CN101342233B - Peppermint prescription particle preparation method - Google Patents
Peppermint prescription particle preparation method Download PDFInfo
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- CN101342233B CN101342233B CN 200710118747 CN200710118747A CN101342233B CN 101342233 B CN101342233 B CN 101342233B CN 200710118747 CN200710118747 CN 200710118747 CN 200710118747 A CN200710118747 A CN 200710118747A CN 101342233 B CN101342233 B CN 101342233B
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Abstract
The invention discloses a herbal menthae ingredient particle and a preparation method and a quality control method thereof. The ingredient particle uses the herbal menthae as raw materials. The herbal menthae is processed by quantitative extraction and quantitative volatile oil is added. The herbal methae and the volatile oils are processed by water extraction, inclusion and spray drying, and thelike, to obtain spray drying herbal menthae powder. The herbal menthae ingredient particle is prepared by the spray drying herbal menthae powder directly or by the spraying drying herbal menthae powder and the auxiliary materials with proper amount. Every gram of the herva menthae ingredient particle of the invention is provided with an IR fingerprint spectra indicated as a Fig3. The preparation method of the invention adopts the quantitative equivalent extracting addition method of the volatile oil so as to ensure drug effect and reduce toxicity and side effects. The technology of the IR fingerprint spectra is adopted by the invention for quality control and the quality control method is scientific, advanced, quick and highly feasible.
Description
Technical field
The present invention relates to a kind of Chinese medicinal granule and preparation method thereof and method of quality control, particularly a kind of peppermint prescription particle and preparation method thereof and method of quality control.
Background technology
Chinese medicinal granule is under Chinese medical theory instructs, and the prepared slices of Chinese crude drugs are formed through various processes, is used for the granule that clinical tcm prescription allotment is used; Compare with traditional Chinese herbs decoction, its taking convenience, dose is little, and is quality controllable, preserves easily, is easy to carry; Chinese medicinal granule is in the pilot production status at home at present, product technology and quality standard disunity.Peppermint prescription particle is a kind of of conventional Chinese medicine granule, peppermint prescription particle mostly is the traditional water extraction at present, perhaps extract water extraction behind the volatile oil, and different production units are because production equipment is different with production technology, there are very big-difference in volatile oil extraction ratio and utilization rate, and extraction process by water also exists difference.Present volatile oil extraction process is owed science, perhaps is difficult to obtain its main effective ingredient volatile oil, reduces drug effect greatly; The oil mass of perhaps volatilizing is excessive, causes the property of medicine too quickly, untoward reaction occurs.Its quality standard is generally the Mentholum thin-layer qualitative and differentiates and volatile oil content testing, the specificity of this standard is limit by certain test conditions and scope, lack other due quality informations of product, this standard can't be judged the quality good or not and the overall picture of peppermint prescription particle product comprehensively.
Infrared spectrometry is one of conventional means of differentiating chemical compound and definite structure of matter.In pharmaceutical analysis, " fingerprint " characteristic that has with infrared spectrum is the common method that adopts of various countries' pharmacopeia as the foundation of drug identification.But since Chinese crude drug, the prepared slices of Chinese crude drugs and Chinese patent medicine itself all be more than the Western medicine complexity many mixture systems, the spectrum analysis difficulty makes conventional infrared spectrometry fail its due effect of performance in Chinese medicine quality control and management in the long term.
Summary of the invention
The objective of the invention is to disclose a kind of peppermint prescription particle; The present invention also aims to disclose the preparation method of this granule; The present invention also aims to disclose the method for quality control of this granule.
The present invention seeks to be achieved through the following technical solutions.
The every gram of peppermint prescription particle of the present invention contains suitable crude drug amount 10 grams; Volatile oil contents is between 0.48%-0.96% in the granule; Measure its Infrared fingerprint spectra with Fourier transform infrared spectrometer; Highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, according to the peak 1047cm appears from high to low by force simultaneously
-1, 1149cm
-1, 767cm
-1And 817cm
-14 peaks; Strong peak: peak position 1418cm
-1Except that above-mentioned feature, must have 2932cm simultaneously
-1, 1269cm
-12 peaks.
