CN106138141B - A kind of ripe Radix Notoginseng and preparation method thereof - Google Patents

A kind of ripe Radix Notoginseng and preparation method thereof Download PDF

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CN106138141B
CN106138141B CN201610644727.2A CN201610644727A CN106138141B CN 106138141 B CN106138141 B CN 106138141B CN 201610644727 A CN201610644727 A CN 201610644727A CN 106138141 B CN106138141 B CN 106138141B
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ginsenoside
radix notoginseng
saponin
ripe
notoginseng
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CN106138141A (en
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茅仁刚
代向向
吴献荣
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Shanxi Challenge & Young Pharmaceutical Group Co Ltd
Sichuan C&y Traditional Chinese Medicine Co Ltd
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Shanxi Challenge & Young Pharmaceutical Group Co Ltd
Sichuan C&y Traditional Chinese Medicine Co Ltd
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    • A61K36/25Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
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    • A61K31/7028Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
    • A61K31/7034Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin
    • A61K31/704Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin attached to a condensed carbocyclic ring system, e.g. sennosides, thiocolchicosides, escin, daunorubicin
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/13Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
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    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting

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Abstract

The invention discloses a kind of ripe Radix Notoginseng, are calculated according to the percentage of its weight, total saponin content 6.0-12.0%, wherein the sum of the content for the rudimentary property saponin(e being converted into accounts for the 40-90% of ripe arasaponin, the intrinsic saponin(e of Radix Notoginseng includes Panax Notoginseng saponin R1, ginsenoside Rg1, ginsenoside Rb1, the low polarity saponin being converted into includes ginsenoside 20(S) and-Rh1, ginsenoside 20(R)-Rh1, ginsenoside Rd, ginsenoside Rk3, ginsenoside Rh4, ginsenoside 20(S)-Rg3, ginsenoside 20(R)-Rg3, ginsenoside Rk1, ginsenoside Rg5.The invention also discloses the preparation methods of ripe Radix Notoginseng, a kind of ripe Radix Notoginseng formed with specific saponin(e and its ratio is obtained by accurately controlling amount of water, processing temperature and concocted time, there is the low polarity saponin active constituent for improving immune function and antitumor action rich in what be there's almost no in raw sangqi ginseng.

Description

A kind of ripe Radix Notoginseng and preparation method thereof
Technical field
The invention belongs to the field of Chinese medicines, and in particular to a kind of ripe Radix Notoginseng and preparation method thereof.
Background technique
Radix Notoginseng, alias: panicled fameflower root, Panax pseudoginseng, Typhonium flagelliforme (Lodd.) Blume, mountain paint, Radix Notoginseng, Classification system: Panax Notoginseng (Burk.) F.H.Chen is Araliaceae Panax herbaceos perennial, and rhizomes is short, fleshy root cylinder Shape is distributed in the ground such as Yunnan, Guangxi, Jiangxi, Sichuan.Radix Notoginseng is mainly rich in saponin(e, flavones, Argine Monohydrochloride and non-protein amino The ingredients such as acid, polysaccharide, albumen, sterol, inorganic matter, volatile oil and grease.The principle active component of Radix Notoginseng is notoginsenoside, so far Until, from isolated more than 60 monomer saponin ingredient of Radix Notoginseng different parts, most of these monomer saponin ingredients are up to Ma 20 (S)-protopanaxadiol-types [20 (S)-protopanaxadio1] of alkane and 20 (S)-protopanaxatriol type [20 (S)- Peotopanaxatrio1], but do not find containing oleanolic acid type saponin.This has significantly with congener ginseng and American Ginseng Difference.
