CN103585017A - Industrialized preparing process for traditional Chinese medicine decoction pieces simmered monkshood and automatic temperature-control simmering furnace - Google Patents
Industrialized preparing process for traditional Chinese medicine decoction pieces simmered monkshood and automatic temperature-control simmering furnace Download PDFInfo
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Abstract
The invention discloses an industrialized preparing process for traditional Chinese medicine decoction pieces simmered monkshood and an automatic temperature-control simmering furnace. The industrialized preparing process is characterized by including taking salted aconite roots, selecting and grading, placing the salted aconite roots in a container, adding water until the salted aconite roots are completely submerged, changing the water 2-4 times each day during soaking, taking out the salted aconite roots when conductivity of soaked water at 25 DEG C is lowered to be below 6000 microsecond per centimeter, enabling the top ends of the salted aconite roots to be up and the pointed ends of the salted aconite roots to be down, placing the salted aconite roots on a shelf of the automatic temperature-control simmering furnace, covering a plurality of layers of clean ginger pieces on the salted aconite roots, adding fine chaff ash untile a furnace body of the simmering furnace is fully filled, setting heating temperature of a lower heating component to be 70-130 DEG C and that of an upper heating component to be 110-180 DEG C, heating and simmering for 24-48 hours, taking out the salted aconite roots until the ash is cold, steaming, slicing and drying. Production process parameters are accurate and controllable, product difference between batches is obviously reduced, labor intensity is remarkably lowered, production cost is lowered, production environment meets GMP (good manufacturing practice) requirements, and a solid foundation is laid for standardized and industrialized production of the simmered monkshood.
Description
Technical field
The invention belongs to pharmaceutical equipment technical field, relate to a kind of processing procedure and Preparation process equipment of simmering Chinese medicine processed, be specifically related to industrialization processing procedure and temperature automatically controlled stewing stove processed that a kind of prepared slices of Chinese crude drugs are simmered Radix Aconiti Lateralis Preparata, be mainly used in the production and processing that Chinese medicine is simmered Radix Aconiti Lateralis Preparata.
Background technology
Stewing method is the concocting method of often using in Chinese medicine processing, is medicine directly or with wetted surface, l Water Paper is wrapped up, and is embedded in showing tremendous enthusiasm ash, or Pulvis Talci, or the concocting method of slow heating in Testa Tritici is called stewing method.Its object is mainly to reduce toxic and side effects, or relaxes the property of medicine, or strengthens drug effect.As simmer Radix Aconiti Lateralis Preparata, Semen Myristicae, roasted RADIX PUERARIAE, Radix Aucklandiae (roasted), Fructus Chebulae (roasted) etc.But, while processing medical material due to the system of stewing, still adopt traditional empirical method, it concocts the duration and degree of heating and the time is difficult for grasping, simmering technological parameter processed is difficult to quantize, easily burn, burn out medical material, do not meet modern pharmaceutical production GMP requirement, be difficult to realize industrialized great production, cause stewing method to be on the verge of in modern Chinese medicine processing technique lost.As simmer Radix Aconiti Lateralis Preparata, and its poison of can dispelling after the famous doctor of the Qing Dynasty thanks that star is shining and claims it to simmer, Liu Qiwen, declines and waits disease to have the merit of original recuperating depleted YANG benefit fire yang deficiency fire.But because of it, produce with quality control and still need pharmaceutical worker's experience to control, be difficult to meet the requirement of the production of modern Chinese medicine decoction pieces and clinical practice, cause simmering goods without manufacturer production Radix Aconiti Lateralis Preparata, this method has been condition in imminent danger.According to Chinese Academy of Social Sciences's Chinese medicine national conditions investigation, Chinese medicine quality has become one of major reason affecting Efficacy of Traditional Chinese Medicine, wherein Preparation process method can not adhere to traditional handicraft be very crucial influence factor [Chen Qiguang. take into account for eight and carry out Chinese medicine succession [N]. Chinese Chinese medicine report, 2012-2-13 (3)]. therefore, exploitation has modernization that temperature automatically controls, and to simmer control equipment be to produce to simmer Radix Aconiti Lateralis Preparata and other simmer a Chinese medicines processed difficult problem urgently to be resolved hurrily, to inheriting with development Chinese medicine stewing method processing technique, has important practice significance.
Summary of the invention
The object of the invention is to design industrialization processing procedure and the temperature automatically controlled stewing stove processed that a kind of prepared slices of Chinese crude drugs are simmered Radix Aconiti Lateralis Preparata, the process of preparing Chinese medicine materials such as each kind of plant or mineral grey, sand, rice, Testa Tritici, rice husk, bran coat, Pulvis Talci, Pulvis concha Mactrae of take are heat transfer medium, be mainly used in simmering the Preparation process of Radix Aconiti Lateralis Preparata, there is parameter accurately controlled, production technology favorable reproducibility and meet the features such as national GMP production requirement.Separately can be used for the stewing system processing of other Chinese crude drugs such as Semen Myristicae, Radix Puerariae, the Radix Aucklandiae, Fructus Chebulae.