The Infrared fingerprint spectra condition determination: instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
The preparation method of peppermint prescription particle of the present invention is:
The raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Herba Menthae HerbaMenthae standard Infrared fingerprint spectra has following feature: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get above-mentioned Herba Menthae medical material 1 weight portion, extract Herba Menthae Haplocalycis volatile oil, the amount that gets volatile oil is 0.06%-0.12% of a Herba Menthae inventory; To extract Herba Menthae behind the volatile oil with 5-10 parts by volume water reflux, extract, 0.5-2 hour, being evaporated to relative density is 1.1-1.2, the Herba Menthae water extracting liquid; Behind β-cyclodextrin that Herba Menthae Haplocalycis volatile oil and himself 4-10 are doubly measured, the 20-50 purified water mix homogeneously doubly, be that 5-15 microns colloid mill ground 10-30 minute, carry out inclusion essential oil, Benexate Hydrochloride that must Herba Menthae Haplocalycis volatile oil with the slit slit; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The Herba Menthae spray drying powder is directly granulated or add the dextrin or the lactose of himself weight 0%-25% in the Herba Menthae spray drying powder; Dry granulation gets 20-60 purpose peppermint prescription particle.
Above-mentioned preparation method is preferably: get Herba Menthae 1 weight portion, extract Herba Menthae Haplocalycis volatile oil with straight-through steaming process, the amount that gets volatile oil is 0.06%-0.12% of a Herba Menthae inventory; To extract Herba Menthae behind the volatile oil with 6-8 parts by volume water reflux, extract, 1-2 hour, being evaporated to relative density is 1.1-1.2, the Herba Menthae water extracting liquid; Behind β-cyclodextrin that Herba Menthae Haplocalycis volatile oil and himself 6-8 are doubly measured, the 30-40 purified water mix homogeneously doubly, be that 5-10 microns colloid mill ground 15-20 minute, carry out inclusion essential oil, Benexate Hydrochloride that must Herba Menthae Haplocalycis volatile oil with the slit slit; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The Herba Menthae spray drying powder is directly granulated or add the dextrin or the lactose of himself weight 0%-25% in the Herba Menthae spray drying powder; Dry granulation gets 20-40 purpose peppermint prescription particle.
Above-mentioned preparation method is preferably: get Herba Menthae 1 weight portion, extract Herba Menthae Haplocalycis volatile oil with straight-through steaming process, the amount that gets volatile oil is 0.06%-0.12% of a Herba Menthae inventory; To extract Herba Menthae behind the volatile oil with 8 times of parts by volume water reflux, extract, 1.5 hours, being evaporated to relative density is 1.1-1.2, the Herba Menthae water extracting liquid; Behind the β-cyclodextrin of Herba Menthae Haplocalycis volatile oil and himself 8 times of amount, 40 times purified water mix homogeneously, be that 5 microns colloid mill ground 20 minutes with the slit slit, carry out inclusion essential oil, the Benexate Hydrochloride of Herba Menthae Haplocalycis volatile oil; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The Herba Menthae spray drying powder is directly granulated or add adjuvant dextrin or the lactose of himself weight 0-25% in the Herba Menthae spray drying powder; Dry granulation gets 20-60 purpose peppermint prescription particle.
The method of quality control of peppermint prescription particle of the present invention comprises one or more in the following method:
A. the method for quality control of Herba Menthae spray drying powder: the Herba Menthae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Herba Menthae spray drying powder standard Infrared fingerprint spectra is: highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, 1047cm appears in intensity according to the peak from high to low simultaneously simultaneously
-1, 1031cm
-1, 1149cm
-1, 767cm
-1And 816cm
-15 peaks; Strong peak: peak position 1419cm-1; Except that above-mentioned peak, must have 2932cm simultaneously
-1, 1267cm
-12 peaks.
B. the method for quality control of peppermint prescription particle: peppermint prescription particle adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; Peppermint prescription particle standard Infrared fingerprint spectra is: highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, according to the peak 1047cm appears from high to low by force simultaneously
-1, 1149cm
-1, 767cm
-1And 817cm
-14 peaks; Strong peak: peak position 1418cm
-1Except that above-mentioned peak, must have 2932cm simultaneously
-1, 1269cm
-12 peaks.
