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Objective:To screen the optimal process of ambi-extracting of Xinyi Powder and inclusion of volatile oil.Methods:Single factor experiment was used to optimize the extraction process of Xinyi Powder by taking crushing particle size, extraction times, the amount of water added and extraction time as the investigation factors. L 9(3 4) orthogonal test was used to optimize the inclusion process of volatile oil in Xinyi Powder. Results:The optimal extraction process of ambi-extracting of Xinyi Powder was as follows: the slices were not crushed, 10 times the amount of water was added, and extracted for 3 hours; the best inclusion process of volatile oil as follows: β-cyclodextrin:water=1:25, β-cyclodextrin:volatile oil=6:1, inclusion temperature 35 ℃, inclusion time 3 hours.Conclusion:The ambi-extracting process and volatile oil inclusion process are simple, stable and feasible.
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By reviewing ancient materia medica and combining with modern literature， the textual research of Magnoliae Flos has been conducted to verify the name， origin， producing area， harvesting and processing methods， in order to provide basis for the selection and use of this herb in the development of famous classical formulas. After the textual research， it could be seen that the correct name of Magnoliae Flos was Xinyi in the past dynasties， meaning spicy flower buds. The main original plants used in past dynasties are Magnolia denudata and M. biondii. The history of the research on its scientific name in recent times is complicated， many foreign scholars have given several different scientific names， but most of them are inconsistent with the actual situation of Magnoliae Flos used in ancient China， because foreign scholars failed to collect the original plants of Magnoliae Flos for accurate identification. Before the Ming dynasty， Magnoliae Flos was mainly produced in Shaanxi， and then the recorded production areas gradually increased. After the founding of the People's Republic of China， the products produced in Henan named M. biondii were highly respected， and Henan was regarded as authentic producing area， and because of the collection and distribution through Yuzhou， it was customarily called Huichunhua. In ancient times， the harvesting period of Magnoliae Flos mostly concentrated in the first and second months of the lunar calendar， and the flower buds of M. biondii were also recommended to be used as medicine， but nowadays the flower buds are mostly collected in winter and spring， and those with dry buds， large size， yellow-green color， tight inner petals， fragrant smell， and no impurities are preferred. In the past dynasties， raw products were the mainstream， and there were also frying， soaking and so on. Based on the results， it is suggested that the flower buds of M. biondii should be used in the development of famous classical formulas. If the original formula does not specify the processing requirements， the raw products can be used as medicine.
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Objective To analyze the volatile components of Magnoliae Flos, Magnoliae Flos kernels, and Magnoliae Flos bracts and compare the differences of these components in order to provide a theoretical basis for the usage of kernels of Magnolia Flos in classical famous prescriptions. Methods The volatile components were extracted by steam distillation and analyzed by gas chromatography-mass spectrometry (GC-MS). The volatile components in different parts of Magnoliae Flos were identified by searching the retention index in the mass spectrometry database. The relative content of volatile components was calculated by peak area normalization method, and the data of GC-MS was further proceeded by principal component analysis (PCA). Results The average volatile components content in Magnoliae Flos, Magnoliae Flos kernels, and Magnoliae Flos bracts was 1.70%, 6.79%, and 0.45%, respectively. The numbers of compounds identified by GC-MS in those three different parts were 87, 82, and 85, respectively. These compounds mainly included terpene olefins and alcohols type chemicals. PCA method was then applied to process the GC-MS data and distinguish different parts and habitats of Magnoliae Flos. Conclusion The volatile components in the kernels of Magnoliae Flos were generally the same as those of Magnoliea Flos, while the content of which was much higher than those of whole flower bud of Magnoliae Flos. The results indicated that it was rational to use the kernels of Magnolia Flos in classical famous prescriptions.