According to the difference of concocting method, the mitogenetic Radix Notoginseng of notoginseng decoction piece, ripe Radix Notoginseng.Raw sangqi ginseng its intrinsic soap after high temperature processes The configuration that cracking reaction, side chain dehydration and C-20 occur for the glycosidic bond of glycosides changes and generates new saponin(e, i.e. Radix Notoginseng soap Glycosides R1, ginsenoside Rg1, ginsenoside Rb1The content of 3 kinds of monomer saponins gradually decreases, newly-generated ginsenoside 20 (S)- Rh1, ginsenoside 20 (R)-Rh1, ginsenoside Rd, ginsenoside Rk3, ginsenoside Rh4, ginsenoside 20 (S)-Rg3, ginseng Saponin(e 20 (R)-Rg3, ginsenoside Rk1, ginsenoside Rg5Content be stepped up.Shifting degree is by the aqueous of Radix Notoginseng Amount and processing temperature and time correlation, the percentage composition for the low polarity saponin being converted into change between zero to 100%, This creates the ripe Radix Notoginseng product from raw sangqi ginseng to full ripe numerous differing maturities, the different ripe Radix Notoginseng of these maturity There is different effects because material base is different.Radix Notoginseng just has saying for " the raw ripe benefit that disappears " from ancient times, and raw sangqi ginseng stops with scattered silt Blood, detumescence ding-tong effect are mainly used for spitting blood, and spit blood, hematochezia, metrorrhagia and metrostaxis, traumatic hemorrhage, chest and abdomen are sharp, tumbling and swelling.Ripe Radix Notoginseng Be longer than nourishing, Radix Notoginseng can mitigate the haemostatic properties of Radix Notoginseng by processing, and enhancing Radix Notoginseng enriches blood, the curative effect of tonifying Qi, have it is anti-inflammatory, It is anti-aging, antitumor, the function of immunity of organism is improved, maturity is higher, and benefiting action is stronger.
In many factors for influencing ripe Radix Notoginseng maturity, the water content of Radix Notoginseng and the temperature and time of processing are to determine Three big key factors of ripe Radix Notoginseng maturity, directly decide the variation of saponin(e type and content in ripe Radix Notoginseng.With amount of water Increase, temperature increases and the time extends, the intrinsic saponin(e such as Panax Notoginseng saponin R in raw sangqi ginseng1, ginsenoside Rg1, ginsenoside Rb1 It will be converted and gradually decrease by lasting cracking, and gradually be down to the extremely low water close to zero from 5% or more raw sangqi ginseng weight percentage It is flat, and crack low polarity saponin ginsenoside 20 (the S)-Rh being converted into1, ginsenoside 20 (R)-Rh1, ginsenoside Rd, people Join saponin(e Rk3, ginsenoside Rh4, ginsenoside 20 (S)-Rg3, ginsenoside 20 (R)-Rg3, ginsenoside Rk1, ginsenoside Rg5Then gradually increase, almost nil extremely low value sustainable growth is to 5% or more of ripe three seven weight from raw sangqi ginseng.Thus may be used Prepared by different amount of water, steaming temperature and ageing ripe three are seen seventh is that the different product of inherent quality, accurate control are steamed The technical parameter for boiling technique is the necessary condition for obtaining the ripe Radix Notoginseng with specific low polarity saponin type and content.Low polarity people Join saponin(e Rg3It is used as the approval listing of a kind new medicine, which is suitable for the treatment of tumour, has and significantly inhibit tumour thin Born of the same parents' proliferation function.And ginsenoside Rh1, ginsenoside Rh4, ginsenoside Rk3, ginsenoside Rg3, ginsenoside Rg5, ginseng soap Glycosides Rk1Immune function of human body and anti-tumor activity are improved Deng also having been demonstrated to have, the type and content of these low polarity saponins Difference determine the difference of ripe Radix Notoginseng curative effect.
