CN103585017B - 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 the Preparation process equipment of simmering Chinese medicine processed, be specifically related to a kind of prepared slices of Chinese crude drugs and simmer the industrialization processing procedure of monkshood and temperature automatically controlled stewing stove, be mainly used in the production and processing that monkshood simmered by Chinese medicine.
Background technology
Stewing method is the concocting method often used in Chinese medicine preparation, is directly or with wetted surface, l Water Paper to be wrapped up by medicine, is embedded in showing tremendous enthusiasm ash, or talcum powder, or the concocting method of slowly heating in wheat bran is called stewing method.Its object mainly reduces toxic and side effect, or relaxes the property of medicine, or strengthens drug effect.As simmered monkshood, simmering nutmeg, roasted RADIX PUERARIAE, roasted RADIX AUCKLANDIAE, roasted FRUCTUS CHEBULAE etc.But, owing to still adopting Conventional wisdom method when simmering system processing medicinal material, it concocts the duration and degree of heating and the time is not easily grasped, simmer technological parameter processed to be difficult to quantize, easily burn, burn out medicinal material, do not meet current Good and produce GMP requirement, be difficult to realize industrialized production, cause stewing method to be on the verge of in modern Chinese herbal medicine processing technique lost.As simmered RADIX ACONITI LATERALIS PREPARATA, 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 to deficiency of yang fire and waits disease to have the original merit of returning sun benefit fire.But producing because of it still needs the experience of pharmaceutical worker to control with quality control, be difficult to meet modern CMM processing piece and produce the requirement with clinical practice, cause simmering goods without manufacturer production monkshood, this method is in condition in imminent danger.According to Chinese Academy of Social Sciences's traditional Chinese medicine national conditions investigation, traditional 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 traditional Chinese medicine succession [N]. Chinese traditional Chinese medicine report, 2012-2-13 (3)]. therefore, the modernization stewing control equipment that exploitation has temperature automatic control is that monkshood is simmered in production and other simmer a Chinese medicine processed difficult problem urgently to be resolved hurrily, simmers method processing technique have important practice significance to Inheritance＆ development traditional Chinese medicine.
Summary of the invention
The object of the invention is to design a kind of prepared slices of Chinese crude drugs and simmer the industrialization processing procedure of monkshood and temperature automatically controlled stewing stove, with process of preparing Chinese medicine materials such as each Plants or mineral grey, sand, rice, wheat bran, husk, cavings, talcum powder, clam meal for heat transfer medium, be mainly used in the Preparation process simmering monkshood, there is parameter controllable precise, 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 medicines such as nutmeg, the root of kudzu vine, the banksia rose, myrobalan.
One of technical scheme of the present invention: the industrialization processing procedure that monkshood simmered by a kind of prepared slices of Chinese crude drugs is as follows:
(1), get salted aconite root, select stepping, in placing container, add water to and flood salted aconite root completely, between soak period, every day changes water 2-4 time, when in time soaking water at 25 DEG C, electrical conductivity is down to 6000 below μ s/cm, preferably to 4000 below μ s/cm, takes out, and drain the water to obtain the obtained thing of step (1);
(2), by the enlargement top of the obtained thing of step (1) upper, most advanced and sophisticated under, be placed on temperature automatically controlled stewing stove rack processed, cover the clean ginger slice of some layers in the above, 8-16kg ginger is added by the obtained thing of every 100kg step (1), preferably 10-12kg, add thin chaff ash, furnace body processed is simmered to filling, the heating-up temperature arranging lower heating component is 70-130 DEG C, preferred 80-110 DEG C, the heating-up temperature of upper heating component is 110-180 DEG C, preferred 140-170 DEG C, add fire bending system 24-48 hours, preferred 36-48 hour, treat ash cooling, take out monkshood, obtain the obtained thing of step (2),
(3), the obtained thing of step (2) is placed in heating container, uninterruptedly steams 6-12 hours, preferably 8-10 hours, to mouth taste without or micro-have a numb feeling in the tongue time, take out, airing to room temperature obtains the obtained thing of step (3);
(4), get the obtained thing of step (3), cut the vertical thin slice that 1-4mm is thick, preferred 2-3mm, is dried to water content 5%-13% at 60-80 DEG C, and preferred water content 6%-12% to obtain final product;
Technical scheme two 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, in described body of heater 2 up and down and/or left and right be provided with heating component, each heating component comprises heating part and temperature sensing portion, the control circuit of heating component and control cabinet 6 connects to form heating system, each heating component has independently temperature control unit, control cabinet 6 is arranged on the outside of body of heater 2, rack 9 is provided with in body of heater 2, rack 9 put the thing scope of operation between each heating component, when simmering processed, in body of heater 2, be provided with heat transfer medium.