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Objective To establish the fingerprint of Magnoliae Flos and Asari Radix et Rhizoma of Liujing Toutong Tablets (LTT), provide the basis for the evaluation of the quality of LTT. Methods Aglient DB-WAX (20 m × 0.18 mm, 180 μm) gas chromatography column, select the appropriate temperature conditions, the determination of the 11 batch of Magnoliae Flos, Asari Radix et Rhizoma, the use of SPSS clustering analysis and chromatographic fingerprint evaluation system (2004A version) the establishment of Xinyi medicine fingerprints, and through the Agilent 7890A-5975C gas quality for instrument on the common peaks were identified. Results The 11 batches of samples were measured and SPSS cluster analysis of 10 batches of medicinal materials were clustered into one group, and the establishment of Xinyi medicine GC fingerprint, the similarity was more than 0.9, a total of 22 common peaks, which belongs to the whole party into 14 components, medicinal unique ingredients 8; 10 batches of Asarum medicinal materials were clustered into one group, and the establishment of Asarum GC fingerprint, the similarity was more than 0.9, a total of 11 common peaks, which belongs to the whole Party composition for 4, 7 for a particular component of medicinal materials. Conclusion This method has strong specificity, high accuracy, good repeatability, and provide the basis for quality control of Herba Magnoliae Flos and Asari Radix et Rhizoma.
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Objective To optimize the extraction process of mixed volatile oil from Forsythiae Fructus, Saposhnikoviae Radix and Magnoliae Flos and inclusion process of β-cyclodextrin (β-CD). Methods With yield ratio of volatile oil as evaluation index, single factor experiments were used to study the extraction process of volatile oil;saturated aqueous solution was used, with inclusion rate of volatile oil as index, and orthogonal design was adopted to examine effects of charge ratio of volatile oil and β-CD, inclusion temperature and inclusion time on the inclusion process; X-ray scattering technique, infrared spectroscopy and scanning electron microscopy were used to characterize the inclusion compound. Results The optimum extraction process of volatile oil was soaking fine powder extracted 5 hours with 10 folds the amount of water. The optimum conditions of inclusion process were as follows:mixed ratio of volatile oil (mL) and β-CD (g) was 1:10; inclusion temperature was 50 ℃; the inclusion time was 2 h. X-ray scattering technique, infrared spectroscopy and scanning electron microscopy proved the inclusion compound had been formed. Conclusion Optimum extraction and inclusion processes are stable and feasible, and can provide research foundation for further research and development of preparation.
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OBJECTIVE:To study the effect of HP-β-CD on solubility of 1,8-oxido-p-menthane in volatile oil of magnoliae flos,and optimize the extraction technology of Xinzhi nasal drops. METHODS:Steam distillation method was adopted to extract the volatile oil in magnoliae flos. Using the content of 1,8-oxido-p-menthane in volatile oil of magnoliae flos as index,HPLC was adopted to determine the effects of HP-β-CD with different concentration on solubility of 1,8-oxido-p-menthane in volatile oil of magnoliae flos. Using the comprehensive scores of imperatorin and extract yield as indexes,orthogonal test was used to optimize the amount of ethanol,volume fraction and extraction time in extraction technology of Xinzhi nasal drops. Verification test was car-ried out. RESULTS:50% HP-β-CD aqueous solution can improve the solubility of 1,8-oxido-p-menthane to 7.6 times. The optimal extraction technology of Xinzhi nasal drops was as follow as 10-fold 80% ethanol,extracting twice,1 h every time. In verification test,the average content of imperatorin was 0.078%(RSD=2.01%,n=3),and extract yield was 10.80%(RSD=1.85%,n=3). CONCLUSIONS:HP-β-CD shows good solubilization effect on the 1,8-oxido-p-menthane in volatile oil of magnoliae flos,and the optimized extration technology for Xinzhi nasal drops is feasible.
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Objective: To optimize the extraction technology of Saposhnikoviae Radix, Perillae Folium, Magnoliae Flos, Armeniacae Amarum Semen, and honey-fried Ephedrae Herba in Xiaochuan Decoction by information entropy theory. Methods: With the contents of prem-O-glucosylcimifugin, 4'-O-beta-glucopyranosyl-5-O-methylvisamminol, amygdalin, and the yield of extract as comprehensive evaluation indexes in order to optimize the extraction process parameters of orthogonal test, the weight coefficient of each index was determined by the information entropy weight method. Results: Optimum extraction technology was as follows: reflux extraction for 3 times with 10 fold water, for 1.5 h each time. Conclusion: The optimized method is stable and reliable, and can provide the reference for further development and utilization of the formula.
