CN104138420B - A kind of processing method of Herba Cistanches medical material - Google Patents

A kind of processing method of Herba Cistanches medical material Download PDF

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CN104138420B
CN104138420B CN201310167453.9A CN201310167453A CN104138420B CN 104138420 B CN104138420 B CN 104138420B CN 201310167453 A CN201310167453 A CN 201310167453A CN 104138420 B CN104138420 B CN 104138420B
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processing method
sheet
herba cistanches
medical material
cistanche
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CN104138420A (en
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姜勇
屠鹏飞
邹萍萍
鲍忠
田闯
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Peking University
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Abstract

The present invention provides the processing method of a kind of Herba Cistanches medical material, including: 1) fresh herba cistanches medical material is removed impurity, get silt express developed with water, cut into sheet;2) the described sheet that step 1 obtains, high temperature kill enzymes processes 1 15min;3) the described sheet after heat treatment, lyophilization.The desertliving cistanche sheet color and luster that processing method of the present invention obtains is pale, attractive in appearance, and quality is dried, and the content of principle active component echinacoside and verbascoside is more than 10 times of natural drying method.

Description

A kind of processing method of Herba Cistanches medical material
Technical field
The processing method that the invention belongs to tcm and herbal slice, improves decoction pieces outward appearance product particularly to one Effective ingredient echinacoside and the Herba Cistanches of verbascoside content in matter, raising Herba Cistanches medical material The processing method of medical material.
Background technology
Herba Cistanches is famous traditional tonic medicine, have the laudatory title of " desert Radix Ginseng ", have kidney-replenishing, The effect such as benefiting essence-blood, loosening bowel to relieve constipation, be usually used in treat impotence in male, infertilitas feminis, chills and pain of the waist and kness, The diseases such as blood depletion constipation.Herba Cistanches is parasitic plant, and main parasitic is at the plant sacsaoul checked winds and fixed drifting sand With the root of red building, it is distributed in the desert regions such as Xinjiang, Inner Mongol, Ningxia.Echinacoside And verbascoside (acteoside) is its principle active component (echinacoside)." middle traditional Chinese medicines Allusion quotation " to record its base plant be Herba Cistanches (Cistanche deserticola) and pipe to 2010 years versions one Flower herba cistanches (Cistanche tubulosa), medicinal part is the fleshy stem of dry zone scale leaf.Tradition Habitat processing method is: excavates when Seedling is not unearthed or is just unearthed spring, removes inflorescence, cutting, shine Dry.Tradition decoction pieces processing method is that Herba Cistanches medical material is cut into sheet, natural drying.But due to Herba Cistanches Fleshy stem volume is relatively big, and water content is higher, and dry run often needs time several months, easily goes mouldy.And Research finds, Herba Cistanches plant is contained within substantial amounts of hydrolytic enzyme, at Herba Cistanches medical material and decoction pieces thereof Dry run often make its effective ingredient phenylethanoid glycoside hydrolyze so that it is content is significantly Reduce, thus reduce the curative effect of Herba Cistanches.Therefore, prior art occurring in that, enzyme is killed in heating, with Improve the Herba Cistanches processing method of phenylethanol composition in Herba Cistanches, as publication number CN1709292A(is public Open 2005 days December 21) Chinese patent application disclosed in the processing method of Herba Cistanches Herba Cistanches cuts sheet, and hot water kills enzyme, then dries or dries.Although strobile can be made by this method The content of echinacoside improves more than 5 times, but the desertliving cistanche sheet color and luster blackout that the method processes, It is difficult to enter high-end decoction pieces market.
Summary of the invention
It is an object of the invention to provide effective ingredient echinacoside in a kind of raising Herba Cistanches medical material With verbascoside content, the processing method improving the Herba Cistanches medical material of decoction pieces exterior quality simultaneously.Through this The desertliving cistanche sheet color and luster inventing the processing of described method is pale, attractive in appearance, and quality is dried, crisp, and it is main The content of effective ingredient echinacoside and verbascoside is more than 10 times of tradition decoction pieces processing method, It is that the hot water that publication number CN1709292A records kills enzyme, dries or more than 2 times of furnace drying method.Therefore, The processing method of Herba Cistanches medical material of the present invention, substantially increases the product of Herba Cistanches medical material and decoction pieces thereof Matter, simultaneously because of the increase of active constituent content, improves service efficiency and the clinical efficacy of Herba Cistanches, subtracts Lack the use of medicinal raw material, and indirectly protect environment.