Traditional concocting method of Radix Notoginseng is net system, baking or sunning, profit cutting or crushing, and raw sangqi ginseng, raw sangqi ginseng piece is made With raw sangqi ginseng powder.Ripe Radix Notoginseng in the prior art is also such as the Chinese patent CN200910113914.8 public by steaming to obtain A kind of Radix Notoginseng processing method and products thereof is opened, it is characterised in that take the root and rhizome of Radix Notoginseng, be first processed into raw sangqi ginseng or moisturize Radix Notoginseng;Or raw sangqi ginseng piece, the sanqi tablets that moisturize;Or Radix Notoginseng powder;106~125 DEG C of high temperature, high pressure in flowing steam pot are set again 0.03~0.14MPa is steamed 1~15 hour, until inside and outside is in sepia, is taken out, it is dry to get.Using ripe the three of technique preparation Seven, wherein arasaponin is possible to from substantially unconverted to conversion completely, i.e., processes within the scope of its different technology conditions At the different ripe Radix Notoginseng of maturity, inherent quality has the difference of essence, and from the patent specification attached drawing It can't see low polarity saponin ginsenoside 20 (the S)-Rh being converted into HPLC chromatogram at all1, ginsenoside 20 (R)-Rh1、 Ginsenoside Rd, ginsenoside Rk3, ginsenoside Rh4, ginsenoside 20 (S)-Rg3, ginsenoside 20 (R)-Rg3, ginseng soap Glycosides Rk1, ginsenoside Rg5Chromatographic peak.And application No. is 201510023537.4 patent of invention disclose a kind of ripe Radix Notoginseng and Preparation method and use, the ripe Radix Notoginseng are based on weight percent, contain Panax Notoginseng saponin R1, ginsenoside Rg1, ginsenoside Rb1 The total amount of three must not be less than 5.0%, wherein Panax Notoginseng saponin R1Content must not be less than 0.4%, ginsenoside Rg1Content not It obtains and is less than 2.0%, ginsenoside Rb1Content must not be less than 1.5%;Contain ginsenoside Rh4, ginsenoside 20 (S)-Rg3、 Ginsenoside 20 (R)-Rg3The total amount of three must not be less than 0.5%, wherein ginsenoside Rh4Content must not be less than 0.3%, ginseng Saponin(e 20 (S)-Rg3Content is no less than 0.06%, ginsenoside 20 (R)-Rg3Content is no less than 0.03%.Should patent disclosed that A kind of low-down ripe Radix Notoginseng of transforming degree.Notoginsenoside in 2015 editions regulation raw sangqi ginsengs of Pharmacopoeia of People's Republic of China R1, ginsenoside Rg1, ginsenoside Rb1Total content must not be less than 5.0%, i.e., according to preparation process disclosed in the patent of invention The ripe Radix Notoginseng of preparation still conforms to the standards of pharmacopoeia of raw sangqi ginseng, Panax Notoginseng saponin R therein1, ginsenoside Rg1, ginsenoside Rb1 Substantially unconverted, and the low polarity saponin content being converted into is very low, the composition ratio and this patent of saponin constituent are complete It is inconsistent, illustrate that above-mentioned patent is unrelated with this patent.
Summary of the invention
An object of the present invention is to provide a kind of ripe Radix Notoginseng, be provided in particular in it is a kind of disappear mend it is in a basic balance have it is specific The ripe Radix Notoginseng of saponin(e composition.
An object of the present invention is to provide a kind of new processing procedure of ripe Radix Notoginseng.
Ripe Radix Notoginseng provided by the invention, have following technical characteristic: i.e. based on its weight percent, which contains Total saposins are 6.0-12.0%, wherein the sum of the content of the rudimentary property saponin(e in 9 be converted into kind accounts for the 40- of ripe arasaponin 90%, preferably 50-80%.The intrinsic saponin(e of Radix Notoginseng includes Panax Notoginseng saponin R1, ginsenoside Rg1, ginsenoside Rb1, three's total content Less than 5.0%, each monomer saponin content is successively less than 0.01-0.5%, 0.2-2.0% and 0.3-3.0%;Nine be converted into A low polarity saponin ginsenoside 20 (S)-Rh1, ginsenoside 20 (R)-Rh1, ginsenoside Rd, ginsenoside Rk3, ginseng soap Glycosides Rh4, ginsenoside 20 (S)-Rg3, ginsenoside 20 (R)-Rg3, ginsenoside Rk1, ginsenoside Rg5Content be followed successively by 0.3-1.5%, 0.1-1.0%, 0.05-1.0%, 0.2-1.5%, 0.5-3.0%, 0.1-1.0%, 0.05-0.5%, 0.1- 1.0%, 0.5-3.0%.