One of technical scheme of the present invention: a kind of industrialization processing procedure of prepared slices of Chinese crude drugs stewing Radix Aconiti Lateralis Preparata is as follows:
(1), get Radix Aconiti Lateralis Preparata, select stepping, in placing container, add water to and flood Radix Aconiti Lateralis Preparata completely, between soak period, change water 2-4 every day, and when soaking water at 25 ℃, electrical conductivity is down to 6000 μ s/cm when following, below preferably to 4000 μ s/cm, take out, drain the water step (1) make thing;
(2), by step (1) make thing expand operative tip upper, most advanced and sophisticated under, be placed on temperature automatically controlled stewing stove rack processed, cover in the above the clean ginger slice of some layers, the thing that makes by every 100kg step (1) adds 8-16kg Rhizoma Zingiberis Recens, preferred 10-12kg, add thin bran ash, to filling, simmer furnace body processed, the heating-up temperature that lower heating component is set is 70-130 ℃, preferred 80-110 ℃, the heating-up temperature of upper heating component is 110-180 ℃, preferred 140-170 ℃, add fire bending system 24-48 hours, preferred 36-48 hour, treat ash cooling, take out Radix Aconiti Lateralis Preparata, obtain the thing that makes of step (2),
(3), the thing that makes of step (2) is placed in heating container, uninterruptedly steam 6-12 hours, preferably 8-10 hours, to mouth taste without or micro-while having numb feeling in the tongue, take out, airing to room temperature obtains the thing that makes of step (3);
(4), get the thing that makes of step (3), cut the vertical thin slice that 1-4mm is thick, preferably 2-3mm, is dried to water content 5%-13% at 60-80 ℃, preferred water content 6%-12%, obtains;
Two of technical scheme of the present invention: a kind of temperature automatically controlled stewing stove processed, it comprises cover plate 1, body of heater 2 and heating system, the interior upper and lower and/or left and right of described body of heater 2 is provided with heating component, each heating component comprises heating part and temperature sensing part, the control circuit of heating component and control chamber 6 connects to form heating system, each heating component has independently temperature control unit, control chamber 6 is arranged on the outside of body of heater 2, in body of heater 2, be provided with rack 9, rack 9 put the thing scope of operation between each heating component, simmer when processed, in body of heater 2, be provided with heat transfer medium.
Preferred: on described body of heater 2 inwalls, have and be respectively provided with a set of heating component, the thing scope of operation of putting of rack 9 is overlapped between the heating part of heating components upper and lower two.
Between the heating part of upper and lower two cover heating components, upper and lower spacing distance is 8-50cm.
Further preferably: the heating part of described heating component is electrothermal tube 5, the temperature sensing of described heating component is partly temperature sensor 4; Temperature sensor 4 and electrothermal tube 5 form a heating component independently, and independently heating component is connected with the independently temperature control unit circuit of control chamber 6.
Described electrothermal tube 5 is U-shaped, W type, snakelike, screw type heating tube or finned, flange form, threaded heating tube.
Described heat transfer medium comprises each kind of plant or mineral grey, sand, rice, Testa Tritici, rice husk, bran coat, Pulvis Talci and Pulvis concha Mactrae.
It is room temperature-300 ℃ that the temperature control parameter of stewing stove processed arranges scope.
Between described body of heater 2 body walls, be provided with thermal insulation layer 3.
On described rack 9, be evenly provided with and put thing hole 10.
Using method: Radix Aconiti Lateralis or Radix Aconiti Lateralis Preparata, with top or unified upward with tip, are placed in respectively and have equally distributed circle and put on the rack of thing hole, put into Chinese medicine and simmer furnace body processed.According to the legal processing standard of traditional concocting method or modern Chinese medicine decoction pieces, select suitable heat transfer medium, add and simmer in stove processed, and cover Radix Aconiti Lateralis or Radix Aconiti Lateralis Preparata completely.According to Radix Aconiti Lateralis Preparata, simmer process characteristic processed, depend on sub-top from most advanced and sophisticated different, the heating-up temperature upper and lower and/or heating component that left and right distributes is set respectively, wherein near the heating component temperature of Radix Aconiti Lateralis Preparata top one side, arranging need be higher than its most advanced and sophisticated side, while open temp control unit, to the concocted time of regulation, take out medical material.
Advantage of the present invention:
(1) production environment adapts to GMP requirement.Traditional method bran coat is fuel, and smog and dust are large, and production environment is severe, cannot meet the clean requirement of GMP to pharmaceutical production environment, and traditional method is on the verge of lost.The thermal source of temperature automatically controlled stewing stove processed adopts electric heating, and production environment is airtight, produces hardly smog and dust, and production environment can meet GMP requirement, for simmering Radix Aconiti Lateralis Preparata production regularization, industrialization establish a firm foundation.
