CN114191473B - Preparation method of high-efficiency poison ratio prepared common monkshood daughter root - Google Patents

Preparation method of high-efficiency poison ratio prepared common monkshood daughter root Download PDF

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CN114191473B
CN114191473B CN202111306276.9A CN202111306276A CN114191473B CN 114191473 B CN114191473 B CN 114191473B CN 202111306276 A CN202111306276 A CN 202111306276A CN 114191473 B CN114191473 B CN 114191473B
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radix aconiti
aconiti lateralis
aconite
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steaming
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CN114191473A (en
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刘宸
张姜岚
刘振宇
张艳茹
孙清荣
张国彦
崔浪军
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Chenggu Qunli Traditional Chinese Medicine Professional Cooperative
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Abstract

The invention relates to a preparation method of a high-efficiency-toxicity-ratio processed radix aconiti lateralis preparata tablet, belonging to the technical field of radix aconiti preparata. The preparation method comprises the following steps: moistening the dried radix Aconiti lateralis Preparata with water to obtain thoroughly moistened radix Aconiti lateralis Preparata; steaming the thoroughly moistened accessory pieces to obtain steamed accessory pieces; drying the steamed sliced aconite to obtain dried sliced aconite; and (4) frying the dried accessory piece, and obtaining the processed accessory piece after the surface is discolored and swollen. The preparation method solves the problems that the existing technology has low content of choline, low alkaloid content, low toxicity ratio, and insoluble components of water, ash and acid can not reach the regulations of pharmacopoeia.

Description

Preparation method of high-efficiency poison ratio prepared common monkshood daughter root
Technical Field
The invention relates to the technical field of processing of aconite, in particular to a preparation method of high-efficiency toxicity ratio processed aconite.
Background
Monkshood, a processed product of the root of Aconitum carmichaeli Debx, a plant of Ranunculaceae, is pungent and sweet in taste, strong in nature and heat, toxic, enters heart, kidney and spleen channels, floats yang, can be lifted and lowered, has the effects of restoring yang and relieving the adverse rise of energy, tonifying fire and supporting yang, dispelling cold and relieving pain and the like, is known as the first product of Yang recuperation and rescue and the first medicine of Mingmen true fire from Shen nong Ben Cao Jing, known as 'good general will of disorder of the world'. The monkshood is rich in diester alkaloids and monoester alkaloids, has various pharmacological effects, and has effects of tonifying heart, resisting arrhythmia, diminishing inflammation, relieving pain, resisting tumor, resisting aging, reducing blood sugar, reducing blood lipid, and enhancing immunity. Alkaloid is the main medicinal component of monkshood, the content of alkaloid is an important index for measuring the quality of monkshood, the toxicity of diester alkaloid in raw monkshood is higher than the drug effect, and the diester alkaloid must be hydrolyzed into monoester alkaloid through processing to achieve the aims of reducing toxicity and enhancing efficacy. Compared with 2015 edition of Chinese pharmacopoeia, 2020 edition of Chinese pharmacopoeia, the diester alkaloid is determined to be not more than 0.020% of total amount of aconitine, hypaconitine and mesaconine, the monoester alkaloid is determined to be not less than 0.010% of total amount of benzoylaconitine, benzoylhypaconitine and benzoylmesaconine, the water content is not more than 15.0%, the total ash content is not more than 6.0%, and the acid insoluble ash content is not more than 1.0%, so that the prescription can reach the drug entry standard. However, in the literature on monkshood processing at present, few reports are made on whether processed products meet the 2020 edition of Chinese pharmacopoeia regarding moisture, total ash and acid insoluble ash. Therefore, it is necessary to develop monkshood products meeting 2020 edition of Chinese pharmacopoeia.