For achieving the above object, technical scheme is as follows:
A kind of processing method of Herba Cistanches medical material, including:
1) fresh herba cistanches medical material is removed impurity, get silt express developed with water, cut into sheet;
2) the described sheet that step 1 obtains, high temperature kill enzymes processes 1-15min;
3) the described sheet after heat treatment, lyophilization.
The desertliving cistanche sheet color and luster that processing method of the present invention obtains is pale, and quality is dried, the most effectively The content of composition echinacoside and verbascoside is more than 10 times of tradition decoction pieces processing method.
Preferably, in step 3, described lyophilization, temperature is-50 DEG C ± 30 DEG C, pressure 2~20Pa, It is dried 12-48 hour;It is furthermore preferred that described lyophilization, temperature is-40 DEG C ± 10 DEG C, pressure 2~10Pa, It is dried 24-48 hour.
Preferably, in step 2, described in kill ferment treatment and include: hot water soaks described sheet 1-10min, Sheet 1-15min described in Steam by water bath or utilize pipeline steam to fumigate described sheet 1-15min.
In step 2, preferably kill ferment treatment temperature and be 70-100 DEG C;Killing ferment treatment temperature described in more preferably is 100℃.The described enzyme processing time that kills is preferably 2-5min.
Preferably, the thickness of described sheet is 0.1-1.5cm;More preferably 0.5-1.0cm.
Herba Cistanches medical material of the present invention includes Herba Cistanches (Cistanche deserticolia), pipe fat and red meat desert Rong (C.tubulosa), Saline Cistanche Herb (C.salsa (C.A.Mey.) G.Beck), Herba Cistanches sinensis (C. Sinensis G.Beck) and other pharmaceutically acceptable plant of Cistanche deserticola.
Further object is that a kind of desertliving cistanche sheet of offer, fresh herba cistanches medical material utilizes this Processing method processing described in invention obtains, and described decoction pieces is surface light brown yellow, canescence or white, The visible fleshly scale leaf having, matter is crisp, and tangent plane has point-like vascular bundle, is arranged in wavy ring grain, feeble QI, taste Sweet, micro-hardship;The total content of echinacoside and verbascoside is more than 0.6%.
Improve active constituent content and the effect of decoction pieces quality to investigate processing method of the present invention, enter Go following experiment:
(1) content of effective ingredient in the desertliving cistanche sheet of Syrups by HPLC different processing methods is utilized
1. test sample:
1) processing method of the present invention (killing enzyme lyophilizing): take fresh herba cistanches fleshy stem, removes impurity, Cut into 0.5cm~0.8cm sheet, steam 3 minutes on boiling water, take out, lyophilization, to obtain final product, Decoction pieces is as shown in Figure 1 d.
2) method (killing enzyme to dry) that publication number CN1709292A records: take the fresh meat desert in the same place of production Rong's fleshy stem, cuts into 0.5cm~0.8cm sheet, boiling water boiling 3 minutes, takes out, 60 DEG C of drying, Obtaining, decoction pieces is as shown in Figure 1a.
3) direct lyophilization: take the fresh meat Herba Cistanches fleshy stem in the same place of production, cut into 0.5cm~0.8cm Sheet, direct lyophilizing, to obtain final product, decoction pieces is as illustrated in figure 1 c.
4) tradition decoction pieces processing method (natural drying): take the fresh meat Herba Cistanches fleshy stem in the same place of production, cut Making 0.8cm~1.4cm sheet, natural drying, to obtain final product, decoction pieces is as shown in Figure 1 b.
2. detection method:
Measure according to echinacoside in " Chinese Pharmacopoeia " (version one in 2010) and containing of verbascoside Determine method, use high-efficient liquid phase technique to be measured.
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler;With first Alcohol is mobile phase A, and with 0.1% formic acid solution as Mobile phase B, the regulation of according to the form below 1 carries out gradient elution; Detection wavelength is 330nm.Theoretical value is calculated by echinacoside peak should be not less than 3000.
Table 1 assay HPLC eluent gradient elution requirement
The preparation of reference substance solution: take echinacoside, verbascoside reference substance in right amount, accurately weighed, Add 50% methanol and make every 1ml mixed solution respectively containing 0.2mg, to obtain final product.