(2) processing parameter is controlled.The technological parameter of traditional method mainly depends on operator's experience, obviously random, especially the firepower size in the time of cannot grasping bran coat burning, the little Radix Aconiti Lateralis Preparata of fire is difficult to be simmered thoroughly, the too greatly easy carbonization of Radix Aconiti Lateralis Preparata of fire, so product difference between batch is large, by experimental result also between known batch the standard deviation of content be obviously greater than Radix Aconiti Lateralis Preparata and simmer stewing Radix Aconiti Lateralis Preparata prepared by stove processed.Temperature automatically controlled stewing stove processed by upper and lower two can accurate temperature controlling heating tube heat, the processing parameters such as firepower, time are accurately controlled, product difference between batch obviously reduces, and easily meets GMP production requirement.
(3) labor intensity significantly reduces.Adopting traditional method to need several individuals to supervise in turn stewing process processed, need to pay close attention to the variation of firepower, add in time bran coat, is 48 hours owing to simmering the stewing time processed of Radix Aconiti Lateralis Preparata, so the production process monitoring in night be unable to do without people, labor intensity is large.Along with the rising gradually of human cost, the production cost of simmering Radix Aconiti Lateralis Preparata increases, and has a strong impact on economic benefit.And that temperature automatically controlled stewing stove processed adopts is temperature automatically controlled, only need people watch-dog ruuning situation at any time, labor intensity is little, and human cost significantly reduces, production cost decline.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention 1.
Fig. 2 is the structural representation of the embodiment of the present invention 1 rack.
Fig. 3 is the embodiment of the present invention 1 diester-type alkaloids reference substance HPLC figure.
Fig. 4 is the embodiment of the present invention 1 Radix Aconiti Lateralis Preparata diester-type alkaloids HPLC figure.
Fig. 5 is the stewing Radix Aconiti Lateralis Preparata diester-type alkaloids HPLC figure of the embodiment of the present invention 1 Jianchang side traditional method.
Fig. 6 is the stewing Radix Aconiti Lateralis Preparata diester-type alkaloids HPLC figure that the embodiment of the present invention 1 Aconitum carmichaeli is simmered stove processed.
Fig. 7 is the embodiment of the present invention 1 monoester alkaloid reference substance HPLC figure.
Fig. 8 is the embodiment of the present invention 1 Radix Aconiti Lateralis Preparata monoester alkaloid HPLC figure.
Fig. 9 is the stewing Radix Aconiti Lateralis Preparata monoester alkaloid HPLC figure that the embodiment of the present invention 1 Aconitum carmichaeli is simmered stove processed.
Figure 10 is the stewing Radix Aconiti Lateralis Preparata monoester alkaloid HPLC figure of the embodiment of the present invention 1 Jianchang side traditional method.
In Fig. 1-2, cover plate 1, body of heater 2, thermal insulation layer 3, temperature sensor 4, electrothermal tube 5, control chamber 6, display window 7, switch 8, rack 9, puts thing hole 10.
In Fig. 3-10: A-mesaconitine, B-aconitine, C-hypaconitine, a-Benzoylmesaconine, b-benzoyl aconine, c-benzoyl hypo-aconine.
The specific embodiment
The present invention can specifically implement by the technical scheme illustrating in summary of the invention, be described further, yet scope of the present invention is not limited to following embodiment by following accompanying drawing, embodiment.
Embodiment 1:
In simmering the body of heater of stove processed, be provided with the two cover heating components that distribute up and down, be wherein placed with movably Chinese medicine rack 9.On body of heater side, be fixedly connected with two cover on and off switch 8 and display window 7, control respectively two cover heating components.According to Chinese medicine characteristic and Chinese medicine tradition concocting method or existing legal processing standard, select the suitable process of preparing Chinese medicine to use material as heat transfer medium.The heat transfer medium wherein adding, is mainly process of preparing Chinese medicine material, comprises each kind of plant or mineral grey, sand, rice, Testa Tritici, rice husk, bran coat, Pulvis Talci, Pulvis concha Mactrae etc.Its layout structure is as Fig. 1, mainly by cover plate 1, and body of heater 2, thermal insulation layer 3, temperature sensor 4, electrothermal tube 5, control chamber 6, display window 7, switch 8, rack 9 forms, and between described body of heater 2 body walls, is provided with thermal insulation layer 3, on described rack 9, is evenly provided with and puts thing hole 10.Wherein, need rack 9 to put in stove case before processing, guarantee that its four feets steadily place at body of heater inner bottom part, the upper plane of rack 9 is just in time between two electrothermal tubes 5.Radix Aconiti Lateralis Preparata is placed on to be put on thing hole 10, treats that Radix Aconiti Lateralis Preparata Preparation process is complete, first the stewing Radix Aconiti Lateralis Preparata on hole is taken out, then shifts out rack 9, cleans in time.
The electrothermal tube 5 distributing up and down in body of heater is the heating tubes such as U-shaped, W type, snakelike, screw type or finned, flange form, threaded; The upper and lower distribution distance of two cover heating tubes is 8-50cm.
It is room temperature-300 ℃ that Automatic Temperature Control parameter arranges scope.