The relation of weight portion/parts by volume of the present invention is: grams per milliliter.
Description of drawings
Fig. 1: Herba Menthae Herba Menthae standard Infrared fingerprint spectra
Fig. 2: Herba Menthae spray drying powder standard Infrared fingerprint spectra
Fig. 3: peppermint prescription particle standard Infrared fingerprint spectra
Fig. 4: contain the classical medicine of Herba Menthae decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram are compared
Fig. 5: peppermint prescription particle and Herba Menthae medical material thin layer chromatography are relatively
Fig. 6: peppermint prescription particle and Herba Menthae medical material thin-layer sample Infrared fingerprint spectra are relatively
Granule of the present invention has complete, advanced production technology and strong, the controlled quality control standard of specificity, and technology advanced person can realize, the detection method science that quality standard relates to, advanced person, quick, workable. The present invention is applied to the quality control of Chinese medicine with infrared spectrum technology, and this is the innovation on a kind of thinking. This not only meets traditional chinese medicine about the theory of " monarch, minister, help, make ", also given prominence to the group effect of Chinese medicine, simultaneously the problem of complexity is oversimplified, do certain Chinese medicine as a whole, observe its " fingerprint ", thereby solved rapidly a matter of utmost importance---the evaluation of the Chinese medicine true and false in the control of Chinese medicine macroscopic quality.
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
The decoction utilization rate of experimental example 1 Herba Menthae Haplocalycis volatile oil is investigated:
1, peppermint actual utilization of volatile oil in traditional decoction is investigated
In traditional decocting for Chinese herbal medicine method, the medicine take volatile oil as main pharmacodynamics, the decocting method under general employing is rear. The actual process of boiling medicine of this experimental design simulation traditional decocting medicine, according to a prescription 6-15 flavor medicine, every flavor medicine 9-15 gram calculates, every pair of medicine is greatly between 70 grams restrain to 180, and boiling medicine, routine one fries in shallow oil amount of water generally between the 800-1200 milliliter in the process, be amount of water be drug dose 6-15 doubly between, two fry in shallow oil amount of water fries in shallow oil slightly than one and lacks. Time under rear is that other drug was fried in shallow oil front 0-20 minute. The main utilization rate scope by Herba Menthae Haplocalycis volatile oil in the orthogonal experiment investigation decoction of this test, and repeat orthogonal experiment analysis gained optimum and test and the poorest experiment each three times, volatile oil utilization rate bound tried to achieve. According to above-mentioned orthogonal experiment arrangement, boil medicine, measure the amount of volatile oil in the soup with the method on the pharmacopeia appendix, and the decoction utilization rate of definite Herba Menthae Haplocalycis volatile oil, take the utilization rate of volatile oil as performance analysis, for peppermint prescription particle is determined reasonable, safe volatile oil addition, the result proves, one fries in shallow oil: the time is that 20 minutes, amount of water are 14 times, and two fry in shallow oil: the time is that 10 minutes, amount of water are 8 times, and the Herba Menthae Haplocalycis volatile oil utilization rate is the highest with this understanding; One fries in shallow oil: the time is that 30 minutes, amount of water are 6 times, and two fry in shallow oil: the time is that 20 minutes, amount of water are 4 times, and the Herba Menthae Haplocalycis volatile oil utilization rate is minimum with this understanding; Repeated experiments result shows: optimum experiment reproducible results is followed successively by 11.85%, 12.02%, 12.16%, the decoction utilization rate that is Herba Menthae Haplocalycis volatile oil is the highest about 12%, the poorest experiment reproducible results is followed successively by 6.05%, 6.13%, 5.91%, and namely the decoction utilization rate of Herba Menthae Haplocalycis volatile oil is minimum about 6%.
2, volatile oil beta-cyclodextrin inclusion compound orthogonal experiment
Take the ratio of volatile oil and beta-schardinger dextrin-, water and milling time as factor, 3 levels of each factor, the design orthogonal experiment take the inclusion rate of volatile oil as investigating index, is estimated the beta-cyclodextrin inclusion compound degree of volatile oil.
Orthogonal experiment results shows that the amount of beta-schardinger dextrin-is for affecting the topmost factor of inclusion essential oil, consider to reduce as much as possible in the product adding of auxiliary material, carry out 2 groups of repeated tests, the use amount of beta-schardinger dextrin-when determining whether suitably to reduce inclusion.