The preparation of need testing solution:
Take above-mentioned test sample powder (crossing No. 4 sieves) 1g respectively, accurately weighed, put 100ml brown In measuring bottle, precision adds 50% methanol 50ml, close plug, shakes up, weighed weight, soaks 30 minutes, Supersound process 40 minutes (power 250W, frequency 35kHz), lets cool, more weighed weight, adds 50% Methanol supplies the weight of less loss, shakes up, and stands, takes supernatant, filters, takes subsequent filtrate, to obtain final product.
3. measure and result:
Precision draws reference substance solution and each 10 μ l of need testing solution respectively, injects chromatograph of liquid, surveys Fixed, to obtain final product.
Measurement result: be shown in Table 2.
The assay result (mg/g) of table 2 different processing methods desertliving cistanche sheet effective ingredient
Processing method Echinacoside Verbascoside Decoction pieces outward appearance
Kill enzyme lyophilizing 0.91 0.82 Color is pale, and quality is dried, crisp
Kill enzyme to dry 0.44 0.32 Color is dark brown, and quality is viscous hard
Directly lyophilizing 0.10 0.05 Color is pale, and quality is dried, crisp
Natural drying 0.07 0.03 Color is dark brown, and quality is viscous hard
From table 2 it can be seen that the processing method of Herba Cistanches of the present invention, can significantly improve in decoction pieces and have The content of effect composition, and decoction pieces color and luster is pale, attractive in appearance, quality is crisp, have other processing methods without The advantage of method analogy.
(2) the HPLC finger printing of the desertliving cistanche sheet of different processing methods
1. test sample: with () described
2. detection method
Chromatographic condition and system suitability with octadecylsilane chemically bonded silica as filler, with 0.095% phosphoric acid acetonitrile-0.095% phosphoric acid is eluent gradient eluting (gradient is shown in Table 3), flow velocity 1.0mL/min, detects wavelength 330nm, column temperature 30 DEG C, and theoretical cam curve is pressed echinacoside peak and calculated, 3000 should be not less than.
Table 3 Herba Cistanches HPLC finger printing detection eluent gradient elution requirement
3. the preparation of reference substance solution: with () described
4. the preparation of need testing solution: with () described
5. measure and result:
Precision draws reference substance solution and each 10 μ l of need testing solution respectively, injects chromatograph of liquid.
The finger printing of different processing methods Herba Cistanches medical material is as shown in Figure 2.Fig. 2 b shows, tradition drink The sample of slice processing method, chromatographic peak significantly reduces, weakens, and illustrates that major part effective ingredient drops the most Solve change.After directly the collection of illustrative plates of the sample (Fig. 2 c) of lyophilizing amplifies with kill enzyme lyophilizing sample (Fig. 2 d) Compare with killing enzyme drying sample (Fig. 2 a), although the retention time at chromatographic peak quantity and each peak and the two base This is consistent, but the peak height of each chromatographic peak is significantly lower than killing enzyme lyophilizing and killing the sample that enzyme is dried.With other Three kinds of processing methods compare, and the peak height of each chromatographic peak of sample (Fig. 2 d) killing enzyme lyophilizing is the highest, and, The ratio of each chromatographic peak is also different from other method, illustrate the method can more efficiently retain each effectively Composition, it is to avoid its enzymolysis, for one efficient Herba Cistanches processing of crude drugs method.
The processing method of the present invention, compared with the processing method of prior art, has the advantage that
1, compared with the desertliving cistanche sheet of present invention processing directly shines drying method with tradition, effective ingredient echinacoside More than 10 times are improved with the content of verbascoside;Compared with direct freeze drying process, echinacoside and hair The content of stamen flower glucosides also improves more than 10 times;With publication number CN1709292A record hot water kill enzyme, Drying or furnace drying method is compared, the content of echinacoside and verbascoside improves more than 2 times;The method Substantially increase the content of effective ingredient in Herba Cistanches medical material, improve the utilization rate of medical material, reduce life Produce cost.
2, the medical material condition after the processing method processing of the present invention is good, and color and luster is pale, and quality is dried, and is suitable for The production of high-quality pharmaceutical decocting piece, improves the market value of decoction pieces.