Preferred: described body of heater 2 inwall to have and is 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, spacing distance is 8-50cm up and down.
Further preferably: the heating part of described heating component is electrothermal tube 5, and the temperature sensing portion of described heating component is temperature sensor 4; A temperature sensor 4 and electrothermal tube 5 form an independently heating component, and independently heating component is connected with the independently temperature control unit circuit of control cabinet 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 Plants or mineral grey, sand, rice, wheat bran, husk, cavings, talcum powder and clam meal.
It is room temperature-300 DEG C that the temperature control parameter simmering stove processed arranges scope.
Thermal insulation layer 3 is provided with between described body of heater 2 body wall.
Described rack 9 is evenly provided with and puts thing hole 10.
Using method: by unprocessed Radix Aconiti Lateralis or salted aconite root with top or unified upward with tip, is placed in respectively and has 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 CMM processing piece, select suitable heat transfer medium, add and simmer in stove processed, and covering unprocessed Radix Aconiti Lateralis or salted aconite root completely.Process characteristic processed is simmered according to monkshood, depend on sub-top different from tip, arrange up and down and/or the heating-up temperature of the heating component of left and right distribution respectively, heating component temperature wherein near side, monkshood top is arranged need higher than its most advanced and sophisticated side, open temp control unit simultaneously, to the concocted time of regulation, take out medicinal material.
Advantage of the present invention:
(1) production environment adapts to GMP requirement.Conventional method cavings is fuel, and greatly, production environment is severe, and cannot meet the clean requirement of GMP to pharmaceutical production environment, conventional method is on the verge of lost for smog and dust.The thermal source of temperature automatically controlled stewing stove processed adopts electrothermal, and production environment is airtight, and produce smog and dust hardly, production environment can meet GMP requirement, for simmering monkshood production regularization, industrialization establish a firm foundation.
(2) processing parameter controls.The technological parameter of conventional method depends on the experience of operating personnel, obviously random, especially firepower size during cavings burning cannot be grasped, the little then monkshood difficulty of fire is simmered thoroughly, the too large then easy carbonization of monkshood 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 monkshood and simmer stewing monkshood prepared by stove processed.Temperature automatically controlled stewing stove processed by upper and lower two can accurate temperature controlling heating tube heat, the processing parameter such as firepower, time is accurately controlled, and product difference between batch obviously reduces, and easily meets GMP production requirement.
(3) labour intensity significantly reduces.Adopt conventional method to need a few individual to supervise stewing process in turn, need pay close attention to the change of firepower, add cavings in time, because the stewing time of simmering RADIX ACONITI LATERALIS PREPARATA is 48 hours, so the production process monitoring in night be unable to do without people, labour intensity is large.Along with the rising gradually of human cost, the production cost simmering monkshood increases, and has a strong impact on economic benefit.And temperature automatically controlled stewing stove processed adopts temperature automatically controlled, only need people watch-dog ruuning situation at any time, labour intensity is little, and human cost significantly reduces, and production cost declines.
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 that the embodiment of the present invention 1 diester-type alkaloids reference substance HPLC schemes.
Fig. 4 is that the embodiment of the present invention 1 salted aconite root diester-type alkaloids HPLC schemes.
Fig. 5 is that the stewing RADIX ACONITI LATERALIS PREPARATA diester-type alkaloids HPLC of the embodiment of the present invention 1 Jianchang side conventional method schemes.
