CN103961717A - Preparation method of decomposed bighead atractylodes rhizome volatile oil/beta-cyclodextrin inclusion compound - Google Patents
Preparation method of decomposed bighead atractylodes rhizome volatile oil/beta-cyclodextrin inclusion compound Download PDFInfo
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Abstract
The invention relates to the field of inclusion compound preparation, and particularly relates to a preparation method of a decomposed bighead atractylodes rhizome volatile oil/beta-cyclodextrin inclusion compound. The preparation method comprises the following steps: step one. accurately weighing beta-CD, adding hot water, and stirring so as to dissolve the beta-CD, thus obtaining a beta-CD saturated solution; reducing the temperature of the saturated solution to an internal temperature of a constant temperature stirring water bath kettle, putting in the 30-60 DEG C constant temperature stirring water bath kettle, stirring at a constant temperature, slowly adding decomposed bighead atractylodes rhizome volatile oil dissolved by using absolute ethyl alcohol, and stirring for above 0.5 hour, wherein the mass ratio of the beta-CD to the decomposed bighead atractylodes rhizome volatile oil is (4-10): 1; and step two. taking out, putting at a room temperature, then refrigerating and staying overnight; and carrying out suction filtration, washing prepared solid materials by using distilled water and an organic solvent, drying in a 40-DEG C constant temperature drying box, and grinding so as to obtain the decomposed bighead atractylodes rhizome volatile oil/beta-cyclodextrin inclusion compound. The preparation method can be used for effectively obtaining the decomposed bighead atractylodes rhizome volatile oil/beta-cyclodextrin inclusion compound which is high in inclusion rate and oil content, good in solubleness, convenient to store and stable in nature.
Description
Technical field
The present invention relates to the preparation field of clathrate, specifically a kind of preparation method of decomposing rear Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride.
Background technology
Rhizoma Atractylodis Macrocephalae volatile oil antitumor action is definite, and side effect is little.Decompose forward and backward volatile oil tumor cell line is all had to the inhibitory action of killing and wounding, and there is inducing tumor cell generation apoptotic effect.Rhizoma Atractylodis Macrocephalae volatile oil after decomposing is developed to clinical applicable dosage form, is a key technique in medicinal R&D process.
Beta-schardinger dextrin-(β-CD) inclusion technique is a kind of new technique that is applied at present field of traditional Chinese, adopt beta-schardinger dextrin-and traditional medicine volatile oil effect to form a kind of releasable pressed powder, reduce the volatilization of volatile oil, the clathrate dissolubility of making obviously increases, can be made into the dosage forms such as tablet, capsule, Emulsion, there is vast potential for future development.
At present, yet there are no relevant report prepared by the rear Rhizoma Atractylodis Macrocephalae volatile oil of decomposition and Benexate Hydrochloride.
Summary of the invention
The present invention aims to provide a kind of preparation method of decomposing rear Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride, for the research and development of anti-cancer agent preparation provide medicinal intermediate.
The present invention is achieved by the following technical solutions: the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposing, the steps include:
I. accurately take β-CD, heating water stirs it is dissolved, and makes β-CD saturated solution; Be down to constant temperature until the temperature of saturated solution and stir after water-bath kettle temperature, be placed in 30～60 DEG C of constant temperature and stir constant temperature stirring in water-bath, slowly add with Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution, more than stirring 0.5h; β-CD is 4～10:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil;
II. take out and put to room temperature, subsequent cold storage spends the night; Sucking filtration, distilled water and organic solvent washing for the solid material making, 40 DEG C of thermostatic drying chamber inner dryings, grind and obtain the rear Rhizoma Atractylodis Macrocephalae volatile oil-beta cyclodextrin clathrate of decomposition.