Implementation result
[the different Radix Aconiti Lateralis Preparata Comparative Analysis on Qualities of simmering are tested]
1. material and instrument
1.1 instrument Shimadzu LC-10ATvp high performance liquid chromatographs (Shimadzu company); N2000 Data Processing in Chromatography Workstation (Zhejiang University's intelligent information Graduate School of Engineering); The automatic aqua bi-distilling apparatus of BSZ-2 type (Shanghai Botong); ST-400 column oven (Tianjin first Deco instrument company); Ultrasonic cleaner (Kunshan ultrasonic instrument company limited); METTLER-TOLEOD ABS265-S type electronic balance (Switzerland); DHG101-7A electric heating blowing-type drying baker (Gongyi City Ying Yu Yu Hua instrument plant); Tu-1901 type ultraviolet-uisible spectrophotometer (Beijing is general analyses); The accurate AC cleaning regulated device (regulator factory, Shanghai City) of JJW-5KVA; Aconitum carmichaeli is simmered stove processed (self-control).
1.2 material Radix Aconiti Lateralis Preparatas: purchased from You Zhong dam, river Radix Aconiti Lateralis Preparata development in science and technology company limited, through being accredited as the daughter root processed goods of cohosh Aconitum carmichjaelii Debx. Aconitum carmichaeli; Adjuvant: Rhizoma Zingiberis Recens is purchased from food synthetic supermarket; Reference substance: mesaconitine (110799-200404), aconitine (110720-200410), hypaconitine (110798-200404), benzoyl aconine (111794-200901),, Benzoylmesaconine (111795-200901), benzoyl hypo-aconine (111796-200901), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.Reagent except methanol, acetonitrile for HPLC be that chromatographically pure, other are analytical pure.
2. different Radix Aconiti Lateralis Preparatas are simmered the preparation of goods
2.1 adopt traditional method preparation to simmer Radix Aconiti Lateralis Preparata.
Get Radix Aconiti Lateralis Preparata, clean, with clear water, soak and float 7-10 days, change water every day 2-3 times, after going to the greatest extent to salinity, take out, dry.Then evenly tiling is stood in the clean thin bran ash burning, and covers the clean ginger slice of one deck above, 2 toilet paper of flat covering on ginger slice, on paper, repave the clean thin bran ash of one deck, approximately 4-5cm is thick, a small amount of Caulis et Folium Oryzae of tiling, dry bran shell (every Radix Aconiti Lateralis Preparata 100kg, with dry bran 80-100kg) on ash.And then ignite in four angle point fire, after approximately 2-3 days, treat bran cinder ash cooling, take out Radix Aconiti Lateralis Preparata, then steam 8-10 hours.To mouth taste without or micro-while having numb feeling in the tongue, take out, day stand night is vexed cuts vertical thin slice to half-dried, dry in the sun is dry.
Supplementary product consumption: 100 kilograms of every Radix Aconiti Lateralis Preparata, with 12 kilograms, Rhizoma Zingiberis Recens.
2.2 adopt Radix Aconiti Lateralis Preparata to simmer stove preparation processed simmers Radix Aconiti Lateralis Preparata.
(1), get Radix Aconiti Lateralis Preparata, select stepping, in placing container, add water to and flood Radix Aconiti Lateralis Preparata completely, between soak period, change water 2-4 every day, when soaking water at 25 ℃, electrical conductivity is down to below 4000 μ s/cm, takes out, drain the water step (1) make thing;
(2), by step (1) make thing expand operative tip upper, most advanced and sophisticated under, be placed on temperature automatically controlled stewing stove rack processed, cover in the above the clean ginger slice of some layers, the thing that makes by every 100kg step (1) adds 10-12kg Rhizoma Zingiberis Recens, add thin bran ash, to filling, simmer furnace body processed, the heating-up temperature that lower heating component is set is 80-110 ℃, the heating-up temperature of upper heating component is 140-170 ℃, adds fire bending 36-48 hour processed, treats ash cooling, take out Radix Aconiti Lateralis Preparata, obtain the thing that makes of step (2);
(3), the thing that makes of step (2) is placed in heating container, uninterruptedly steam 8-10 hours, to mouth taste without or micro-while having numb feeling in the tongue, take out, airing to room temperature obtains the thing that makes of step (3);
(4), get the thing that makes of step (3), cut the vertical thin slice that 2-3mm is thick, at 60-80 ℃, be dried to water content 6%-12%, obtain;
3. Comparative Analysis on Quality
3.1 diester-type alkaloids content analysis.
3.1.1 the preparation of solution
It is appropriate that the preparation precision of 3.1.1.1 mixing reference substance solution takes mesaconitine, aconitine, hypaconitine reference substance, adds methanol and make every 1 mL respectively containing the mixing reference substance solution of 51.4 μ g, 65.3 μ g, 72.6 μ g, standby.
3.1.1.2 the preparation of need testing solution takes Radix Aconiti Lateralis Preparata coarse powder and Radix Aconiti Lateralis Preparata stewing goods coarse powder approximately 2 g, and precision weighing, puts respectively in 150 mL tool plug conical flasks, add strong aqua ammonia 3 mL moistening 0.5 h, add the close plug of ether 100 mL, placement is spent the night, next day, ultrasonic 15 min, filtered, then filtered with 30 mL ether gradation washing filtering residues, merging filtrate and washing liquid, 40 ℃ of water-baths volatilize, and dissolve with methanol residue is also settled to 2 mL, shakes up, with 0.45 μ m microporous filter membrane, filter before use, standby.