The result shows that after β-cyclodextrin that Herba Menthae Haplocalycis volatile oil and himself 6-8 doubly measure, 30-40 purified water doubly mixed, the inclusion essential oil effect was better, and inclusion rate is not less than 80%.
The Herba Menthae Haplocalycis volatile oil utilization of experimental example 2 crude drugs and granule of the present invention relatively
According to " the regulation peppermint medicinal material of Chinese pharmacopoeia contains volatile oil must not be less than 0.80% (ml/g), according to above-mentioned experimental example 1, the utilization rate of Herba Menthae Haplocalycis volatile oil is between 6%-12% in the tradition decoction, be per 100 gram peppermint medicinal materials, the utilization of volatile oil is 0.048ml-0.096ml in decoction.
Per 1 gram of peppermint prescription particle of the present invention is equivalent to peppermint medicinal material 10 grams, and the content of volatile oil is 0.48%-0.96% in the peppermint prescription particle, and namely per 10 gram peppermint prescription particles (being equivalent to crude drug 100 grams) contain volatile oil 0.048ml-0.096ml. Can find out from above-mentioned data: the peppermint raw material of peppermint prescription particle and equivalent is consistent at the utilization of volatile oil, this for peppermint prescription particle safely and effectively material base prove.
Experimental example 3
(1) peppermint prescription particle and the comparative studies of peppermint medicinal material thin-layer chromatography
Differentiate that according to middle Herba Menthae medical material of Pharmacopoeia of the People's Republic of China version in 2005 the thin layer chromatography test method prepares Herba Menthae medical material sample and peppermint prescription particle sample of the present invention under the item, measure, the gained result as shown in Figure 5, in the peppermint prescription particle chromatograph, with the corresponding position of Herba Menthae medical material chromatograph on, show the speckle of same color.
(2) peppermint prescription particle and Herba Menthae medical material thin-layer sample Infrared fingerprint spectra are relatively
Measure the Herba Menthae medical material of preparation in (1) and the thin-layer sample of peppermint prescription particle with Fourier transform infrared spectrometer, its result as shown in Figure 6, the thin-layer sample Infrared fingerprint spectra peak shape of peppermint prescription particle and Herba Menthae medical material, peak position, peak intensity basically identical, dependency reaches 96.5%.
To sum up (1), (2) result prove that peppermint prescription particle of the present invention is consistent with the Herba Menthae medicinal ingredient, and technology of the present invention is rational.
Experimental example 4 contains the classical medicine of Herba Menthae to decoction pieces decocting liquid and the comparative study of granular recipe " whole part " infrared spectrogram
Herba Menthae-Periostracum Cicadae 5 usefulness come from Jing-Yue Complete Works two flavor XIAOFENG SAN, the light clear fragrance of Herba Menthae, and Xin Liang is capable to loose, the diffusing wind heat of inducing sweat, the clear sharp head, rash is antipruritic; The Periostracum Cicadae sweet in the mouth is cold in nature, and the energy wind and heat dispersing is sent out urticaria thoroughly, and light clear liter is diffusing, is apt to away myocutaneous junction, site where the skin and muscle are joined.Multiplication is then renderd a service in two medicine mutual reinforcements between pairing, receives the wind heat of loosing altogether, throat, and the refresh oneself, row flesh table, the letting out skin rashes completely rash is gone the antipruritic effect of wind; General Herba Menthae 3g-9g, Periostracum Cicadae 3g-9g compatibility uses, for the classical Chinese medicine medicine to one of.This experimental example purpose is studied the similarities and differences of the two decoction pieces decocting liquid and granular recipe, determines peppermint prescription particle technology and normal reasonability.
Experimental technique: get Herba Menthae decoction pieces, each 10g prescription of Periostracum Cicadae decoction pieces, decoct preparation decoction pieces decocting liquid sample down after pressing the decocting method Herba Menthae of decoction pieces decoction; Other gets Periostracum Cicadae decoction pieces 10g, and the decocting method of pressing the decoction pieces decoction decocts, and medicinal liquid suitably concentrates, and adds peppermint prescription particle 1g of the present invention, is stirred to dissolving fully, system granular recipe sample; Drinking sheet decocting liquid sample, granular recipe sample respectively carries out infrared spectrum and detects.