In step I of the present invention, adopt hot water to make β-CD saturated solution, this hot water all can as long as the hot water that temperature stirs the arbitrary temp of water-bath kettle temperature higher than constant temperature.The constant temperature that the present invention adopts stirs water-bath method for general ultrasonic method, and in ultrasonic method enclose process, after many decomposition, Rhizoma Atractylodis Macrocephalae volatile oil floats on β-CD saturated aqueous solution surface, is difficult to directly contact well with β-CD, causes enclose Efficiency Decreasing; And constant temperature stirring water-bath method enclose efficiency is very high.
Further, described β-CD is 6:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil.The inclusion rate of the clathrate that this ratio is made is higher.
Further, constant temperature stirring water-bath kettle temperature is 60 DEG C.Do not affecting under the suitable high temperature of volatile oil character (60 DEG C), the motion aggravation of β-CD and volatile oil molecule, collision probability strengthens, and is conducive to the carrying out of enclose process, and the clathrate inclusion rate making is higher.
Further, the described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:8～10(w/v).Because Rhizoma Atractylodis Macrocephalae volatile oil after decomposing is water insoluble, but be soluble in dehydrated alcohol, and dehydrated alcohol is soluble in water, therefore in order to decompose the enclose of rear Rhizoma Atractylodis Macrocephalae volatile oil and β-CD, adopt in theory the mass volume ratio of Rhizoma Atractylodis Macrocephalae volatile oil and dehydrated alcohol after the decomposition of arbitrary proportion all can, if but the amount of dehydrated alcohol is too many in enclose process, can compete the binding site of volatile oil and β-CD, cause inclusion rate to reduce; If the amount of dehydrated alcohol very little, volatile oil can not finely dissolve, and affects contacting of volatile oil and β-CD, thereby reduces inclusion rate; Therefore think and adopt 1:8～10(w/v) can make volatile oil well dissolve, can not form too much influence to the inclusion rate of clathrate again.
Further, add with mixing time after Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution be 1.5h.This mixing time makes volatile oil fully contact with β-CD, and the clathrate inclusion rate making is higher.
Further, to be selected from boiling range be any one in the petroleum ether, dehydrated alcohol, ether, ethyl acetate of 30～60 DEG C to the organic solvent in step II.The effect of organic solvent is to wash away the not volatile oil of enclose of clathrate surface, and above-mentioned organic solvent is the organic solvent that volatile oil therein can excellent dissolution.
Adopt the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition of the present invention, can effectively obtain that inclusion rate is high, oil content is high, dissolubility is good, be convenient to preserve, Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after the decomposition of stable in properties, the inclusion rate of preparation method is at least more than 80%, and the oil content of clathrate is at least more than 18%; This clathrate can reach the high retention rate of volatile oil active ingredient, is convenient to the exploitation of clinical preparation.
experiment: the preparation research of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposing
1. instrument and material
Varian Cary Eclipse spectrofluorophotometer; Shimadzu UV-1601 spectrophotometer; Olympus optical microscope; HJS-8 digital display constant temperature stirs water-bath; SK250H Ultrasound Instrument; KDC-1044 low speed centrifuge; FA-1004 analytical balance, DHG-9123A type electric heating constant-temperature blowing drying box; GM-0.33 II vacuum diaphragm pump; Sucking filtration device; Mortar; 0.22 μ m micropore filtering film, β-CD, ethanol, petroleum ether (30 ~ 60 DEG C), deionized water.
2. Rhizoma Atractylodis Macrocephalae volatile oil preparation after decomposing
3. Rhizoma Atractylodis Macrocephalae volatile oil after decomposing/β-
cyclodextrin clathrate preparation
Based on the key influence factor of inclusion rate and oil content etc.,, respectively get 3 levels and carry out Orthogonal Experiment and Design as investigation factor taking mass ratio, mixing time, the enclose temperature (constant temperature stirs water-bath kettle temperature) of decomposing rear Rhizoma Atractylodis Macrocephalae volatile oil and β-CD.According to preliminary experiment result, this experiment arranges factor level in table 1.