3.1.2 chromatographic condition chromatographic column: Venusil XBP-C
18post (5 μ m, 4.6 * 250mm); Mobile phase: acetonitrile-20 mmolL
-1naH
2pO
4(phosphoric acid is adjusted pH4.0) (50:50) (includes 10 mmolL
-1sodium lauryl sulphate); Flow velocity: 1.0mL/min; Detect wavelength: 235 nm; Column temperature: 35 ℃.
Accurate absorption mixed reference substance solution under 3.1.1 item and each 10 μ L of need testing solution carry out chromatography, records chromatogram.The results are shown in Figure 3-Fig. 6.
3.1.3 accurate absorption mixing reference substance solution 0.5 mL, 1 mL, 2 mL, 4 mL, 8 mL, 10 mL put in 10 mL measuring bottles respectively in linear relationship investigation, add methanol and be diluted to scale, shake up, respectively the accurate 20 μ L that draw, injection liquid chromatography, measures successively.With sample size X(μ g) peak area A is carried out to linear regression, regression equation is respectively: mesaconitine:
a=371 603
x+ 590.59,
r=0.9 993; Aconitine:
a=351 702
x– 2283.2,
r=0.9 997; Hypaconitine:
a=409 988
x+ 914.24,
r=0.9 994.Known mesaconitine is good linear relation at 0.032-0.642 μ g, aconitine at 0.0 408-0.816 μ g, hypaconitine peak area and sample size within the scope of 0.0454-0.908 μ g.
3.1.4 precision test is drawn the mixing reference substance solution 10 μ L of same concentration, repeats sample introduction and measures 5 times, records chromatogram, and the RSD of result mesaconitine, aconitine, hypaconitine peak area is respectively 0.89%, 0.10%, 0.85%.
3.1.5 stability test precision takes Traditional Method stewing Radix Aconiti Lateralis Preparata sample 2 g of Jianchang side, press 3.1.1.2 item below legal system available test sample solution, difference sampling and measuring after room temperature is placed 0 h, 2 h, 4 h, 8 h and 24 h, the RSD of result mesaconitine, aconitine, hypaconitine peak area is respectively 1.49%, 1.69%, 2.48%, shows that need testing solution is stable in 24 h.
3.1.6 replica test precision takes 5 parts of Traditional Method stewing Radix Aconiti Lateralis Preparata sample 2 g of Jianchang side, by 3.1.1.2 item below legal system available test sample solution, measure in accordance with the law, the mass fraction of mesaconitine, aconitine, hypaconitine in results sample (
ω b) be respectively 6.05 μ gg
-1, 37.23 μ gg
-1, 3.72 μ gg
-1, RSD is respectively 2.03%, 2.75%, 2.16%.
3.1.7 the accurate Jianchang side Traditional Method that takes 6 parts of known content of average recovery test is simmered Radix Aconiti Lateralis Preparata sample 1 g, every part respectively precision add reference substance solution mesaconitine 100 μ L, aconitine 500 μ L, hypaconitine 50 μ L, press 3.1.1.2 item below legal system available test sample solution, measure in accordance with the law.Result mesaconitine, aconitine, hypaconitine average recovery rate are respectively: 95.28%, RSD2.38%; 96.15%, RSD1.89%; 95.31%, RSD2.44%.
3.1.8 sample size is measured accurate Radix Aconiti Lateralis Preparata and the 2 kinds of stewing Radix Aconiti Lateralis Preparata race goods prepared by different concocting methods of taking respectively, by 3.1.1.2 item below legal system available test sample solution.Accurate absorption mixed reference substance solution and each 10 μ L of need testing solution, and injection liquid chromatography, records chromatogram.By external standard method, with the mass fraction of mesaconitine (mesaaconitine), aconitine (aconitine), hypaconitine (hypaaconitine) in calculated by peak area sample (
ω b).The results are shown in Table 1.
3 kinds of diester-type alkaloids assay results in table 1 sample (
￣ X±
s)
Note: "/" cannot integration.
According to stipulating under 2010 editions Radix Aconiti Lateralis Preparata items of < < Chinese Pharmacopoeia > >, Radix Aconiti Lateralis Preparata contains diester-type alkaloids with mesaconitine (C
33h
45nO
11), hypaconitine (C
33h
45nO
10) and aconitine (C
34h
47nO
11) total amount meter, must not cross 0.020%.As shown in Table 1, in 2 kinds of stewing Radix Aconiti Lateralis Preparata processed products, diester-type alkaloids content is close, and all lower than statutory standards, wherein the standard deviation of traditional method stewing Radix Aconiti Lateralis Preparata content is large.
3.2 monoester alkaloid content analyses.
3.2.1 the preparation of solution
3.2.1.1 the preparation of reference substance solution
It is appropriate that precision takes Benzoylmesaconine, benzoyl aconine, benzoyl hypo-aconine reference substance, adds mobile phase and make every 1ml respectively containing the mixed solution of 48.40 μ g, 99.8 μ g, 99.5 μ g, obtains.