The monkshood is harvested in seventy and august months, the monkshood is hot and humid in positive weather, and is extremely easy to rot after harvesting, so that the monkshood has the characteristic of 'rotting overnight', and therefore, the monkshood needs to be subjected to preservative treatment immediately after harvesting. The main antiseptic measures in the current production include low-temperature preservation, drying and airing and gallbladder-crust soaking. The low-temperature preservation technology is perfect, but the requirement on equipment is high, a special refrigeration house is required for preservation, the cost is high, the per mu yield of the monkshood is high, the unit price is low, and the low-temperature preservation technology is not suitable for large-scale preservation; the existing drying technology is perfect, but similar to low-temperature storage, a professional large-scale dryer or drying room is needed, and the cost is high (but far lower than that of low-temperature storage); the drying is convenient and the cost is low; the technology for soaking and preserving the radix aconiti lateralis preparata is simple to operate and low in technical requirement, can be operated in large batch by only one water tank, can be directly fed into the water tank after the radix aconiti lateralis preparata is harvested, is added with the radix aconiti lateralis preparata, is very suitable for operation of farmers and enterprises, and is a main measure for preserving the radix aconiti lateralis preparata at present. The study shows that the immersion of the common monkshood daughter root can effectively inhibit the growth of pathogenic bacteria of the common monkshood daughter root. In actual production, the harvest time of the monkshood is short, so farmers and enterprises generally adopt a mode of immersing 100 jin of monkshood and 30 jin of gallbladder in water to store the monkshood for a long time, and process the monkshood while soaking, wherein the longest soaking time can reach 9-12 months, thereby effectively prolonging the processing period of the monkshood. In addition, researches show that the gallbladder soaking has an important effect on the shape fixation of the monkshood, and the 30% gallbladder solution soaking can ensure that the decoction pieces are relatively stable in three texture parameters of hardness, elasticity and compactness. However, monkshood soaked in the bile-bar needs to be soaked and rinsed with clear water for many times in the processing process to remove the bile, and a large amount of loss of active ingredients can be caused while removing the bile, and the loss of total alkaloids of a product processed by the bile-monkshood is recorded in literatures to reach 80-90 percent, even the loss rate reaches 96.74 percent, so that monkshood processed by the bile-monkshood cannot reach the standard specified by pharmacopoeia easily; if the washing frequency is reduced, although the content of the effective components is kept, the gallbladder-crust residue is serious, and after the accessory piece with high gallbladder-crust residue is used, adverse reactions of the digestive tract such as stomach burning, spasm, vomiting and the like are easily caused, and the life safety is influenced. Therefore, the development of the gallbladder-free accessory piece is of great significance.
The processing method of the radix aconiti lateralis preparata tablet has the functions of resisting inflammation, relieving pain and resisting thrombus, and is described in pharmacopoeia in the specification that the radix aconiti lateralis preparata tablet is taken and scalded by sand according to a stir-frying method (general regulation 0213) until the radix aconiti lateralis preparata tablet swells and changes color slightly, details such as processing temperature, processing time and the like are not described excessively, the current commercially available radix aconiti lateralis preparata tablet is mainly processed by black and white radix aconiti lateralis preparata tablets, and the total alkaloid amount of the processed radix aconiti lateralis preparata tablet is greatly reduced because the black and white radix aconiti lateralis preparata tablets have the processes of soaking and rinsing to remove bile in the processing process, so that the total alkaloid amount of the processed radix aconiti lateralis preparata tablet is further reduced, and the radix aconiti lateralis preparata tablet is suspected to be excessively processed. The study finds that the content of monoester alkaloid in the ironed black tablets is 25.490 percent of the raw monkshood, the total content is 0.013 percent, the content of diester alkaloid is reduced to 0 percent, and the content of total alkaloid is 8.497 percent of the raw monkshood; the content of monoester alkaloid in the Chinese medicinal material aconite processed by the sand-scald and radix aconiti lateralis praeparata is 29.411 percent, the total content is 0.015 percent, the content of diester alkaloid is reduced to 0, and the content of total alkaloid is 9.803 percent of the raw radix aconite. The alkaloid is not only a toxic component of monkshood, but also a medicinal component of monkshood, and the aconite prepared from black and smooth slices and white monkshood has a great loss of alkaloid, so that the medicinal effect is reduced, time and labor are wasted, and the dosage is increased, so that the medicine is wasted and cannot be paid. Therefore, the method has important significance for processing the firecracker tag by using the gallbladder-free tag.