Ripe Radix Notoginseng provided by the invention the preparation method is as follows:
1) it cleans: taking Radix Notoginseng dry product, carry out prewashing with water, wash away the soil for being attached to Radix Notoginseng surface, add Radix Notoginseng dry product weight The drinking water of 0.5~2 times of amount of amount is dipped to water and blots, then carries out fine purifiation to Radix Notoginseng with drinking water, thoroughly removes Radix Notoginseng surface Soil and impurity must moisten Radix Notoginseng;Or Radix Notoginseng fresh goods is taken, the soil and impurity for removing Radix Notoginseng surface are thoroughly cleaned with drinking water, are obtained Moisten Radix Notoginseng;
2) it pre-processes: taking profit Radix Notoginseng, dry, pulverize, obtain raw sangqi ginseng powder, 0.5-2 times of weight of raw sangqi ginseng powder weight is added Drinking water infiltrates to the saturating heart, obtains profit Radix Notoginseng powder;Or profit Radix Notoginseng is taken, 1-3 millimeters of piece is cut into, profit sanqi tablets are obtained;
3) it steams: taking profit Radix Notoginseng, profit sanqi tablets or profit Radix Notoginseng powder, be laid in charging tray, with a thickness of 1-5 centimetres, set pressure In pot, steamed in 116-125 DEG C 1-4 hours;
4) dry: it is 2-24 hours dry in 50-105 DEG C, obtain ripe Radix Notoginseng, ripe sanqi tablets or ripe Radix Notoginseng powder;
5) it crushes: crushing, obtain ripe Radix Notoginseng powder;Or crush, air-flow crushing obtains ripe Radix Notoginseng superfine powder.
Radix Notoginseng dry product described in step 1) or fresh Radix Notoginseng raw material be the main root of araliaceae ginseng plant Radix Notoginseng, supporting root, One or more of rhizome, preferably rhizomes of Panax notoginseng;Profit Radix Notoginseng in step 3), profit sanqi tablets or moisten Radix Notoginseng powder to steam condition excellent It is selected as 118-122 DEG C of temperature, time 2-3 hour;Drying means described in step 4) is constant pressure and dry or vacuum drying.
The present invention obtains a kind of ripe Radix Notoginseng that depth processes by the accurate control of amount of water, processing temperature and time, It has the low polarity saponin active constituent for improving immune function and antitumor action rich in what be there's almost no in raw sangqi ginseng.
Detailed description of the invention
Fig. 1 is the HPLC chromatogram for mixing reference substance, wherein 1: Panax Notoginseng saponin R1, 2: ginsenoside Rg1, 3: ginsenoside Rb1, 4: ginsenoside 20 (S)-Rh1, 5: ginsenoside 20 (R)-Rh1, 6: ginsenoside Rd, 7: ginsenoside Rk3, 8: ginseng Saponin(e Rh4, 9: ginsenoside 20 (S)-Rg3, 10: ginsenoside 20 (R)-Rg3, 11: ginsenoside Rk1, 12: ginsenoside Rg5
Fig. 2 is the HPLC chromatogram of ripe Radix Notoginseng prepared by embodiment 1, wherein 1: Panax Notoginseng saponin R1, 2: ginsenoside Rg1, 3: Ginsenoside Rb1, 4: ginsenoside 20 (S)-Rh1, 5: ginsenoside 20 (R)-Rh1, 6: ginsenoside Rd, 7: ginsenoside Rk3, 8: ginsenoside Rh4, 9: ginsenoside 20 (S)-Rg3, 10: ginsenoside 20 (R)-Rg3, 11: ginsenoside Rk1, 12: people Join saponin(e Rg5
Specific embodiment
Present pre-ferred embodiments are provided with reference to the accompanying drawing, in order to explain the technical scheme of the invention in detail.
The preparation of the ripe Radix Notoginseng powder of embodiment 1
Raw sangqi ginseng rhizome (clip) dry product 5kg is taken, is cleaned up with drinking water, 5kg drinking water is added to be dipped to the heart, with drink It is thoroughly cleaned with water and removes soil impurity, be cut into 1 millimeter of piece, set and steamed in pressure cooker in 118 DEG C 3 hours, 50 DEG C of decompressions are dry Dry 24 hours, fine powder was ground into get ripe Radix Notoginseng powder 4.56kg.HPLC method measures the saponin content in ripe Radix Notoginseng powder, and as a result three Seven saponin(e R10.38%, ginsenoside Rg11.78%, ginsenoside Rb12.53%, ginsenoside 20 (S)-Rh1 0.63%, ginsenoside 20 (R)-Rh10.34%, ginsenoside Rd 0.56%, ginsenoside Rk30.51%, ginsenoside Rh41.58%, ginsenoside 20 (S)-Rg30.44%, ginsenoside 20 (R)-Rg30.24%, ginsenoside Rk1 0.26%, ginsenoside Rg51.11%.