Fig. 6 is that the stewing RADIX ACONITI LATERALIS PREPARATA diester-type alkaloids HPLC of the embodiment of the present invention 1 Aconitum carmichaeli stewing stove processed schemes.
Fig. 7 is that the embodiment of the present invention 1 monoester alkaloid reference substance HPLC schemes.
Fig. 8 is that the embodiment of the present invention 1 salted aconite root monoester alkaloid HPLC schemes.
Fig. 9 is that the stewing RADIX ACONITI LATERALIS PREPARATA monoester alkaloid HPLC of the embodiment of the present invention 1 Aconitum carmichaeli stewing stove processed schemes.
Figure 10 is that the stewing RADIX ACONITI LATERALIS PREPARATA monoester alkaloid HPLC of the embodiment of the present invention 1 Jianchang side conventional method schemes.
In Fig. 1-2, cover plate 1, body of heater 2, thermal insulation layer 3, temperature sensor 4, electrothermal tube 5, control cabinet 6, display window 7, switch 8, rack 9, puts thing hole 10.
In Fig. 3-10: A-mesaconine, B-aconitine, C-Hypaconitine, a-benzoylmesaconine, b-benzoyl aconine, c-benzoyl time aconine.
Detailed description of the invention
The present invention specifically can be implemented by the technical scheme illustrated in summary of the invention, is described further by following accompanying drawing, embodiment, but scope of the present invention is not limited to following embodiment.
Embodiment 1:
In the body of heater simmering stove processed, be provided with the two cover heating components distributed up and down, be wherein placed with moveable Chinese medicine rack 9.Be fixedly connected with two cover power switches 8 and display window 7 on body of heater side, control two cover heating components respectively.According to Chinese medicine characteristic and Chinese medicine tradition concocting method or existing legal processing standard, select suitable process of preparing Chinese medicine material as heat transfer medium.The heat transfer medium wherein added, mainly process of preparing Chinese medicine material, comprise each Plants or mineral grey, sand, rice, wheat bran, husk, cavings, talcum powder, clam meal etc.Its layout structure is as Fig. 1, and primarily of cover plate 1, body of heater 2, thermal insulation layer 3, temperature sensor 4, electrothermal tube 5, control cabinet 6, display window 7, switch 8, rack 9 forms, and is provided with thermal insulation layer 3 between described body of heater 2 body wall, described rack 9 is evenly provided with and puts thing hole 10.Wherein, need rack 9 to put in stove case before processing, ensure that its four feets are steadily placed at body of heater inner bottom part, the upper plane of rack 9 is just in time between two electrothermal tubes 5.Monkshood is placed on to be put on thing hole 10, treats that monkshood Preparation process is complete, is first taken out by the stewing monkshood on hole, then shifts out rack 9, clean in time.
The heating tubes such as the electrothermal tube 5 distributed up and down in body of heater is 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.
Automatic Temperature Control optimum configurations scope is room temperature-300 DEG C.
Implementation result
[different RADIX ACONITI LATERALIS PREPARATA Comparative Analysis on Quality of simmering is tested]
1. material and instrument
1.1 instrument Shimadzu LC-10ATvp high performance liquid chromatographs (Shimadzu Corporation); 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 Co., Ltd); METTLER-TOLEOD ABS265-S type electronic balance (Switzerland); DHG101-7A electric heating blowing-type drying box (Ying Yu Yu Hua instrument plant of Gongyi City); Tu-1901 type ultraviolet-uisible spectrophotometer (Beijing is general analyses); Accurate AC cleaning regulated device (Shanghai City regulator factory) of JJW-5KVA; Aconitum carmichaeli simmers stove processed (self-control).
1.2 material monkshoods: purchased from You Zhong dam, river monkshood development in science and technology Co., Ltd, through being accredited as the sub-root processed goods of cohosh rhizome of Chinese monkshood Aconitum carmichaeli; Auxiliary material: ginger is purchased from food synthetic supermarket; Reference substance: mesaconine (110799-200404), aconitine (110720-200410), Hypaconitine (110798-200404), benzoyl aconine (111794-200901), benzoylmesaconine (111795-200901), benzoyl time aconine (111796-200901), purchased from Nat'l Pharmaceutical & Biological Products Control Institute.Reagent except HPLC methyl alcohol, acetonitrile be except chromatographically pure, other be analyze pure.