3.2.1.2 the preparation of need testing solution
Get respectively Radix Aconiti Lateralis Preparata and each Radix Aconiti Lateralis Preparata and simmer the about 3g of goods powder (crossing sieve No. three), accurately weighed, put in tool plug conical flask, add ammonia solution 3ml, precision adds the weighed weight supersound process of isopropyl alcohol-ethyl acetate (1:1) mixed solution 50ml(), at water temperature ultrasonic 30min below 25 ℃, let cool, weighed weight again, with isopropyl alcohol-ethyl acetate (1:1) mixed solution, supply the weight of less loss, shake up, filter, precision measures subsequent filtrate 25ml, 40 ℃ of following decompression and solvent recoveries are to dry, residue precision adds isopropyl alcohol-dichloromethane (1:1) mixed solution 3ml to dissolve, filter, get subsequent filtrate, obtain.
3.2.2 chromatographic condition chromatographic column: Venusil XBP-C18 post (5 μ m, 4.6 * 250mm); Mobile phase: acetonitrile-20 mmolL
-1naH
2pO
4(triethylamine is adjusted pH6.5) (47:53) (includes 10 mmolL
-1sodium lauryl sulphate); Flow velocity: 1.0ml/min; Detect wavelength: 235nm; Column temperature: 35 ℃.
According to appendix high performance liquid chromatography of < < Chinese Pharmacopoeia > > version in 2010 (appendix VI D), measure.Precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.The results are shown in Figure 7-Figure 10.
3.2.3 linear relationship is investigated accurate absorption respectively and is mixed reference substance solution 1 mL, 2 mL, 4 mL, 8 mL, 10 mL and put in 10 mL measuring bottles, adds methanol and is diluted to scale, shake up, and accurate 10 μ L that draw respectively, injection liquid chromatography, measures successively.With sample size X(μ g) peak area A is carried out to linear regression, regression equation is respectively: benzoyl mesaconitine:
a=843 288
x+ 920.65,
r=0.9 999; Benzoyl aconite alkali:
a=713 106
x+ 237.35,
r=0.9 999; Benzoylhypaconitine:
a=763 932
x+ 6087.1,
r=0.9 999.Known benzoyl mesaconitine is good linear relation at 0.061-0.605 μ g, benzoyl aconite alkali at 0.124-1.244 μ g, benzoylhypaconitine peak area and sample size within the scope of 0.125-1.248 μ g.
3.2.4 precision test is drawn the mixing reference substance solution 10 μ L of same concentration, repeating sample introduction measures 6 times, record chromatogram, the RSD of result benzoyl mesaconitine, benzoyl aconite alkali, benzoylhypaconitine peak area is respectively 1.03%, 0.69%, 1.34%.
3.2.5 stability test precision takes Traditional Method stewing Radix Aconiti Lateralis Preparata sample 3g, press 3.2.1.2 item below legal system available test sample solution, difference sampling and measuring after room temperature is placed 0 h, 2 h, 4 h, 8 h and 24 h, the RSD of result benzoyl mesaconitine, benzoyl aconite alkali, benzoylhypaconitine peak area is respectively 2.09%, 1.88%, 2.27%, shows that need testing solution is stable in 24 h.
3.2.6 replica test precision takes 5 parts of Traditional Method stewing Radix Aconiti Lateralis Preparata sample 3g, by 3.2.1.2 item below legal system available test sample solution, measure in accordance with the law, the mass fraction of benzoyl mesaconitine, benzoyl aconite alkali, benzoylhypaconitine in results sample (
ω b) be respectively 5.85 μ gg
-1, 24.04 μ gg
-1, 87.57 μ gg
-1, RSD is respectively 1.92%, 2.17%, 2.08%.
3.2.7 the accurate Traditional Method that takes 6 parts of known content of average recovery test is simmered Radix Aconiti Lateralis Preparata sample 1.5 g, every part respectively precision add reference substance solution benzoyl mesaconitine 50 μ L, benzoyl aconite alkali 200 μ L, benzoylhypaconitine 1mL, press 3.2.1.2 item below legal system available test sample solution, measure in accordance with the law.The new benzoyl aconite alkali of result, benzoyl aconite alkali, benzoylhypaconitine average recovery rate are respectively: 96.26%, RSD2.58%; 98.03%, RSD2.44%; 99.65%, RSD2.15%.
3.2.8 sample size measurement result is in Table 2.
Monoester alkaloid content measurement result in table 2 sample (
)
Note: "/" is cannot integration.
According to stipulating under 2010 editions Radix Aconiti Lateralis Preparata items of < < Chinese Pharmacopoeia > >, by dry product, to calculate, this product is containing Benzoylmesaconine (C
31h
43nO
10), benzoyl aconine (C
32h
45nO
10) and benzoyl hypo-aconine (C
31h
43nO
9) total amount, must not be less than 0.010%.This is tested, and to take containing Benzoylmesaconine, benzoyl aconine, benzoyl hypo-aconine be contrast, in Radix Aconiti Lateralis Preparata, content is lower, and can reach standards of pharmacopoeia after adopting simmer method to concoct, the content of the Radix Aconiti Lateralis Preparata that wherein traditional method and Radix Aconiti Lateralis Preparata stewing stove processed are concocted all can meet standards of pharmacopoeia, but adopts the Radix Aconiti Lateralis Preparata content data fluctuation of traditional method large.