The dry aconite slice is easy to prepare in actual production, and has no treatment of soaking choline He Shuipiao in the processing, so that the alkaloid can be greatly preserved. Researches indicate that after unprocessed radix aconiti lateralis (dry radix aconiti lateralis) is scalded for 7min at 200 ℃, the content of monoester alkaloid can reach 270.9 percent of unprocessed radix aconiti lateralis, the total amount is 0.038 percent, the content of diester alkaloid can be reduced by 2.2 percent of unprocessed radix aconiti, the total amount is 0.0015 percent, the content of total alkaloid is 48.6 percent of unprocessed radix aconiti, the total alkaloid is reduced by 51.4 percent, and the monoester alkaloid and diester alkaloid accord with the regulation of pharmacopoeia. However, during the high-temperature sand ironing process of the dried aconite, the situation that the diester alkaloid is not reduced to the standard specified by pharmacopoeia and is scorched easily occurs, and the drug effect and the apparent quality of the aconite are influenced. The effective toxicity ratio (monoester alkaloid content/diester alkaloid content) can be used for comprehensively analyzing the change of the chemical components of the monkshood in the processing process, and can reflect the loss proportion of toxic components and effective components of the monkshood, and the higher the effective toxicity ratio is, the higher the loss degree of the toxic components is, the higher the loss degree of the effective components is. Therefore, the development of a high-toxicity-ratio auxiliary piece is necessary.
Disclosure of Invention
The invention aims to provide a preparation method of a high-efficiency toxicity ratio radix aconiti lateralis preparata tablet. The preparation method solves the problems that the existing technology has low content of choline, low alkaloid content, low toxicity ratio, and insoluble components of water, ash and acid can not reach the regulations of pharmacopoeia.
The invention provides a preparation method of a high-efficiency toxicity ratio radix aconiti lateralis preparata tablet, which comprises the following steps:
moistening the dried radix Aconiti lateralis Preparata with water to obtain thoroughly moistened radix Aconiti lateralis Preparata;
steaming the thoroughly moistened accessory pieces to obtain steamed accessory pieces;
drying the steamed sliced aconite to obtain dried sliced aconite;
and (4) frying the dried accessory piece, and obtaining the processed accessory piece after the surface is discolored and swollen.
Preferably, the preparation method of the dry aconite comprises the following steps: cleaning fresh radix Aconiti lateralis, slicing, oven drying or air drying to obtain dried radix Aconiti lateralis.
Preferably, the temperature of the drying does not exceed 50 ℃.
Preferably, the wetting through method comprises spraying water onto the dried appendage sheet.
Preferably, the rehydration rate of the moistened coupon is 35 to 65%.
Preferably, the steaming time is 1.5 to 2.7 hours.
Preferably, the drying temperature is 55-85 ℃.
Preferably, the frying temperature is 130-165 ℃.
The invention provides a preparation method of a high-efficiency toxicity ratio radix aconiti preparata tablet. Compared with the traditional processed radix aconiti lateralis (black aconite, white aconite or the dried radix aconiti lateralis directly processed into the processed radix aconiti lateralis), the processed radix aconiti lateralis is processed without being soaked in the bile, so that most of alkaloid is kept, the kidney toxicity and the ash content caused by the residue of the bile are prevented from being too high to be used as medicine, and the medicine safety and the production efficiency are improved; compared with the prepared aconite slice directly prepared from the dried aconite, the dried aconite slice prepared by the invention is added with the steps of rehydration and steaming, the reserved total alkaloid content is high, the effective toxicity ratio is high, and the appearance more conforms to the prepared aconite slice shape described in pharmacopoeia: the radix aconiti lateralis preparata powder is swelled and changed in color slightly, meets the pharmacopoeia requirements in the aspects of water content, total ash content and acid insoluble ash content, improves the medicinal value of radix aconiti lateralis preparata, and has wide market prospect.
Drawings
FIG. 1 is a UPLC diagram provided by the present invention;
FIG. 2 is the effect of the interaction of rehydration rate (A) and steaming time (B) provided by the present invention on the efficacy to toxicity ratio of a gun sliced aconite;
FIG. 3 is the effect of the interaction of rehydration rate (A) and drying temperature (C) provided by the present invention on the efficacy to toxicity ratio of the auxiliary pieces of the gun;
FIG. 4 shows the effect of the interaction between rehydration rate (A) and processing temperature (D) on the toxicity ratio of radix Aconiti lateralis Preparata;
FIG. 5 shows the effect of the interaction between steaming time (B) and drying temperature (C) on the efficacy-toxicity ratio of the auxiliary material;
FIG. 6 shows the effect of the interaction between steaming time (B) and processing temperature (D) on the effect-toxicity ratio of the processed radix Aconiti lateralis;
FIG. 7 shows the effect of the interaction between the drying temperature (C) and the processing temperature (D) on the toxicity of the processed radix Aconiti lateralis;
fig. 8 is a finished product diagram of the high-efficiency toxicity ratio auxiliary piece provided by the invention.