Testing conditions: detecting instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
Testing result: decoction pieces decocting liquid sample and granular recipe sample Infrared fingerprint spectra peak shape, peak position, peak intensity basically identical as shown in Figure 4, dependency reaches 97.8%.It is consistent to prove that soup that granule is joined and decoction pieces close the decocting liquid composition, and promptly 1g peppermint prescription particle of the present invention is consistent with a 10g Herba Menthae decoction pieces fried composition, and equivalent and production technology that peppermint prescription particle 1g of the present invention is equivalent to Herba Menthae decoction pieces 10g are rational.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: peppermint prescription particle of the present invention
The raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Gained result and Herba Menthae standard Infrared fingerprint spectra similarity are 96%; Specifically being characterized as of Herba Menthae standard Infrared fingerprint spectra: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get Herba Menthae 1000kg, extract Herba Menthae Haplocalycis volatile oil, get volatile oil 0.86L with the direct-flow steam method; To extract Herba Menthae behind the volatile oil with 6000L water reflux, extract, 2.5 hours, being evaporated to relative density is 1.15, the Herba Menthae water extracting liquid; Behind Herba Menthae Haplocalycis volatile oil and 6.8kg β-cyclodextrin, 36L purified water mix homogeneously, be that 5 microns colloid mill ground 20 minutes with the slit slit, carry out inclusion essential oil, the Benexate Hydrochloride of Herba Menthae Haplocalycis volatile oil; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The adjuvant dextrin that adds himself weight 20% in the Herba Menthae spray drying powder; Directly dry granulation gets 20-60 purpose peppermint prescription particle.
Embodiment 2: peppermint prescription particle of the present invention
The raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Gained result and Herba Menthae standard Infrared fingerprint spectra similarity are 99%: specifically being characterized as of Herba Menthae standard Infrared fingerprint spectra: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get Herba Menthae 1000kg, extract Herba Menthae Haplocalycis volatile oil, get volatile oil 0.8L with the direct-flow steam method; To extract Herba Menthae behind the volatile oil with 8000L water reflux, extract, 1.5 hours, being evaporated to relative density is 1.2, the Herba Menthae water extracting liquid; Behind Herba Menthae Haplocalycis volatile oil and 5kg β-cyclodextrin, 24L purified water mix homogeneously, be that 8 microns colloid mill ground 18 minutes with the slit slit, carry out inclusion essential oil, the Benexate Hydrochloride of Herba Menthae Haplocalycis volatile oil; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and medicinal liquid is 50 ℃ of preheatings, 170 ℃ of inlet temperature, 600 rev/mins of material revolution speeds, 75 ℃ of leaving air temps, wind send spray drying under the condition of 50 ℃ of temperature, obtain the Herba Menthae spray drying powder; 15% of adding spray drying powder own wt adjuvant dextrin in the Herba Menthae spray drying powder; At main pinch roller pressure is 6MPa, and side pressure wheel pressure is 0.4MPa, and the speed of mainshaft is 450 rev/mins, and feed voltage is a dry granulation under the condition of 100V, 20-60 purpose peppermint prescription particle.
Embodiment 3: peppermint prescription particle of the present invention
The raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The gained result is consistent with Herba Menthae standard Infrared fingerprint spectra; The standard Infrared fingerprint spectra specifically is characterized as: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get Herba Menthae 1000kg, extract Herba Menthae Haplocalycis volatile oil, get volatile oil 0.75L with the direct-flow steam method; To extract Herba Menthae behind the volatile oil with 5000L water reflux, extract, 2 hours, being evaporated to relative density is 1.1, the Herba Menthae water extracting liquid; Behind Herba Menthae Haplocalycis volatile oil and 6kg β-cyclodextrin, 30L purified water mix homogeneously, be that 5 microns colloid mill ground 25 minutes with the slit slit, carry out inclusion essential oil, the Benexate Hydrochloride of Herba Menthae Haplocalycis volatile oil; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and medicinal liquid is 40 ℃ of preheatings, 180 ℃ of inlet temperature, 500 rev/mins of material revolution speeds, 85 ℃ of leaving air temps, wind send spray drying under the condition of 45 ℃ of temperature, obtain the Herba Menthae spray drying powder; 25% of adding spray drying powder own wt adjuvant lactose in the Herba Menthae spray drying powder; At main pinch roller pressure is 4.5MPa, and side pressure wheel pressure is 0.6MPa, and the speed of mainshaft is 350 rev/mins, and feed voltage is a dry granulation under the condition of 150V, 20-60 purpose peppermint prescription particle.