4. brief summary
The standard that the technological parameter of two kinds of concocting methods all selects side tradition in Jianchang to simmer Radix Aconiti Lateralis Preparata, by experimental result, several zero differences of stewing Radix Aconiti Lateralis Preparata quality prepared by the method that adopts traditional method and Radix Aconiti Lateralis Preparata to simmer stove processed, the stewing Radix Aconiti Lateralis Preparata that adopts stewing stove processed to prepare can reach the quality standard that Radix Aconiti Lateralis Preparata is simmered by Jianchang side.
Claims (10)
1. the prepared slices of Chinese crude drugs are simmered an industrialization processing procedure for Radix Aconiti Lateralis Preparata, it is characterized in that concocting method is as follows:
(1), get Radix Aconiti Lateralis Preparata, select stepping, in placing container, add water to and flood Radix Aconiti Lateralis Preparata completely, between soak period, change water 2-4 every day, and when soaking water at 25 ℃, electrical conductivity is down to 6000 μ s/cm when following, below preferably to 4000 μ s/cm, take out, drain the water step (1) make thing;
(2), by step (1) make thing expand operative tip upper, most advanced and sophisticated under, be placed on temperature automatically controlled stewing stove rack processed, cover in the above the clean ginger slice of some layers, the thing that makes by every 100kg step (1) adds 8-16kg Rhizoma Zingiberis Recens, preferred 10-12kg, add thin bran ash, to filling, simmer furnace body processed, the heating-up temperature that lower heating component is set is 70-130 ℃, preferred 80-110 ℃, the heating-up temperature of upper heating component is 110-180 ℃, preferred 140-170 ℃, add fire bending system 24-48 hours, preferred 36-48 hour, treat ash cooling, take out Radix Aconiti Lateralis Preparata, obtain the thing that makes of step (2),
(3), the thing that makes of step (2) is placed in heating container, uninterruptedly steam 6-12 hours, preferably 8-10 hours, to mouth taste without or micro-while having numb feeling in the tongue, take out, airing to room temperature obtains the thing that makes of step (3);
(4), get the thing that makes of step (3), cut the vertical thin slice that 1-4mm is thick, preferably 2-3mm, is dried to water content 5%-13% at 60-80 ℃, preferred water content 6%-12%, obtains;
It comprises cover plate 1, body of heater 2 and heating system described temperature automatically controlled stewing stove processed, on described body of heater 2 is interior, have heating component, each heating component comprises heating part and temperature sensing part, the control circuit of heating component and control chamber 6 connects to form heating system, and each heating component has independently temperature control unit, and control chamber 6 is arranged on the outside of body of heater 2, in body of heater 2, be provided with rack 9, rack 9 put the thing scope of operation between each heating component, simmer when processed, in body of heater 2, be provided with heat transfer medium.
2. a kind of prepared slices of Chinese crude drugs according to claim 1 are simmered the industrialization processing procedure of Radix Aconiti Lateralis Preparata, it is characterized in that: in step (1), when soaking water at 25 ℃, electrical conductivity is down to 4000 μ s/cm when following, takes out; The heating-up temperature that lower heating component is set in step (2) is 80-110 ℃, and the heating-up temperature of upper heating component is 140-170 ℃.
3. a temperature automatically controlled stewing stove processed, it comprises cover plate 1, body of heater 2 and heating system, it is characterized in that: the interior upper and lower and/or left and right of described body of heater 2 is provided with heating component, each heating component comprises heating part and temperature sensing part, the control circuit of heating component and control chamber 6 connects to form heating system, each heating component has independently temperature control unit, control chamber 6 is arranged on the outside of body of heater 2, in body of heater 2, be provided with rack 9, rack 9 put the thing scope of operation between each heating component, simmer when processed, in body of heater 2, be provided with heat transfer medium.
4. a kind of temperature automatically controlled stewing according to claim 3 stove processed, is characterized in that: on described body of heater 2 inwalls, have and be respectively provided with a set of heating component, the thing scope of operation of putting of rack 9 is overlapped between the heating part of heating components upper and lower two.
5. a kind of temperature automatically controlled stewing according to claim 3 stove processed, is characterized in that: between the heating part of upper and lower two cover heating components, upper and lower spacing distance is 8-50cm.
6. according to a kind of temperature automatically controlled stewing stove processed described in 3-5 arbitrary claim, it is characterized in that: the heating part of described heating component is electrothermal tube 5, the temperature sensing of described heating component is partly temperature sensor 4; Temperature sensor 4 and electrothermal tube 5 form a heating component independently, and independently heating component is connected with the independently temperature control unit circuit of control chamber 6.