The β-cdinclusion technique orthogonal test factor level of Rhizoma Atractylodis Macrocephalae volatile oil after table 1 decomposes
4. solution preparation
4.1 decompose rear Rhizoma Atractylodis Macrocephalae volatile oil stock solution preparation
Precision takes 100mg decompose after Rhizoma Atractylodis Macrocephalae volatile oil, go in 100 mL volumetric flasks, be settled to 100mL scale with dehydrated alcohol, make Rhizoma Atractylodis Macrocephalae volatile oil stock solution after the decomposition that concentration is 1mg/mL.
the preparation of β-CD ethanol solution
Precision takes β-CD30 mg, adds 10mL dehydrated alcohol, and sonic oscillation 10 min place 24h for 4 DEG C.Next day, with the centrifugal 10min of 2500 r/min, get the supernatant and get final product.
the preparation of volatile oil need testing solution in clathrate
Precision takes Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion 30 mg, adds 10mL dehydrated alcohol, and sonic oscillation 10 min place 24h for 4 DEG C.Next day, with the centrifugal 10min of 2500 r/min, get the supernatant and get final product.
the assay of volatile oil in clathrate
5.1 decompose rear Rhizoma Atractylodis Macrocephalae volatile oil spectral scan
Rhizoma Atractylodis Macrocephalae volatile oil stock solution after the decomposition that step 4.1 makes, at excitation wavelength 300 ~ 700nm, carries out spectral scan within the scope of emission wavelength 400 ~ 700nm, slit width is 5nm.Fluorescence spectrum is shown in Fig. 1.
As shown in Figure 1, after decomposing, Rhizoma Atractylodis Macrocephalae volatile oil is at excitation wavelength (λ ex) 396nm, and emission wavelength (λ em) 485nm place launches hyperfluorescence.
specification Curve of Increasing
Rhizoma Atractylodis Macrocephalae volatile oil stock solution 0.025,0.5,1.0,2.0 after the decomposition that accurate absorption step 4.1 makes respectively, 3.0 and 4.0mL in 5 ml volumetric flasks, add dehydrated alcohol to scale, making Concentraton gradient is 0.05,0.1, the volatile oil series reference substance solution of 0.2,0.4,0.6 and 0.8 mg/mL.Taking dehydrated alcohol as blank, be respectively 396nm and 485nm place mensuration fluorescence intensity exciting with emission wavelength, experimental result is in table 2.Taking fluorescence intensity as vertical coordinate, concentration (mg/mL) is abscissa simultaneously, and Criterion curve, the results are shown in Figure 2.
Result shows, decomposes rear volatile oil alcoholic solution good in 0.05 ~ 0.8mg/mL scope internal linear relation, regression equation F=38.68 C+7.01(r=0.9995).
Rhizoma Atractylodis Macrocephalae volatile oil concentration and fluorescence intensity corresponding relation after table 2 decomposes
| Concentration (mg/mL) | 0.05 | 0.1 | 0.2 | 0.4 | 0.6 | 0.8 |
| Fluorescence intensity | 8.94 | 10.88 | 14.44 | 22.71 | 30.41 | 37.66 |
5.3 decompose rear Rhizoma Atractylodis Macrocephalae volatile oil/β-cdinclusion technical study
Taking inclusion rate and oil content as investigating index, according to table 1, adopt L
9(3
4) carry out orthogonal design, according to volatile oil content testing method in step 5.1 and 5.2 clathrates of setting up, the inclusion rate and the oil content that calculate the rear Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion of gained decomposition under each experiment condition, preferably the process conditions of rear Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion are decomposed in preparation.Result of study is in table 3 and table 4.