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OBJECTIVE:To study the pharmacokinetics of magnolin in rats. METHODS:High performance liquid chromatog-raphy(HPLC)was adopted. The determination was performed on Kromasil C18 with mobile phase consisted of acetonitrile-tetrahy-drofuran-water (39∶1∶60),at the flow rate of 1.0 ml/min,with the measurement wavelength of 278 nm,column temperature of 35 ℃ and the sample size of 20 μl. 8 Wistar rats were docked to collect blood from the caudal vein before administration [10 mg(medicinal materials)/kg] and 0.25,0.5,0.75,1,1.5,2,4,8,12 and 20 h after administration,to determine the concentra-tion of the drug in blood. DAS2.1.1 software was used to calculate pharmacokinetic parameters. RESULTS:In the determination of magnolin,the mass concentration linear range was found to be 0.05-10.00 μg/ml(r=0.999 5);the RSD of precision test and sta-bility test were less than 13%(n=6);relative recovery rate was 97.32%-102.15%(n=6);extraction recovery rate was 84.63%-90.02%;t1/2α of magnolin in rats was(0.48±0.22)h,t1/2β was(7.96±2.57)h,CL/F was(0.09±0.032)L/(h·kg),and AUC0-20 h was(944.43±212.83)mg·h/L. CONCLUSIONS:This method conforms to the requirements for the determination of bio-logical samples with respect to precision,stability and accuracy. Magnolin demonstrates a good linear relationship between AUC0-20 h and the dose in rats,with the process compatible with two-compartment model.
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Objective: To study the optimal preparation process of nasal ethosome sprays of volatile oil in Magnoliae Flos after removing a-terpineol alcohol (VOMF) and to investigate its characteristics and mucociliotoxicity. Methods: The 5% VOMF ethosome was prepared with ultrasonic injection method, and the orthogonal test was used to design the formulations of VOMF ethosome which was evaluated by entrapment efficiency and drug loading as indexes. Quality evaluation included appearance, particle diameter distribution, Zeta potential, entrapment efficiency (EE), and stability. The persistent vibration duration (PVD) and percentage of persistent vibration (PPV) in situ toad oral palate cilia were observed to evaluate the mucociliotoxicity administered by various constituents. Results: The optimal preparation was 1.5% of phospholipid, 0.15% of cholesterol, and 36% of ethyl alcohol. The quality evaluation showed that the ethosome was round and uniform, while the mean Zeta potential was (-55.9 ± 2.1) mV. The average particle diameter was getting smaller, the EE had no change, and no mucociliotoxicity was found after spraying. Conclusion: Ultrasonic injection method used to prepare VOMF ethosome is rational and stable and it can be used for nasal administration.
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A high performance liquid chromatography-electrospray ionization mass spectrometry- charged aerosol detection ( HPLC-MS-CAD) method was established for the simultaneous quantitative analysis of four Lignans in Magnoliae Flos extract. The components were separated on a YMC-Pack ODS-A column (250 mm× 4. 6 mm, 5 μm) by gradient elution with methanol and water as the mobile phase at aflow rate of 1. 0 mL/min. Then the elution solution was routed into MS equipment at a flow rate of 0. 3 mL/min and CAD detector at a flow rate of 0. 7 mL/min by a split ratio of 3:7 for the further detection. The column temperature was 25 ℃ and the detection wavelength was 278 nm. A method was developed for the quantitative analysis of muti-components by single maker ( QAMS) to determine pinoresinol dimethylether, magnoli, 1irioresinol B dimethylethe and epi-magnoli A . Magnoli was selected as internal standard and the relative correction factors ( RCF) of the four Lignans were calculated. The contents of the four Lignans in Magnoliae Flos extract were determined by both external standard method and QAMS. The QAMS method was evaluated by comparison of its assay result and that of external standard method. Under the selected chromatographic condition, the limits of detection of pinoresinol dimethylether, magnoli, lirioresinol B dimethylethe and epi-magnoli A were 0. 34, 0. 55, 0. 50 and 0. 58 mg/L, respectively, while the linear range were within 6. 8-270 mg/L, 11-546 mg/L, 2. 0-101 mg/L and 2. 3-116 mg/L. The recoveries ( n=9 ) were 98. 2%-99. 5%, and the correlation coefficient were 0 . 9995-0 . 9998 . No significant differences were found between the quantitative results of external standard method and QAMS method. The developed method is accurate, feasible, and can be used for quality evaluation of Magnoliae Flos .