2. the preparation of goods simmered by different monkshood
2.1 adopt conventional method preparation to simmer monkshood.
Get salted aconite root, clean, with clear water leaching drift 7-10 days, change water every day 2-3 times, go to the greatest extent to salinity, take out, dry.Then evenly tiling is stood in the thin chaff ash totally burnt, and covers the clean ginger slice of one deck above, flat covering 2 toilet paper on ginger slice, paper repaves the clean thin chaff ash of one deck, about 4-5cm is thick, and ash tiles a small amount of straw, dry chaff shell (every salted aconite root 100kg, with dry chaff 80-100kg).And then in corner, igniting is ignited, and after about 2-3 days, treats chaff cinder ash cooling, takes out monkshood, then steams 8-10 hours.To mouth taste without or micro-have a numb feeling in the tongue time, take out, stand night day is vexed cuts vertical thin slice to half-dried, and airing is done.
Supplementary product consumption: every salted aconite root 100 kilograms, with 12 kilograms, ginger.
2.2 adopt monkshood to simmer stove processed preparation simmers monkshood.
(1), get salted aconite root, select stepping, in placing container, add water to and flood salted aconite root completely, between soak period, every day changes water 2-4 time, and in time soaking water at 25 DEG C, electrical conductivity is down to 4000 below μ s/cm, takes out, and drain the water to obtain the obtained thing of step (1);
(2), by the enlargement top of the obtained thing of step (1) upper, most advanced and sophisticated under, be placed on temperature automatically controlled stewing stove rack processed, cover the clean ginger slice of some layers in the above, 10-12kg ginger is added by the obtained thing of every 100kg step (1), add thin chaff ash, furnace body processed is simmered to filling, the heating-up temperature arranging lower heating component is 80-110 DEG C, the heating-up temperature of upper heating component is 140-170 DEG C, adds fire bending 36-48 hour, treats ash cooling, take out monkshood, obtain the obtained thing of step (2);
(3), the obtained thing of step (2) is placed in heating container, uninterruptedly steams 8-10 hours, to mouth taste without or micro-have a numb feeling in the tongue time, take out, airing to room temperature obtains the obtained thing of step (3);
(4), get the obtained thing of step (3), cut the vertical thin slice that 2-3mm is thick, be dried to water content 6%-12% at 60-80 DEG C, obtain final product;
3. Comparative Analysis on Quality
3.1 diester-type alkaloids content analysis.
3.1.1 the preparation of solution
3.1.1.1 the preparation precision mixing reference substance solution takes mesaconine, aconitine, Hypaconitine reference substance in right amount, adds methyl alcohol and makes every 1 mL respectively containing the mixing reference substance solution of 51.4 μ g, 65.3 μ g, 72.6 μ g, for subsequent use.
3.1.1.2 the preparation of need testing solution takes salted aconite root meal and monkshood stewing goods meal about 2 g, and precision weighing, puts in 150 mL tool plug conical flasks respectively, add wetting 0.5 h of concentrated ammonia liquor 3 mL, 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 filter residues, merging filtrate and washing lotion, 40 DEG C of water-baths volatilize, and methyl alcohol dissolved residue is also settled to 2 mL, shakes up, filter with 0.45 μm of miillpore filter before use, for subsequent use.
3.1.2 chromatographic condition chromatographic column: Venusil XBP-C
18post (5 μm, 4.6 × 250mm); Mobile phase: acetonitrile-20 mmolL
-1naH
2pO
4(phosphoric acid adjusts pH4.0) (50:50) (includes 10 mmolL
-1lauryl sodium sulfate); Flow velocity: 1.0mL/min; Determined wavelength: 235 nm; Column temperature: 35 DEG C.