Rhizoma Atractylodis Macrocephalae volatile oil/β-cdinclusion technique orthogonal experiments after table 3 decomposes
| Serial number | A: proportioning | B: time | C: temperature | D | Inclusion rate | Oil content | Comprehensive grading |
| 1 | 1 | 1 | 1 | 1 | 69.16 | 18.52 | 79.86 |
| 2 | 1 | 2 | 2 | 2 | 60.39 | 16.00 | 69.58 |
| 3 | 1 | 3 | 3 | 3 | 86.51 | 22.46 | 99.27 |
| 4 | 2 | 1 | 2 | 3 | 80.73 | 18.77 | 90.69 |
| 5 | 2 | 2 | 3 | 1 | 87.31 | 19.54 | 97.40 |
| 6 | 2 | 3 | 1 | 2 | 86.83 | 21.47 | 98.68 |
| 7 | 3 | 1 | 3 | 2 | 80.76 | 18.85 | 90.78 |
| 8 | 3 | 2 | 1 | 3 | 62.03 | 9.73 | 65.50 |
| 9 | 3 | 3 | 2 | 1 | 68.08 | 14.16 | 74.99 |
| K 1 | 248.71 | 261.33 | 244.04 | 252.25 | |||
| K 2 | 286.77 | 232.48 | 235.26 | 259.04 | |||
| K 3 | 231.27 | 272.94 | 287.45 | 255.46 | |||
| R | 55.5 | 40.46 | 52.19 | 6.79 |
Note: comprehensive grading=80% × inclusion rate/maximum inclusion rate+20% × oil content/maximum oil content
Input amount × 100% of actual oil content/volatile oil in inclusion rate=clathrate
The amount of volatile oil (ml)/clathrate weight (g) × 100% in oil content=clathrate
Table 4 decomposes the variance analysis of Rhizoma Atractylodis Macrocephalae volatile oil/β-cdinclusion technique
| Soruces of variation | Sum of deviation square | Degree of freedom | Variance | F value | P value |
| A | 536.99 | 2 | 268.50 | 69.74 | ＜0.05 |
| B | 289.35 | 2 | 144.68 | 37.58 | ＜0.05 |
| C | 520.59 | 2 | 260.30 | 67.61 | ＜0.05 |
| D | 7.69 | 2 | 3.85 | 1.00 | ＞0.05 |
Result in analytical table 3, each factor to the size order that decomposes rear inclusion essential oil influential effect is: A > C > B > D, factor A(mass ratio) K2> K1 > K3, factor B (mixing time) K3 > K1 > K2, factor C (enclose temperature) K3 > K1 > K2.
Result in analytical table 4, has significant difference, there was no significant difference between three levels of D factor between A, B, tri-each levels of factor of C.To sum up draw, after decomposing, Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion the best conditions of preparation pr ocess is A2B3C3D1, adds the beta-schardinger dextrin-of 6 times of amounts, and 60 DEG C are stirred 1.5 h.With this understanding, prepare Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion after 3 batches of decomposition, and volatile oil in clathrate is carried out to assay, the results are shown in Table 5.
After 3 batches of decomposition of table 5, Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion is prepared the result
| Sample | 1 | 2 | 3 | Meansigma methods | RSD（%） |
| Inclusion rate | 87.56 | 87.88 | 88.17 | 87.87 | 0.35 |
| Oil content | 21.13 | 21.29 | 20.98 | 21.13 | 0.73 |
In table 5, result shows, after decomposition, under Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion the best conditions of preparation pr ocess, enclose is tested in triplicate, the RSD(% of inclusion rate and oil content) be all less than 0.8%.Illustrate that this preparation process condition stablizes feasible.
rhizoma Atractylodis Macrocephalae volatile oil after decomposing/beta-CD inclusion characterizes
6.1 ultraviolet spectral analysis
Respectively taking water and dehydrated alcohol as solvent, with β-CD, decompose after Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion, decompose after Rhizoma Atractylodis Macrocephalae volatile oil and decompose after the physical mixture (1: 6 of Rhizoma Atractylodis Macrocephalae volatile oil and β-CD, w: w) be object, adopt ultraviolet spectral technique, scan in 190 ~ 400nm wave-length coverage.Scanning spectra is shown in Fig. 3.