The preparation of the ripe sanqi tablets of embodiment 2
Raw sangqi ginseng main root dry product 5kg is taken, is cleaned up with drinking water, is added 2.5kg drinking water to be dipped to the heart, use drinking water Thoroughly cleaning removes soil impurity, is cut into 3 millimeters of sheet, sets in pressure cooker in 116 DEG C of temperature, steams 4 hours, 105 DEG C often Dry 8 hours are pressed dry to get ripe sanqi tablets 4.42kg.HPLC method measures the saponin content in ripe Radix Notoginseng powder, as a result Panax Notoginseng saponin R1 0.29%, ginsenoside Rg11.40%, ginsenoside Rb11.94%, ginsenoside 20 (S)-Rh10.61%, ginsenoside 20(R)-Rh10.33%, ginsenoside Rd 0.46%, ginsenoside Rk30.50%, ginsenoside Rh41.57%, ginseng Saponin(e 20 (S)-Rg30.42%, ginsenoside 20 (R)-Rg30.22%, ginsenoside Rk10.25%, ginsenoside Rg5 1.16%.
The preparation of the ripe Radix Notoginseng of embodiment 3
Fresh Radix Notoginseng main root 5kg is taken, is cleaned up, is set in pressure cooker in 121 DEG C of temperature, is steamed 2 hours, 100 DEG C of normal pressures are dry Dry 12 hours to get ripe Radix Notoginseng 4.67kg.HPLC method measures the saponin content in ripe Radix Notoginseng powder, as a result Panax Notoginseng saponin R1 0.21%, ginsenoside Rg10.78%, ginsenoside Rb12.18%, ginsenoside 20 (S)-Rh10.71%, ginsenoside 20(R)-Rh10.12%, ginsenoside Rd 0.06%, ginsenoside Rk30.39%, ginsenoside Rh41.61%, ginseng Saponin(e 20 (S)-Rg30.17%, ginsenoside 20 (R)-Rg30.08%, ginsenoside Rk10.25%, ginsenoside Rg5 0.65%.
The preparation of the ripe Radix Notoginseng of embodiment 4
Raw sangqi ginseng rhizome dry product 4kg, supporting root dry product 1kg are taken, is cleaned up with drinking water, 7.5kg drinking water is added to be dipped to The saturating heart is thoroughly cleaned with drinking water and removes soil impurity, is set and is steamed 1 hour in pressure cooker in 125 DEG C, and 80 DEG C to be dried under reduced pressure 2 small When to get ripe Radix Notoginseng 4.49kg.HPLC method measures the saponin content in ripe Radix Notoginseng powder, as a result Panax Notoginseng saponin R10.47%, ginseng Saponin(e Rg11.93%, ginsenoside Rb12.84%, ginsenoside 20 (S)-Rh10.44%, ginsenoside 20 (R)-Rh1 0.23%, ginsenoside Rd 0.53%, ginsenoside Rk30.41%, ginsenoside Rh40.68%, ginsenoside 20 (S)- Rg30.37%, ginsenoside 20 (R)-Rg30.23%, ginsenoside Rk10.19%, ginsenoside Rg50.96%.
The preparation of the ripe sanqi tablets of embodiment 5
Raw supporting root dry product 5kg is taken, is cleaned up with drinking water, 5kg drinking water is added to be dipped to the heart, it is thoroughly clear with drinking water Soil impurity is removed in washout, is cut into 2 millimeters of sheet, sets in pressure cooker in 120 DEG C of temperature, steams 2.5 hours, 70 DEG C are dried under reduced pressure 16 hours to get ripe sanqi tablets 4.38kg.HPLC method measures the saponin content in ripe Radix Notoginseng powder, as a result Panax Notoginseng saponin R1 0.15%, ginsenoside Rg10.55%, ginsenoside Rb11.61%, ginsenoside 20 (S)-Rh10.73%, ginsenoside 20(R)-Rh10.41%, ginsenoside Rd 0.49%, ginsenoside Rk30.70%, ginsenoside Rh42.71%, ginseng Saponin(e 20 (S)-Rg30.72%, ginsenoside 20 (R)-Rg30.38%, ginsenoside Rk10.52%, ginsenoside Rg5 1.72%.