7. a kind of temperature automatically controlled stewing according to claim 6 stove processed, is characterized in that: described electrothermal tube 5 is U-shaped, W type, snakelike, screw type heating tube or finned, flange form, threaded heating tube.
8. according to a kind of temperature automatically controlled stewing stove processed described in 3-5 arbitrary claim, it is characterized in that: the heating part of described heating component is electrothermal tube 5, electrothermal tube 5 is U-shaped, W type, snakelike, screw type heating tube or finned, flange form, threaded heating tube.
9. according to a kind of temperature automatically controlled stewing stove processed described in 3-5 arbitrary claim, it is characterized in that: described heat transfer medium comprises each kind of plant or mineral grey, sand, rice, Testa Tritici, rice husk, bran coat, Pulvis Talci and Pulvis concha Mactrae.
10. according to a kind of temperature automatically controlled stewing stove processed described in 1-3 arbitrary claim, it is characterized in that: it is room temperature-300 ℃ that the temperature control parameter of stewing stove processed arranges scope.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105534712A (en) * | 2015-12-11 | 2016-05-04 | 江西中医药高等专科学校 | Industrialized processing technology of traditional Chinese medicine decoction pieces simmering fresh ginger |
| CN105560058A (en) * | 2015-12-11 | 2016-05-11 | 江西中医药高等专科学校 | Industrial processing technology of roasted radix aucklandiae in form of Chinese medicinal decoction pieces |
| CN110658236A (en) * | 2019-10-24 | 2020-01-07 | 华润三九（雅安）药业有限公司 | Heishun tablet processing process Ca2+Content monitoring method and rinsing end point judging method |
| CN112891407A (en) * | 2021-03-31 | 2021-06-04 | 建昌帮药业有限公司 | Stewed aconite tablet and preparation method thereof |
| CN113092655A (en) * | 2021-04-12 | 2021-07-09 | 长春中医药大学 | Method for detecting effective components in aconite decoction by high performance liquid chromatography |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2131519Y (en) * | 1992-08-08 | 1993-05-05 | 天津市北方工业炉联合开发服务部 | Electric flatening oven for chinese traditional herb medicine |
| CN2147861Y (en) * | 1993-01-20 | 1993-12-01 | 刘延林 | Multifunctional traditional Chinese medicine preparing machine |
| CN2537385Y (en) * | 2002-04-16 | 2003-02-26 | 程桂俊 | Automatic regulating and preparing Chinese medicine furnace |
| CN101390963A (en) * | 2007-09-17 | 2009-03-25 | 廖德宏 | Process method of aconite |
| CN101485746A (en) * | 2008-12-19 | 2009-07-22 | 杭州惠远实业有限公司 | Method for processing Chinese medicine aconite |
| CN201627740U (en) * | 2009-12-15 | 2010-11-10 | 贺贵全 | Cooling fan |
| CN203539701U (en) * | 2013-09-22 | 2014-04-16 | 江西中医药高等专科学校 | Automatic-temperature-control traditional-Chinese-medicine decocting stove |
-
2013
- 2013-09-22 CN CN201310431357.0A patent/CN103585017B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2131519Y (en) * | 1992-08-08 | 1993-05-05 | 天津市北方工业炉联合开发服务部 | Electric flatening oven for chinese traditional herb medicine |
| CN2147861Y (en) * | 1993-01-20 | 1993-12-01 | 刘延林 | Multifunctional traditional Chinese medicine preparing machine |
| CN2537385Y (en) * | 2002-04-16 | 2003-02-26 | 程桂俊 | Automatic regulating and preparing Chinese medicine furnace |
| CN101390963A (en) * | 2007-09-17 | 2009-03-25 | 廖德宏 | Process method of aconite |
| CN101485746A (en) * | 2008-12-19 | 2009-07-22 | 杭州惠远实业有限公司 | Method for processing Chinese medicine aconite |
| CN201627740U (en) * | 2009-12-15 | 2010-11-10 | 贺贵全 | Cooling fan |
| CN203539701U (en) * | 2013-09-22 | 2014-04-16 | 江西中医药高等专科学校 | Automatic-temperature-control traditional-Chinese-medicine decocting stove |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105534712A (en) * | 2015-12-11 | 2016-05-04 | 江西中医药高等专科学校 | Industrialized processing technology of traditional Chinese medicine decoction pieces simmering fresh ginger |
| CN105560058A (en) * | 2015-12-11 | 2016-05-11 | 江西中医药高等专科学校 | Industrial processing technology of roasted radix aucklandiae in form of Chinese medicinal decoction pieces |
| CN110658236A (en) * | 2019-10-24 | 2020-01-07 | 华润三九（雅安）药业有限公司 | Heishun tablet processing process Ca2+Content monitoring method and rinsing end point judging method |
| CN112891407A (en) * | 2021-03-31 | 2021-06-04 | 建昌帮药业有限公司 | Stewed aconite tablet and preparation method thereof |
| CN113092655A (en) * | 2021-04-12 | 2021-07-09 | 长春中医药大学 | Method for detecting effective components in aconite decoction by high performance liquid chromatography |
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