As can be seen from Figure 3, after decomposing, in Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion, the characteristic absorption peak of volatile oil disappears, and illustrates that decomposing rear volatile oil forms good clathrate with β-CD.
spectrofluorimetry
Respectively taking dehydrated alcohol and water as solvent, taking decompose rear Rhizoma Atractylodis Macrocephalae volatile oil and decompose after Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion as object, adopt fluorescent spectrometry, slit width is 5nm, in 385 ~ 600nm wave-length coverage, carry out spectral scan, scanning spectra is shown in respectively Fig. 4 and Fig. 5.
As seen from the figure, compared with volatile oil without enclose, after decomposing there is larger variation in the peak shape of Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion, and blue shift has occurred maximum emission wavelength.
micro-imaging method
Get β-CD and decompose after Rhizoma Atractylodis Macrocephalae volatile oil/β-CD clathrate each a little, be prepared into suspension with distilled water, film-making, is placed in digital optical microphotograph Microscopic observation (40 × 10), result is shown in respectively Fig. 6 and Fig. 7.
In figure, result shows, β-CD is the tabular transparent crystal of rule, and the clathrate of oil-containing is the black powder that includes yellow transparent shape material, illustrates that clathrate forms.
Brief description of the drawings
Fig. 1 is the fluorescence spectrum of Rhizoma Atractylodis Macrocephalae volatile oil stock solution after decomposing; In figure, 1 is excitation spectrum, and 2 is emission spectra.
Fig. 2 is Rhizoma Atractylodis Macrocephalae volatile oil fluorescence standard curve after decomposing.
Fig. 3 is Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion after β-CD, decomposition, decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil and decompose the UV contrast collection of illustrative plates of the physical mixture of rear Rhizoma Atractylodis Macrocephalae volatile oil and β-CD; 1 physical mixture for Rhizoma Atractylodis Macrocephalae volatile oil after decomposing and β-CD in figure, 2 is Rhizoma Atractylodis Macrocephalae volatile oil after decomposing, and 3 is Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion after decomposing, and 4 is β-CD.
Fig. 4 is the fluorescent scanning spectrogram of Rhizoma Atractylodis Macrocephalae volatile oil in 385 ~ 600nm wave-length coverage after decomposing.
Fig. 5 is the fluorescent scanning spectrogram of Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion in 385 ~ 600nm wave-length coverage after decomposing.
Fig. 6 is the microscope imaging figure (400 ×) of β-CD.
Fig. 7 is the microscope imaging figure (400 ×) of Rhizoma Atractylodis Macrocephalae volatile oil/beta-CD inclusion after decomposing.
Detailed description of the invention
embodiment 1
After decomposing, the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride, the steps include:
I. accurately take β-CD, heating water stirs it is dissolved, and makes β-CD saturated solution; Be down to constant temperature until the temperature of saturated solution and stir after water-bath kettle temperature, be placed in 30 DEG C of constant temperature and stir constant temperature stirring in water-bath, slowly add with Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution, stir 1.0h; β-CD is 8:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil;
II. take out and put to room temperature, subsequent cold storage spends the night; Sucking filtration, the petroleum ether of distilled water and 30～60 DEG C for the solid material making, 40 DEG C of thermostatic drying chamber inner dryings, grind and obtain and decompose Rhizoma Atractylodis Macrocephalae volatile oil-beta cyclodextrin clathrate afterwards.
The described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:10.
The described petroleum ether of 30～60 DEG C is purchased from Tianjin Kermel Chemical Reagent Co., Ltd..
embodiment 2
After decomposing, the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride, the steps include:
I. accurately take β-CD, heating water stirs it is dissolved, and makes β-CD saturated solution; Be down to constant temperature until the temperature of saturated solution and stir after water-bath kettle temperature, be placed in 40 DEG C of constant temperature and stir constant temperature stirring in water-bath, slowly add with Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution, stir 1.5h; β-CD is 10:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil;
II. take out and put to room temperature, subsequent cold storage spends the night; Sucking filtration, distilled water and absolute ethanol washing for the solid material making, 40 DEG C of thermostatic drying chamber inner dryings, grind and obtain the rear Rhizoma Atractylodis Macrocephalae volatile oil-beta cyclodextrin clathrate of decomposition.