The dry Radix Notoginseng of comparative example 1 prepares ripe Radix Notoginseng
According to the ripe Radix Notoginseng of patent of invention CN 200710066195.X and cooked Panax notoginseng standard extract and its Application Example 1 Method, take dry Radix Notoginseng main root 5kg, be broken for granule, be placed in high-pressure sterilizing pot 120 DEG C and steam 12 hours, 55 DEG C are dry It is dry, crush, cross 120 mesh to get.HPLC method measures the saponin content in ripe Radix Notoginseng powder, as a result Panax Notoginseng saponin R10.04%, people Join saponin(e Rg10.12%, ginsenoside Rb10.37%, ginsenoside 20 (S)-Rh10.52%, ginsenoside 20 (R)-Rh1 0.32%, ginsenoside Rd 0.21%, ginsenoside Rk31.28%, ginsenoside Rh42.87%, ginsenoside 20 (S)- Rg30.24%, ginsenoside 20 (R)-Rg30.12%, ginsenoside Rk10.57%, ginsenoside Rg53.54%.
Comparative example 2 steams the preparation of ripe Radix Notoginseng powder
Preparation method and the ripe Radix Notoginseng of purposes embodiment 2b according to a kind of ripe Radix Notoginseng of patent of invention CN201510023537.4 The preparation method of powder takes pseudo-ginseng 5kg, cleans, and cleans, adds 1.75kg drinking water water to moisturize, with either pure steam in temperature 110 At DEG C, steam 3 hours, be dried, crushed into most fine powder to get.HPLC method measures the saponin content in ripe Radix Notoginseng powder, as a result Radix Notoginseng Saponin(e R10.63%, ginsenoside Rg13.27%, ginsenoside Rb13.49%, ginsenoside 20 (S)-Rh10.23%, Ginsenoside 20 (R)-Rh10.10%, ginsenoside Rd 0.47%, ginsenoside Rk30.30%, ginsenoside Rh4 0.87%, ginsenoside 20 (S)-Rg30.21%, ginsenoside 20 (R)-Rg30.11%, ginsenoside Rk10.13%, people Join saponin(e Rg50.62%.
The quantitative analysis method of ripe compound components of panax notoginseng, comprising the following steps:
1) preparation of test solution:
Ripe Radix Notoginseng powder 0.6g is taken, it is accurately weighed, it sets in triangular flask, methanol 50ml is added in precision, and weighed weight sets 80 DEG C of water It is kept in bath slightly boiled 2 hours, lets cool, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, filtered, take subsequent filtrate, i.e., ?;
2) preparation of reference substance solution:
Precision weighs Panax Notoginseng saponin R respectively1, ginsenoside Rg1, ginsenoside Rb1, ginsenoside 20 (S)-Rh1, ginseng Saponin(e 20 (R)-Rh1, ginsenoside Rd, ginsenoside Rk3, ginsenoside Rh4, ginsenoside 20 (S)-Rg3, ginsenoside 20 (R)-Rg3, ginsenoside Rk1, ginsenoside Rg5Reference substance is set in volumetric flask, and methanol is added to be respectively prepared containing about each monomer saponin The reference substance solution of 3-100 μ g/mL takes subsequent filtrate through 0.45 μm of membrane filtration to obtain the final product;
3) chromatographic condition
Chromatographic column: Agilent Zorbax SB-C18 (4.6mm × 250mm, 5 μm);Column temperature: 35 DEG C;Sample volume: 20 μ L; Flow velocity: 1.0mL/min;DAD detector: Detection wavelength: 203nm;Mobile phase: water (A)-acetonitrile (B) is carried out by the condition of table 1 Gradient elution: system suitability research requires the theoretical cam curve of ginsenoside Rb1 not less than 100000.