3, the present invention and conventional drying process ratio, speed is fast, and general lyophilization only needs 2-3 days, and traditional Method needs tens of skies, greatly shortens the production cycle of decoction pieces, improves the productivity.
4, the medical material matter of present invention processing is crisp, it is easy to pulverize, and reduces during Chinese patent medicine produces the cost pulverized.
5, the low light weight of medical material water content of present invention processing, it is simple to transport and preserve.
Accompanying drawing explanation
Hereinafter, describe embodiment of the present invention in detail in conjunction with accompanying drawing, wherein:
Fig. 1 shows the photo of the desertliving cistanche sheet using different processing methods to prepare, wherein:
A: kill decoction pieces prepared by enzyme oven drying method;
Decoction pieces prepared by b: natural seasoning;
C: the decoction pieces that directly prepared by lyophilization;
D: kill decoction pieces prepared by enzyme lyophilization.
Fig. 2 shows the HPLC finger printing of the desertliving cistanche sheet using different processing methods to prepare, wherein:
Fig. 2 a: kill the finger printing of decoction pieces prepared by enzyme oven drying method;
The finger printing of decoction pieces prepared by Fig. 2 b: natural seasoning;
Fig. 2 c: the directly finger printing of decoction pieces prepared by lyophilization;
Fig. 2 d: kill the finger printing of decoction pieces prepared by enzyme lyophilization.
Detailed description of the invention
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these Embodiment is merely to illustrate the present invention, and it limits the scope of the present invention never in any form.
Experimental technique in following embodiment, if no special instructions, is conventional method.
Embodiment 1
Take fresh herba cistanches (Cistanche deserticolia) fleshy stem, remove impurity, cut into 0.3cm Sheet, scalds 1min in the hot water that temperature is 100 DEG C, takes out;-40 DEG C ± 5 DEG C, pressure 2~10Pa, Lyophilization 24 hours,.
Gained decoction pieces light brown yellow, the visible fleshly scale leaf having, matter is crisp, and tangent plane has point-like vascular bundle, row Row corrugate ring grain, feeble QI, taste is sweet, micro-hardship.
In Syrups by HPLC, the desertliving cistanche sheet of present invention processing, the content of echinacoside is 0.44%, the content of verbascoside is 0.32%.
Embodiment 2
Take fresh tube flower herba cistanches (C.tubulosa) fleshy stem, remove impurity, cut into 1.0cm sheet, In the hot water that temperature is 80 DEG C, scald 3min, take out;-45 DEG C ± 10 DEG C, pressure 5~10Pa, freezing It is dried lyophilization in 36 hours,.
Gained decoction pieces white, the visible fleshly scale leaf having, matter is crisp, and tangent plane has point-like vascular bundle, is arranged in Wavy ring grain, feeble QI, taste is sweet, micro-hardship.
In Syrups by HPLC, the Cistanche Tubulosa decoction pieces of present invention processing, the content of echinacoside is 0.486%, the content of verbascoside is 0.73%.
Embodiment 3
Take fresh Saline Cistanche Herb (C.salsa (C.A.Mey.) G.Beck) fleshy stem, remove impurity, Cut into 0.7cm sheet, 100 DEG C of Steam by water bath 5min, take out;-30 DEG C ± 10 DEG C, pressure 10~20Pa, Lyophilization lyophilization in 48 hours,.
Gained decoction pieces canescence, the visible fleshly scale leaf having, matter is crisp, and tangent plane has point-like vascular bundle, arrangement Corrugate ring grain, feeble QI, taste is sweet, micro-hardship.
In Syrups by HPLC, the Cistanche Tubulosa decoction pieces of present invention processing, the content of echinacoside is 0.54%, the content of verbascoside is 0.37%.
Embodiment 4
Take fresh Herba Cistanches sinensis (C.sinensis G.Beck) fleshy stem, remove impurity, cut into 1.5cm Sheet, places 15min in being connected with vapour vessel, takes out;-50 DEG C ± 10 DEG C, pressure 15~20Pa, It is dried lyophilization in 12 hours,.
Gained decoction pieces sundown, the visible fleshly scale leaf having, matter is crisp, and tangent plane has point-like vascular bundle, row Row corrugate ring grain, feeble QI, taste is sweet, micro-hardship.
In Syrups by HPLC, the desertliving cistanche sheet of present invention processing, the content of echinacoside is 0.52%, the content of verbascoside is 0.26%.
In a word, the processing method of Herba Cistanches of the present invention, the decoction pieces color obtained is pale, attractive in appearance;Effectively The content of composition echinacoside and verbascoside is high, and total content is all more than 0.6%.
Specific description of embodiments of the present invention above is not limiting as the present invention, and those skilled in the art can To be variously modified according to the present invention or to deform, without departing from the spirit of the present invention, all should be belonged to this Invention scope of the following claims.