The described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:5.
embodiment 3
After decomposing, the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride, the steps include:
I. accurately take β-CD, heating water stirs it is dissolved, and makes β-CD saturated solution; Be down to constant temperature until the temperature of saturated solution and stir after water-bath kettle temperature, be placed in 50 DEG C of constant temperature and stir constant temperature stirring in water-bath, slowly add with Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution, stir 2.0h; β-CD is 4:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil;
II. take out and put to room temperature, subsequent cold storage spends the night; Sucking filtration, distilled water and ether washing for the solid material making, 40 DEG C of thermostatic drying chamber inner dryings, grind and obtain the rear Rhizoma Atractylodis Macrocephalae volatile oil-beta cyclodextrin clathrate of decomposition.
The described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:8.
embodiment 4
After decomposing, the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride, the steps include:
I. accurately take β-CD, heating water stirs it is dissolved, and makes β-CD saturated solution; Be down to constant temperature until the temperature of saturated solution and stir after water-bath kettle temperature, be placed in 60 DEG C of constant temperature and stir constant temperature stirring in water-bath, slowly add with Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution, stir 0.5h; β-CD is 6:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil;
II. take out and put to room temperature, subsequent cold storage spends the night; Sucking filtration, distilled water and ethyl acetate washing for the solid material making, 40 DEG C of thermostatic drying chamber inner dryings, grind and obtain the rear Rhizoma Atractylodis Macrocephalae volatile oil-beta cyclodextrin clathrate of decomposition.
The described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:9.
Claims (10)
1. after decomposing, the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride, is characterized in that, the steps include:
I. accurately take β-CD, heating water stirs it is dissolved, and makes β-CD saturated solution; Be down to constant temperature until the temperature of saturated solution and stir after water-bath kettle temperature, be placed in 30～60 DEG C of constant temperature and stir constant temperature stirring in water-bath, slowly add with Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution, more than stirring 0.5h; β-CD is 4～10:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil;
II. take out and put to room temperature, subsequent cold storage spends the night; Sucking filtration, distilled water and organic solvent washing for the solid material making, 40 DEG C of thermostatic drying chamber inner dryings, grind and obtain the rear Rhizoma Atractylodis Macrocephalae volatile oil-beta cyclodextrin clathrate of decomposition.
2. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 1, is characterized in that, described β-CD is 6:1 with the mass ratio that decomposes rear Rhizoma Atractylodis Macrocephalae volatile oil.
3. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 1 and 2, is characterized in that, it is 60 DEG C that constant temperature stirs water-bath kettle temperature.
4. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 1 and 2, it is characterized in that, the described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:8～10.
5. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 3, it is characterized in that, the described mass volume ratio with Rhizoma Atractylodis Macrocephalae volatile oil after decomposing in Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution and dehydrated alcohol is 1:8～10.
6. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 1 and 2, is characterized in that, add with mixing time after Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution be 1.5h.
7. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 3, is characterized in that, add with mixing time after Rhizoma Atractylodis Macrocephalae volatile oil after the decomposition of anhydrous alcohol solution be 1.5h.
8. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 1 and 2, it is characterized in that, it is any one in the petroleum ether, dehydrated alcohol, ether, ethyl acetate of 30～60 DEG C that the organic solvent in step II is selected from boiling range.
9. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 3, is characterized in that, it is any one in the petroleum ether, dehydrated alcohol, ether, ethyl acetate of 30～60 DEG C that the organic solvent in step II is selected from boiling range.
10. the preparation method of Rhizoma Atractylodis Macrocephalae volatile oil/Benexate Hydrochloride after decomposition according to claim 4, it is characterized in that, it is any one in the petroleum ether, dehydrated alcohol, ether, ethyl acetate of 30～60 DEG C that the organic solvent in step II is selected from boiling range.
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