Precision mixes reference substance solution under drawing 3.1.1 item and each 10 μ L of need testing solution carry out chromatography, record 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 dilution to scale, shake up, respectively accurate absorption 20 μ L, injection liquid chromatography successively, measures.With sample size X(μ g) linear regression is carried out to peak area A, regression equation is respectively: mesaconine:
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 mesaconine 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 draws the mixing reference substance solution 10 μ L of same concentration, repeats sample introduction and measures 5 times, and record chromatogram, the RSD of result mesaconine, aconitine, Hypaconitine peak area is respectively 0.89%, 0.10%, 0.85%.
3.1.5 stability test precision takes Jianchang side Traditional Method stewing monkshood sample 2 g, by legal system available test sample solution below 3.1.1.2 item, difference sampling and measuring after room temperature places 0 h, 2 h, 4 h, 8 h and 24 h, the RSD of result mesaconine, 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 Jianchang side Traditional Method and simmers monkshood sample 2 g 5 parts, by legal system available test sample solution below 3.1.1.2 item, measures in accordance with the law, in results sample mesaconine, aconitine, Hypaconitine mass fraction (
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 taking 6 parts of known content of average recovery test simmers monkshood sample 1 g, every part respectively precision add reference substance solution mesaconine 100 μ L, aconitine 500 μ L, Hypaconitine 50 μ L, by legal system available test sample solution below 3.1.1.2 item, measure in accordance with the law.Result mesaconine, aconitine, Hypaconitine average recovery rate are respectively: 95.28%, RSD2.38%; 96.15%, RSD1.89%; 95.31%, RSD2.44%.
3.1.8 sample size measures and accurately respectively takes stewing monkshood prepared by salted aconite root and 2 kinds of different concocting methods and run goods, by legal system available test sample solution below 3.1.1.2 item.Accurate absorption mixes reference substance solution and each 10 μ L of need testing solution, injection liquid chromatography, record chromatogram.By external standard method, with the mass fraction of mesaconine (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.
Specify according under " Chinese Pharmacopoeia " 2010 editions monkshood items, tag contains diester-type alkaloids with mesaconine (C
33h
45nO
11), Hypaconitine (C
33h
45nO
10) and aconitine (C
34h
47nO
11) total amount, must not 0.020% be crossed.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 conventional 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
Precision takes benzoylmesaconine, benzoyl aconine, benzoyl time aconine reference substance in right amount, adds mobile phase and makes every 1ml respectively containing the mixed solution of 48.40 μ g, 99.8 μ g, 99.5 μ g, to obtain final product.
3.2.1.2 the preparation of need testing solution
Get salted aconite root and each monkshood stewing goods powder (crossing No. three sieves) about 3g respectively, accurately weighed, put in tool plug conical flask, add ammonia solution 3ml, precision adds the ultrasonic process of the weighed weight of isopropyl alcohol-ethyl acetate (1:1) mixed solution 50ml(), at water temperature less than 25 DEG C ultrasonic 30min, let cool, weighed weight again, the weight of less loss is supplied with isopropyl alcohol-ethyl acetate (1:1) mixed solution, shake up, filter, precision measures subsequent filtrate 25ml, less than 40 DEG C decompression and solvent recoveries are to dry, residue precision adds isopropyl alcohol-carrene (1:1) mixed solution 3ml and dissolves, filter, get subsequent filtrate, obtain.
3.2.2 chromatographic condition chromatographic column: Venusil XBP-C18 post (5 μm, 4.6 × 250mm); Mobile phase: acetonitrile-20 mmolL
-1naH
2pO
4(pH6.5 adjusted by triethylamine) (47:53) (includes 10 mmolL
-1lauryl sodium sulfate); Flow velocity: 1.0ml/min; Determined wavelength: 235nm; Column temperature: 35 DEG C.
Measure according to " Chinese Pharmacopoeia " version in 2010 annex high performance liquid chromatography (annex VI D).Accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.The results are shown in Figure 7-Figure 10.