1 mobile phase gradient of table
4) methodological study
(1) investigation of standard curve:
20 μ L of reference substance solution, successively sample introduction, records chromatogram, draws standard curve to concentration (X) with peak area (Y), It the results are shown in Table 2.
Each saponin(e standard solution linear relationship of table 2 investigates result
The result shows that each standard items are in good linear relationship with peak area within the scope of sample volume.
(2) detection limit, quantitative limit are investigated:
Sample volume when with peak height being about 3 times of baseline noise is detection limit, when with peak height being about 10 times of baseline noise into Sample amount is quantitative limit.It the results are shown in Table 3.
Each saponin(e of table 3 detection limit and quantitative limit test data
(3) recovery test
Precision weighs 6 parts of ripe Notoginseng Root 96.00mg, is set in 25mL volumetric flask respectively, is separately added into and is equal to sample and contains Each saponin(e reference substance of amount adds 70% methanol aqueous solution to close to scale, room temperature ultrasound 40min, after being cooled to room temperature, 70% methanol Aqueous solution constant volume, shakes up, and through 0.45 μm of membrane filtration, takes subsequent filtrate, is measured, and calculates the content of each saponin(e, calculates recycling Rate.It the results are shown in Table 4.
Each saponin(e rate of recovery of table 4 investigates result
(4) precision test
Take mixed mark, the ginsenoside Rb under linear determination item1Titer is repeated in measurement 6 times, the results showed that the analysis Method precision is good.It the results are shown in Table 5.
Each saponin(e standard solution precision test data of table 5
(5) repeated experiment
Precision weighs 6 parts of ripe Notoginseng Root 96.00mg, is set in 25mL volumetric flask respectively, adds 70% methanol aqueous solution to connecing Nearly scale, room temperature ultrasonic extraction 40min, after being cooled to room temperature, 70% methanol aqueous solution constant volume is shaken up, and extracting solution is filtered through 0.45 μm Film filtering, takes subsequent filtrate, is measured, and calculates the content of each saponin(e in ripe Notoginseng Root, calculates RSD.The result shows that: this method It is repeated good.It the results are shown in Table 6.
Each saponin content of the ripe Radix Notoginseng extracting solution of table 6 measures repeated experiment data
(6) stability experiment
The sample (96.07mg) under repeated experiment item is taken, measures 1 time within each 2 hours, investigates 16 hours, each saponin(e The RSD of peak area is respectively less than 3.5%, the results showed that each saponin(e is basicly stable in 16 hours in ripe Radix Notoginseng extracting solution, is shown in Table 7.
Each saponin content of the ripe Radix Notoginseng extracting solution of table 7 measures stability experiment data
5) assay
20 μ L of test solution is taken, successively sample introduction, record chromatogram, calculated according to the standard curve of reference substance solution for examination The content of various saponin(es in product solution.
Reference substance and the typical HPLC chromatogram of ripe Radix Notoginseng are shown in that Fig. 1 reference substance HPLC chromatogram, Fig. 2 are made according to embodiment 1 The HPLC chromatogram of standby ripe Radix Notoginseng.

Claims (3)

1. a kind of preparation method of ripe Radix Notoginseng, it is characterised in that the following steps are included:
Raw sangqi ginseng dry product is taken, is cleaned up with drinking water, 1 times of weight drinking water is added to be dipped to the heart, is thoroughly cleaned with drinking water Soil impurity is removed, 2 millimeters of sheet is cut into, sets and steamed in pressure cooker in 120 DEG C 2.5 hours, 70 DEG C are dried under reduced pressure 16 hours.
2. the preparation method of ripe Radix Notoginseng according to claim 1, which is characterized in that the raw sangqi ginseng dry product of selection is in step 1) One or more of the main root of araliaceae ginseng plant Radix Notoginseng, supporting root, rhizome.
3. the preparation method of ripe Radix Notoginseng according to claim 1, which is characterized in that the raw sangqi ginseng dry product of selection is in step 1) The rhizome of araliaceae ginseng plant Radix Notoginseng.
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