Claims (9)

1. a processing method for Herba Cistanches medical material, including:
1) fresh herba cistanches medical material is removed impurity, get silt express developed with water, cut into sheet;
2) the described sheet that step 1 obtains, high temperature kill enzymes processes 1-15min, and killing ferment treatment temperature is 70-100 ℃;
3) the described sheet after heat treatment, lyophilization, temperature is-50 DEG C ± 30 DEG C, pressure 2~20Pa, dry Dry 12-48 hour;
The desertliving cistanche sheet color and luster that described processing method obtains is pale, surface light brown yellow, canescence or White, quality is dried, and the content of principle active component echinacoside and verbascoside is tradition decoction pieces More than 10 times of processing method.
Processing method the most according to claim 1, it is characterised in that: in step 3, described cold Lyophilizing is dry,
Temperature is-40 DEG C ± 10 DEG C, pressure 2~10Pa, is dried 24-48 hour.
Processing method the most according to claim 1, it is characterised in that: in step 2, described in kill Ferment treatment includes: hot water soaks sheet 1-15min described in described sheet 1-10min, Steam by water bath, Or utilize pipeline steam to fumigate described sheet 1-15min.
Processing method the most according to claim 1, it is characterised in that kill ferment treatment temperature described in: It it is 100 DEG C.
Processing method the most according to claim 3, it is characterised in that kill enzyme processing time described in: For 2-5min.
Processing method the most according to claim 1, it is characterised in that: the thickness of described sheet is 0.1-1.5cm。
Processing method the most according to claim 6, it is characterised in that the thickness of described sheet is 0.5-1.0cm。
8. according to the processing method described in any one of claim 1 to 7, it is characterised in that: described meat Herba Cistanches medical material include Herba Cistanches (Cistanche deserticolia), Cistanche Tubulosa (C.tubulosa), Saline Cistanche Herb (C.salsa (C.A.Mey.) G.Beck), Herba Cistanches sinensis (C.sinensis G.Beck) With other pharmaceutically acceptable plant of Cistanche deserticola.
9. the processing method that a kind utilizes according to any one of claim 1 to 8 processes the meat desert obtained Rong's decoction pieces.
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CN105663261A (en) * 2016-03-18 2016-06-15 内蒙古王爷地苁蓉生物有限公司 Fresh product cistanche salsa raw material processing method
CN105902620A (en) * 2016-03-18 2016-08-31 内蒙古王爷地苁蓉生物有限公司 Fresh cistanche decoction piece and preparation method thereof
CN106692311A (en) * 2016-12-23 2017-05-24 庆阳敦博科技发展有限公司 Processing method of herba cistanche tablet
CN113181243A (en) * 2021-05-18 2021-07-30 甘肃省方熙药业科技有限公司 Method for freeze drying cistanche
CN114391628A (en) * 2022-02-18 2022-04-26 内蒙古农业大学 Cistanche browning prevention color fixative and cistanche crisp chip preparation method
CN118077885A (en) * 2022-04-13 2024-05-28 河西学院 Instant cistanche deserticola product and preparation method thereof
CN115381015B (en) * 2022-08-30 2024-03-22 景泰德勤农业科技有限公司 Fresh cistanche (desert) preservation method
CN118340804B (en) * 2024-03-15 2024-09-24 兰州大学 Processing method for improving content of cynomorium songaricum nutritional ingredients

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CN101223985A (en) * 2007-12-28 2008-07-23 中山大学 Producing process of improving desertliving cistanche sheet quality
CN101249143B (en) * 2008-01-11 2011-08-24 中山大学 Preparation for increasing medicinal value of Parasitism in Cistanche decoction pieces
CN101485731A (en) * 2008-01-16 2009-07-22 杏辉天力(杭州)药业有限公司 Processing method for improving ingredient content of phenylethanoid glycosides in fresh Chinese medicine desertliving cistanche
CN103070447A (en) * 2013-01-14 2013-05-01 孟令刚 Integral herba cistanche slice and preparation method thereof

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