3.2.3 linear relationship is investigated and is accurately respectively drawn mixing reference substance solution 1 mL, 2 mL, 4 mL, 8 mL, 10 mL put in 10 mL measuring bottles, adds methanol dilution to scale, shakes up, and accurately respectively draws 10 μ L, successively injection liquid chromatography, measures.With sample size X(μ g) linear regression is carried out to peak area A, regression equation is respectively: benzoyl mesaconine:
a=843 288
x+ 920.65,
r=0.9 999; Benzoyl aconite alkali:
a=713 106
x+ 237.35,
r=0.9 999; Benzoyl Hypaconitine:
a=763 932
x+ 6087.1,
r=0.9 999.Known benzoyl mesaconine is good linear relation at 0.061-0.605 μ g, benzoyl aconite alkali at 0.124-1.244 μ g, benzoyl Hypaconitine peak area and sample size within the scope of 0.125-1.248 μ g.
3.2.4 precision test draws the mixing reference substance solution 10 μ L of same concentration, repeat sample introduction and measure 6 times, record chromatogram, the RSD of result benzoyl mesaconine, benzoyl aconite alkali, benzoyl Hypaconitine peak area is respectively 1.03%, 0.69%, 1.34%.
3.2.5 stability test precision takes Traditional Method stewing monkshood sample 3g, by legal system available test sample solution below 3.2.1.2 item, difference sampling and measuring after room temperature places 0 h, 2 h, 4 h, 8 h and 24 h, the RSD of result benzoyl mesaconine, benzoyl aconite alkali, benzoyl Hypaconitine 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 Traditional Method and simmers monkshood sample 3g 5 parts, by legal system available test sample solution below 3.2.1.2 item, measures in accordance with the law, in results sample benzoyl mesaconine, benzoyl aconite alkali, benzoyl Hypaconitine mass fraction (
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 taking 6 parts of known content of average recovery test simmers monkshood sample 1.5 g, every part respectively precision add reference substance solution benzoyl mesaconine 50 μ L, benzoyl aconite alkali 200 μ L, benzoyl Hypaconitine 1mL, by legal system available test sample solution below 3.2.1.2 item, measure in accordance with the law.The new benzoyl aconite alkali of result, benzoyl aconite alkali, benzoyl Hypaconitine 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.
Specify according under " Chinese Pharmacopoeia " 2010 editions monkshood items, calculate by dry product, this product is containing benzoylmesaconine (C
31h
43nO
10), benzoyl aconine (C
32h
45nO
10) and benzoyl time aconine (C
31h
43nO
9) total amount, must not 0.010% be less than.This experiment is to contain benzoylmesaconine, benzoyl aconine, benzoyl time aconine for contrast, in salted aconite root, content is lower, and standards of pharmacopoeia can be reached after adopting simmer method to concoct, the content that wherein monkshood that stove processed is concocted simmered by conventional method and monkshood all can meet standards of pharmacopoeia, but adopts the monkshood content data fluctuation of conventional method large.
4. brief summary
The technological parameter of two kinds of concocting methods all selects Jianchang to help tradition to simmer the standard of RADIX ACONITI LATERALIS PREPARATA, by experimental result, a few indifference of stewing monkshood quality prepared by the method adopting conventional method and monkshood to simmer stove processed, the stewing monkshood namely adopting stewing stove processed to prepare can reach the quality standard that monkshood is simmered by Jianchang side.
Claims (10)
1. an industrialization processing procedure for monkshood simmered by the prepared slices of Chinese crude drugs, it is characterized in that concocting method is as follows:
(1), get salted aconite root, select stepping, in placing container, add water to and flood salted aconite root completely, between soak period, every day changes water 2-4 time, when in time soaking water at 25 DEG C, electrical conductivity is down to 6000 below μ s/cm, takes out, and drain the water to obtain the obtained thing of step (1);
(2), by the enlargement top of the obtained thing of step (1) upper, most advanced and sophisticated under, be placed on temperature automatically controlled stewing stove rack processed, cover the clean ginger slice of some layers in the above, 8-16kg ginger is added by the obtained thing of every 100kg step (1), add thin chaff ash, furnace body processed is simmered to filling, the heating-up temperature arranging lower heating component is 70-130 DEG C, the heating-up temperature of upper heating component is 110-180 DEG C, adds fire bending system 24-48 hours, treats ash cooling, take out monkshood, obtain the obtained thing of step (2);
(3), the obtained thing of step (2) is placed in heating container, uninterruptedly steams 6-12 hours, to mouth taste without or micro-have a numb feeling in the tongue time, take out, airing to room temperature obtains the obtained thing of step (3);
(4), get the obtained thing of step (3), cut the vertical thin slice that 1-4mm is thick, be dried to water content 5%-13% at 60-80 DEG C, obtain final product;
Described temperature automatically controlled stewing stove processed it comprise cover plate 1, body of heater 2 and heating system, heating component is had in described body of heater 2, each heating component comprises heating part and temperature sensing portion, the control circuit of heating component and control cabinet 6 connects to form heating system, each heating component has independently temperature control unit, control cabinet 6 is arranged on the outside of body of heater 2, rack 9 is provided with in body of heater 2, rack 9 put the thing scope of operation between each heating component, when simmering processed, in body of heater 2, be provided with heat transfer medium and thin chaff ash.