Embodiment 4: the method for quality control of the peppermint prescription particle of the present invention of embodiment 1 preparation
The method of quality control of Herba Menthae spray drying powder: the Herba Menthae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The standard Infrared fingerprint spectra similarity of gained result and Herba Menthae spray drying powder is 98%; The standard Infrared fingerprint spectra of Herba Menthae spray drying powder is characterized as:
Highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, 1047cm appears in intensity according to the peak from high to low simultaneously simultaneously
-1, 1031cm
-1, 1149cm
-1, 767cm
-1And 816cm
-15 peaks; Strong peak: peak position 1419cm
-1Except that above-mentioned peak, must have 2932cm simultaneously
-1, 1267cm
-12 peaks.
Embodiment 5: the method for quality control of the peppermint prescription particle of the present invention of embodiment 2 preparations
The method of quality control of peppermint prescription particle: peppermint prescription particle adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; The standard Infrared fingerprint spectra similarity of gained result and peppermint prescription particle is 99%; The standard Infrared fingerprint spectra of peppermint prescription particle is characterized as:
Highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, according to the peak 1047cm appears from high to low by force simultaneously
-1, 1149cm
-1, 767cm
-1And 817cm
-14 peaks; Strong peak: peak position 1418cm
-1Except that above-mentioned peak, must have 2932cm simultaneously
-1, 1269cm
-12 peaks.
Embodiment 6: the method for quality control of the peppermint prescription particle of the present invention of embodiment 3 preparations
A. the method for quality control of Herba Menthae spray drying powder: the Herba Menthae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The gained result is consistent with the standard Infrared fingerprint spectra of Herba Menthae spray drying powder; The standard Infrared fingerprint spectra of Herba Menthae spray drying powder is characterized as:
Highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, 1047cm appears in intensity according to the peak from high to low simultaneously simultaneously
-1, 1031cm
-1, 1149cm
-1, 767cm
-1And 816cm
-15 peaks; Strong peak: peak position 1419cm-1; Except that above-mentioned peak, must have 2932cm simultaneously
-1, 1267cm
-12 peaks.
B. the method for quality control of peppermint prescription particle: peppermint prescription particle adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; The gained result is consistent with the standard Infrared fingerprint spectra of peppermint prescription particle; The standard Infrared fingerprint spectra of peppermint prescription particle is characterized as:
Highest peak: peak position 1606cm
-1Inferior strong peak: peak position 1078cm
-1, according to the peak 1047cm appears from high to low by force simultaneously
-1, 1149cm
-1, 767cm
-1And 817cm
-14 peaks; Strong peak: peak position 1418cm
-1Except that above-mentioned peak, must have 2932cm simultaneously
-1, 1269cm
-12 peaks.
Claims (3)
1. the preparation method of a peppermint prescription particle is characterized in that this method is:
The raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Herba Menthae HerbaMenthae standard Infrared fingerprint spectra has following feature: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get above-mentioned Herba Menthae medical material 1 weight portion, extract Herba Menthae Haplocalycis volatile oil, the amount that gets volatile oil is the 0.06%-0.12% of Herba Menthae inventory; To extract Herba Menthae behind the volatile oil with 5-10 parts by volume water reflux, extract, 0.5-2 hour, being evaporated to relative density is 1.1-1.2, the Herba Menthae water extracting liquid; Behind the beta-schardinger dextrin-that Herba Menthae Haplocalycis volatile oil and himself 4-10 are doubly measured, the 20-50 purified water mix homogeneously doubly, be that the colloid mill of 5-15 micron ground 10-30 minute, carry out inclusion essential oil, Benexate Hydrochloride that must Herba Menthae Haplocalycis volatile oil with the slit slit; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The Herba Menthae spray drying powder is directly granulated or add dextrin or the lactose of himself weight 0%-25% in the Herba Menthae spray drying powder; Dry granulation gets 20-60 purpose peppermint prescription particle.
