RESUMO
OBJECTIVE： To optimize the water extraction technology of classic formula Taohe chengqi decoction. METHODS： Based on single factor test， combined with response surface methodology and information entropy theory， the soaking time， solid-liquid ratio and extraction time were investigated. Using the contents of rhein， amygdalin， cinnamaldehyde and glycyrrhizic acid in Taohe chengqi decoction as indexes， information entropy theory was used to assign weight coefficients to each evaluation index and calculate the comprehensive score. Through Design-Expert 10 software， the interactions of each factor were analyzed. Water extraction technology was optimized， and validation test was also performed. RESULTS： According to information entropy theory， the weight coefficients of rhein， amygdalin， glycyrrhizic acid and cinnamaldehyde were located at 0.097 6， 0.363 2， 0.173 5 and 0.365 7. The results of interaction analysis showed that the material-liquid ratio had a greater impact on the comprehensive score. The optimal water extraction technology of Taohe chengqi decoction were determined as that soaking time was 60 min； the ratio of material to liquid was 1 ∶ 10 （g/mL）； total extraction time was 130 min （extracting for 3 times， lasting for 65， 33， 32 min each time）. The results of verification test showed that RSD of content of each index component and the comprehensive score was less than 3％. CONCLUSIONS： The optimal water extraction technology is proved to be stable and feasible， which can provide the basis for the further development and utilization of Taohe chengqi decoction.
RESUMO
OBJECTIVE： To compare the extraction effects of steam distillation method （SD） and extraction-azeotropic distillation coupling technology （WER） on the volatile oil from Citrus aurantium and Cyperus rotundus， so as to determine the suitable extraction method and improve the extraction technology of volatile components in Qizhi weitong granule. METHODS： SD and WER were used to extract the total volatile oil from C. aurantium and C. rotundus. t-test was conducted for the yield of volatile oil extracted by the two methods. GC-MS method was used to analyze the volatile oil， and the main components were determined. The relative content of main components was determined compared by area normalization method. GC-MS conditions included that Agilent HP-5 capillary column （30 m×0.25 mm ， 0.25 μm）， inlet temperature of 250 ℃， nitrogen as carrier gas， flow rate of 1 mL/min， split ratio of 20 ∶ 1， sample size of 2 μL， temperature programmed， electron bombardment， electron bombardment energy of 70 eV， scanning range of m/z 50-500. RESULTS： The appearance of volatile oil extracted by WER was more clear， with better product phase than that by SD. The average yield of volatile oil extracted by WER method were significantly higher than SD method （1.78％ vs. 1.48％， P＜0.01）. The volatile oil extracted by WER method and SD method contained 39 and 38 components， involving 38 common components. Among them， D-limonene， acetophenone， ketoenone and α-ketone were the main components of the total volatile oil from C. aurantium and C. rotundus， and the sum of the 4 main components was about 73.40％ （WER method） and 68.46％ （SD method） of the total components. CONCLUSIONS： Compared with SD method， WER method for extracting volatile oil from C.aurantium and C. rotundus is better in product， phase higher in yield and higher in content of active volatiles， and is more suitable for the extraction of volatile components in Qizhi weitong granule.
RESUMO
OBJECTIVE： To establish the method for content determination of volatile oil of Schizonepeta tenuifolia and Forsythia suspensa， and to optimize the extraction technology of the volatile oil. METHODS： The contents of β-pinene and pulegone were determined by GC method. The determination was performed on Hp-5 capillary column. The detector was hydrogen flame ion detector with programmed temperature. The sample size was 0.5 μL， the split ratio was 70 ∶ 1， the carrier gas was nitrogen， the inlet temperature was 250 ℃， the detector temperature was 280 ℃， the air flow rate was 390 mL/min， the hydrogen flow rate was 36 mL/min， the tail flow rate was 15 mL/min， and the nitrogen flow rate was 1 mL/min. Based on single factor test， orthogonal test combined with information entropy method were used to optimize the extraction technology of S. tenuifolia and F. suspensa using soaking time， extraction time， material-liquid ratio and forsythia grain size as factors， with the extraction amount of volatile oil， the content of β-pinene and pulegone and their comprehensive score as indexes. RESULTS： The linear range of β-pinene and pulegone 1.575-7.875（r＝0.999 9） and 1.892-9.46 μg（r＝0.999 7）， respectively. The limits of quantitation were 0.10 and 0.25 μg； the limits of detection were 0.03 and 0.08 μg； RSDs of precision， stability and reproducibility tests were less than 2％ （n＝6）； the recoveries were 97.77％-100.01％ （RSD＝0.93％，n＝9） and 96.47％-99.00％（RSD＝0.89％， n＝9）. The optimal extraction technology was soaking 2 h， extracting for 6 h， 10-fold water （mL/g）， half a clove of granularity. Under this condition， the extraction amount of volatile oil， the contents of β-pinene and pulegone were 3.6 mL， 1 450.4 mg， 127.6 mg， respectively. RSD were 1.62％， 0.20％， 1.42％. CONCLUSIONS： Established method is simple， accurate and reproducible， and the optimal extraction technology is stable and feasible.