerated pre-freeze method, the lyophilized sample with multi-step annealing pre-freeze method is easier to form the crystal medicine with uniform particle size, less crystal defects, high crystallinity. And the former has lower stability than the later. CONCLUSION: The final lyophilized experiment give us a CONCLUSION that using the multi-step annealing pre-freeze method can improve the freeze-drying efficiency and crystal quality of alanylglutamine, which to achieve the ultimate goal of cost and energy saving.

Effect of different drying methods on quality of Rhizoma Gastrodiae / 中成药

AIM: To evaluate the quality of Rhizoma gastrodiea processed by different drying methods. METHODS: Vacuum freeze drying and oven drying were adopted. The content of gastrodin was determined by RP-HPLC. RESULTS: The content of gastrodin of Rhizoma Gastrodiae processed by vacuum freeze drying was significantly higher than that by boil with water and oven drying. CONCLUSION: The method of vacuum freeze (drying) can prevent Rhizoma Gastrodiae from degradation of gastrodin, to keep the appearance, to make Rhizoma Gastrodiae convenient for further processing.