2. the industrialization processing procedure of monkshood simmered by a kind of prepared slices of Chinese crude drugs according to claim 1, it is characterized in that: when in step (1), in time soaking water at 25 DEG C, electrical conductivity is down to 4000 below μ s/cm, takes out; The heating-up temperature arranging lower heating component in step (2) is 80-110 DEG C, and the heating-up temperature of upper heating component is 140-170 DEG C.
3. the industrialization processing procedure of monkshood simmered by a kind of prepared slices of Chinese crude drugs according to claim 1, it is characterized in that: in step (2), add 10-12kg ginger by the obtained thing of every 100kg step (1), add thin chaff ash, simmering furnace body processed to filling, adding fire bending 36-48 hour;
In step (3), uninterruptedly steam 8-10 hours;
In step (4), cut the vertical thin slice that 2-3mm is thick, be dried to water content 6%-12% at 60-80 DEG C.
4. a temperature automatically controlled stewing stove processed, it comprises cover plate 1, body of heater 2 and heating system, it is characterized in that: in described body of heater 2 up and down and/or left and right be provided with heating component, each heating component comprises heating part and temperature sensing portion, the control circuit of heating component and control cabinet 6 connects to form heating system, each heating component has independently temperature control unit, control cabinet 6 is arranged on the outside of body of heater 2, rack 9 is provided with in body of heater 2, rack 9 put the thing scope of operation between each heating component, when simmering processed, in body of heater 2, be provided with heat transfer medium;
When described body of heater 2 inwall is respectively provided with a set of heating component up and down, the thing scope of operation of putting of rack 9 is overlapped between the heating part of heating components upper and lower two, and described heat transfer medium comprises each Plants or mineral grey, sand, rice, wheat bran, husk, cavings, talcum powder and clam meal.
5. the temperature automatically controlled stewing of one according to claim 4 stove processed, is characterized in that: between the heating part of upper and lower two cover heating components, spacing distance is 8-50cm up and down.
6. according to the temperature automatically controlled stewing of the one according to 4 or 5 stove processed, it is characterized in that: the heating part of described heating component is electrothermal tube 5, the temperature sensing portion of described heating component is temperature sensor 4; A temperature sensor 4 and electrothermal tube 5 form an independently heating component, and independently heating component is connected with the independently temperature control unit circuit of control cabinet 6.
7. the temperature automatically controlled stewing of one according to claim 6 stove processed, is characterized in that: described electrothermal tube 5 is U-shaped, W type or flange-type heating pipe.
8. according to the temperature automatically controlled stewing of the one stove processed described according to 4 or 5, it is characterized in that: the heating part of described heating component is electrothermal tube 5, electrothermal tube 5 is U-shaped, W type or flange-type heating pipe.
9. the industrialization processing procedure of monkshood simmered by a kind of prepared slices of Chinese crude drugs according to 1-3 arbitrary claims, it is characterized in that: it is room temperature-300 DEG C that the temperature control parameter simmering stove processed arranges scope.
10. the temperature automatically controlled stewing of one according to claim 4 stove processed, is characterized in that: it is room temperature-300 DEG C that the temperature control parameter simmering stove processed arranges scope.
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| 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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