Detailed Description
The invention provides a preparation method of a high-efficiency toxicity ratio radix aconiti lateralis preparata tablet, which comprises the following steps:
moistening the dried radix Aconiti lateralis Preparata with water to obtain thoroughly moistened radix Aconiti lateralis Preparata;
steaming the thoroughly moistened accessory pieces to obtain steamed accessory pieces;
drying the steamed sliced aconite to obtain dried sliced aconite;
and (4) frying the dried accessory piece, and obtaining the processed accessory piece after the surface is discolored and swollen.
The invention wets the dry aconite with water to obtain the moistened aconite. In the present invention, the method for preparing the dry aconite preferably includes the steps of: cleaning fresh radix Aconiti lateralis, slicing, oven drying or air drying to obtain dried radix Aconiti lateralis. In the present invention, the temperature of the drying is preferably not more than 50 ℃, more preferably 40 ℃. In the present invention, the method of wetting through preferably comprises spraying water onto the dried coupon. In the present invention, the moisture regain of the moistened aconite is 35 to 65%, more preferably 35 to 45%, and still more preferably 40 to 45%.
After the thoroughly moistened aconite is obtained, the thoroughly moistened aconite is steamed to obtain the steamed aconite. In the present invention, the steaming time is preferably 1.5 to 2.7, more preferably 1.7 to 2.5 hours, and still more preferably 1.7 to 2 hours. In the present invention, the temperature of the steaming is preferably 100 to 105 ℃.
After the steamed sliced aconite is obtained, the steamed sliced aconite is dried by the invention to obtain the dried sliced aconite. In the present invention, the temperature of the drying is preferably 55 to 85 ℃, more preferably 70 to 80 ℃.
After the dried accessory piece is obtained, the invention fries the dried accessory piece, and obtains the processed accessory piece after the surface discolor and swell. In the present invention, the temperature of the stir-frying is preferably 130 to 165 ℃, more preferably 140 to 160 ℃.
The invention takes the dried aconite root slice as the raw material, firstly carries out rehydration and steaming, can quickly hydrolyze toxic diester alkaloid into monoester alkaloid, then carries out baking and processing, can reduce the processing time in the processing process, ensures that the aconite root slice keeps a large amount of effective components and accords with the standard specified by pharmacopeia, and can also ensure that the processed aconite root slice accords with the standard described in the pharmacopeia; the color of the product is changed slightly, and the situation of scorching cannot occur.
The preparation method of the high-efficiency-toxicity-ratio aconite is further described in detail with reference to the following specific examples, and the technical scheme of the invention includes but is not limited to the following examples.
The raw aconite is dry aconite, mud aconite is fresh aconite, and gall aconite is soaked in gall bladder.
Monoester type alkaloids: benzoylmesaconine, benzoylaconitine, benzoylhypaconine.
Diester-type alkaloids (toxic component): aconitine, hypaconitine, neoaconitine.
The total alkaloid content is calculated by the sum of monoester alkaloid and diester alkaloid.
Pharmacopoeia standard: the diester alkaloid content is not more than 0.02%, i.e. each gram of monkshood contains not more than 200 micrograms of diester alkaloid; the monoester alkaloid is not less than 0.01%, i.e. each gram of radix Aconiti lateralis contains not less than 100 microgram monoester alkaloid. The water content is not more than 15%, the total ash content is not more than 6%, and the acid insoluble ash content is not more than 1%.
The rehydration rate calculation formula is as follows: rehydration rate = (water addition/dry aconite mass) × 100%
Example 1
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.0 hr at 50 deg.C and 180 deg.C.
Example 2
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.0 hr at 70 deg.C and 150 deg.C.
Example 3
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.5 hr at 70 deg.C and 180 deg.C.
Example 4
Rehydrating dried radix Aconiti lateralis Preparata to water content of 70%, steaming for 1.5 hr at 70 deg.C and 150 deg.C.
Example 5
Rehydrating dried radix Aconiti lateralis Preparata to water content of 30%, steaming for 2.0 hr at 70 deg.C and 120 deg.C.
Example 6
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.0 hr at 90 deg.C and 120 deg.C.
Example 7
Rehydrating dried radix Aconiti lateralis Preparata to water content of 70%, steaming for 2.0 hr at 50 deg.C and 150 deg.C.
Example 8
Rehydrating dried radix Aconiti lateralis Preparata to water content of 70%, steaming for 2.5 hr at 70 deg.C and 150 deg.C.
Example 9
Rehydrating dried radix Aconiti lateralis Preparata to water content of 70%, steaming for 2.0 hr at 70 deg.C and 120 deg.C.