2. the preparation method of peppermint prescription particle as claimed in claim 1 is characterized in that this method is:
The raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Herba Menthae HerbaMenthae standard Infrared fingerprint spectra has following feature: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get Herba Menthae 1 weight portion, extract Herba Menthae Haplocalycis volatile oil with straight-through steaming process, the amount that gets volatile oil is the 0.06%-0.12% of Herba Menthae inventory; To extract Herba Menthae behind the volatile oil with 6-8 parts by volume water reflux, extract, 1-2 hour, being evaporated to relative density is 1.1-1.2, the Herba Menthae water extracting liquid; Behind the beta-schardinger dextrin-that Herba Menthae Haplocalycis volatile oil and himself 6-8 are doubly measured, the 30-40 purified water mix homogeneously doubly, be that the colloid mill of 5-10 micron ground 15-20 minute, carry out inclusion essential oil, Benexate Hydrochloride that must Herba Menthae Haplocalycis volatile oil with the slit slit; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The Herba Menthae spray drying powder is directly granulated or add dextrin or the lactose of himself weight 0%-25% in the Herba Menthae spray drying powder; Dry granulation gets 20-60 purpose peppermint prescription particle.
3. the preparation method of peppermint prescription particle as claimed in claim 1, it is characterized in that this method is: the raw material Herba Menthae adopts Infrared fingerprint spectra to carry out quality discrimination, the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Herba Menthae HerbaMenthae standard Infrared fingerprint spectra has following feature: highest peak: peak position 1648cm
-1Inferior strong peak: peak position 1070cm
-1Strong peak: peak position 2926cm
-1Intensity according to the peak must have 1416cm from height successively to low simultaneously
-1, 1260cm
-1, 1320cm
-1, 621cm
-1, 771cm
-15 peaks;
Get Herba Menthae 1 weight portion, extract Herba Menthae Haplocalycis volatile oil with straight-through steaming process, the amount that gets volatile oil is the 0.06%-0.12% of Herba Menthae inventory; To extract Herba Menthae behind the volatile oil with 8 times of parts by volume water reflux, extract, 1.5 hours, being evaporated to relative density is 1.1-1.2, the Herba Menthae water extracting liquid; Behind the beta-schardinger dextrin-of Herba Menthae Haplocalycis volatile oil and himself 8 times of amount, 40 times purified water mix homogeneously, be that 5 microns colloid mill ground 20 minutes with the slit slit, carry out inclusion essential oil, the Benexate Hydrochloride of Herba Menthae Haplocalycis volatile oil; The Benexate Hydrochloride of getting Herba Menthae Haplocalycis volatile oil mixes with the Herba Menthae water extracting liquid, and spray drying obtains the Herba Menthae spray drying powder; The Herba Menthae spray drying powder is directly granulated or add adjuvant dextrin or the lactose of himself weight 0-25% in the Herba Menthae spray drying powder; Dry granulation gets 20-60 purpose peppermint prescription particle.
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|---|---|---|---|
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|---|---|---|---|
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| CN106546552A (en) * | 2016-11-24 | 2017-03-29 | 北京康仁堂药业有限公司 | A kind of detection method and device of Chinese medicinal granule specificity |
| CN107748218B (en) * | 2017-10-25 | 2019-10-15 | 安徽出入境检验检疫局检验检疫技术中心 | A kind of fingerprint atlas detection method of Peppermint essential oil |
| CN109528823A (en) * | 2019-01-02 | 2019-03-29 | 江西百神药业股份有限公司 | A kind of preparation process of peppermint spray powder |
| CN109646408A (en) * | 2019-01-02 | 2019-04-19 | 江西百神药业股份有限公司 | A kind of peppermint prescription particle and preparation method thereof |
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Non-Patent Citations (1)
| Title |
|---|
| 张彤.薄荷配方颗粒中薄荷脑和咖啡酸的含量测定研究.《中国药学杂志》.2007,第42卷(第4期),301-304. * |
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