Example 10
Rehydrating the dry radix Aconiti lateralis Preparata until its water content reaches 30%, steaming for 2.0 hr at 90 deg.C and 150 deg.C.
Example 11
Rehydrating the dry radix Aconiti lateralis Preparata until its water content reaches 70%, steaming for 2.0 hr at 70 deg.C and 180 deg.C.
Example 12
Rehydrating the dry radix Aconiti lateralis Preparata until its water content reaches 50%, steaming for 2.0h, drying at 90 deg.C, and processing at 180 deg.C.
Example 13
Rehydrating the dry radix Aconiti lateralis Preparata until its water content reaches 30%, steaming for 2.0 hr at 50 deg.C and 150 deg.C.
Example 14
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 1.5 hr at 50 deg.C and 150 deg.C.
Example 15
Rehydrating dried radix Aconiti lateralis Preparata to water content of 30%, steaming for 1.5 hr at 70 deg.C and 150 deg.C.
Example 16
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.0 hr at 50 deg.C and 120 deg.C.
Example 17
Rehydrating dried radix Aconiti lateralis Preparata to water content of 30%, steaming for 2.5 hr at 70 deg.C and 150 deg.C.
Example 18
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.5 hr at 70 deg.C and 120 deg.C.
Example 19
Rehydrating dried radix Aconiti lateralis Preparata to water content of 70%, steaming for 2.0 hr at 90 deg.C and 150 deg.C.
Example 20
Rehydrating dried radix Aconiti lateralis Preparata to water content of 30%, steaming for 2.0 hr at 70 deg.C and 180 deg.C.
Example 21
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 1.5 hr at 90 deg.C and 150 deg.C.
Example 22
Rehydrating the dry radix Aconiti lateralis Preparata until its water content reaches 50%, steaming for 2.5 hr at 50 deg.C and 150 deg.C.
Example 23
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 1.5 hr at 70 deg.C and processing temperature of 180 deg.C.
Example 24
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 1.5 hr at 70 deg.C and 120 deg.C.
Example 25
Rehydrating dried radix Aconiti lateralis Preparata to water content of 50%, steaming for 2.5 hr at 90 deg.C and 150 deg.C.
Comparative example 1
Dried aconite
Cleaning rhizoma Typhonii, slicing, and oven drying at 40 deg.C.
Comparative example 2
Steamed slice
In comparative example 1, the dried aconite piece is rehydrated to make the water content reach 45%, the steaming time is 2.0h, and the drying temperature is 70 ℃ for standby.
Comparative example 3
Traditional black flake
Decocting radix Aconiti lateralis Preparata and the extractive solution until the decoction is thoroughly soaked, taking out, rinsing with water, longitudinally cutting to 5mm, rinsing with water, dyeing with color matching solution, steaming to oil surface, and oven drying.
Comparative example 4
Black flake processed product
In comparative example 3, the black smooth sheet is processed into a prepared common monkshood daughter root for standby, and the processing method comprises the following steps: putting river sand into a frying pan, frying to a smooth state, putting the black shun tablets in the comparative example 3, frying until the appearance is swelled to change color, taking out, quickly screening out the sand, and cooling.
Comparative example 5
Sand ironing dry accessory piece
Putting river sand into a frying pan, frying to a smooth state, putting the dried aconite slices in the comparative example 1, frying until the appearance is dark brown-yellow and the section is brown-yellow, taking out, quickly screening out sand, and cooling.
Results of UPLC of examples and comparative examples
Detecting the content and toxicity ratio of diester alkaloids (aconitine, hypaconitine, mesaconine) and monoester alkaloids (benzoylaconine, benzoylhypaconine, benzoylmesaconine) in the obtained radix Aconiti lateralis by ultra-performance liquid chromatography (UPLC) (monoester alkaloids/diester alkaloids)
The method comprises the following steps:
preparation of control solutions
Taking appropriate amount of aconitine, hypaconitine, mesaconine, benzoylaconine, benzoylhypaconine, benzoylmesaconine reference substance, 0.05 mol.L -1 Dissolving with hydrochloric acid to obtain control solution containing aconitine 1.0mg, hypaconitine 1.1mg, neoaconitine 1.8mg, benzoylaconine 1.0mg, benzoylhypaconitine 1.8mg, and benzoylmesaconine 2.6mg per 1ml, and storing in refrigerator at 4 deg.C for use. 0.05 mol. L -1 Hydrochloric acid solution was used as a negative control.
Preparation of test solution
Precisely weighing 1.000g of monkshood powder, paralleling 3 parts, placing in a 50ml centrifuge tube, adding 5ml0.05mol.L -1 Mixing with hydrochloric acid, ultrasonic treating for 30min, and 6000r.min -1 Centrifuging for 10min, sucking 0.5ml of supernatant, adding 1mL of 0.05mol. L -1 Diluting with hydrochloric acid, and filtering with 0.22 μm filter membrane.
Chromatographic conditions
And (3) chromatographic column: ultimate UHPLC PolarRP,1.8 μm,2.1 × 100mm, w-Port, column temperature 35 ℃, mobile phase a:2 mmol. L -1 Ammonium acetate solution (containing 0.1% formic acid), mobile phase B: acetonitrile; elution procedure: 0 to 1.5min 0 to 12%; 1.5-3min 12-14 percent; 3-7min 14-20 wt.%; 7-10min 20%; b, 10-13 min 20-25%; 13 to 15min 25 to 30%; the flow rate is 0.4ml/min, the detection wavelength is 240nm, and the sample injection amount is 10 mu l. The UPLC is shown in figure 1, wherein, 1. Aconitine; 2. hypaconitine; 3. neoaconitine; 4. benzoylaconitine; 5. benzoylhypaconine; 6. benzoylmesaconine; control (A), sample (B), raw aconite (C), negative control (D). Various aconitine standard curves (relationship between peak area and content) are obtained by calculation and are shown in the following table 1:
TABLE 1 Standard curves of various aconitines
Figure BDA0003340401460000101
The test results of the pieces of the attached material for the examples 1 to 25 are shown in Table 2.
Table 2 results of component detection in the pieces of the attached shots of examples 1 to 25
Figure BDA0003340401460000102
Figure BDA0003340401460000111
The test results (table 2) were analyzed and fitted to obtain a multiple regression model: y =47.73-2.74A +4.59B +1.27C-3.42D-6.26AB-2.61AC-0.2377AD-0.3837BC +0.6215BD-1.93CD-11.18A 2 -6.84B 2 -7.55C 2 -18.41D 2 。
The regression model variance and the results are shown in table 3, the regression model P =0.0002 is very significant, the distortion term P =0.0513 > 0.05 is not significant, and the experimental error is small. Determining the coefficient R 2 =0.8923, which shows that regression model fits well. Factors B, D, A 2 ，B 2 ，C 2 ，D 2 The obvious influence factor indicates that the effect-toxicity ratio of the auxiliary material is greatly influenced.
TABLE 3 analysis of variance of regression models
Figure BDA0003340401460000112
Figure BDA0003340401460000121
Analyzing the regression model by using Design Expert 12 software, and fixing any two of the four factors as zero level, wherein the interaction of the remaining two factors affects the effect-toxicity ratio of the auxiliary pieces, so as to obtain figures 2-7 (figure 2 shows the effect of the interaction of rehydration rate (A) and steaming time (B) on the effect-toxicity ratio of the auxiliary pieces), figure 3 shows the effect of the interaction of rehydration rate (A) and drying temperature (C) on the effect-toxicity ratio of the auxiliary pieces, figure 4 shows the effect of the interaction of rehydration rate (A) and processing temperature (D) on the effect-toxicity ratio of the auxiliary pieces, figure 5 shows the effect of the interaction of steaming time (B) and drying temperature (C) on the effect-toxicity ratio of the auxiliary pieces, figure 6 shows the effect of the interaction of steaming time (B) and processing temperature (D) on the effect-toxicity ratio of the auxiliary pieces, and figure 7 shows the effect of the interaction of drying temperature (C) and processing temperature (D) on the effect-toxicity ratio of the auxiliary pieces): a 3D response surface graph and a corresponding contour line plane graph. The steaming time and the processing temperature have the greatest influence on the effect-toxicity ratio of the aconite, and then the rehydration rate and the drying temperature have the least influence on the effect-toxicity ratio of the aconite; the interaction of the rehydration rate and the steaming time is most obvious, and the interaction of other factors does not reach a remarkable level.
2.3 Process validation
Optimizing the processing technology of the auxiliary pieces of the firecracker by the response surface, wherein the obtained optimal technological conditions are as follows: the rehydration rate is 44.77%, the steaming time is 2.22h, the drying temperature is 72.59 ℃, the processing temperature is 147.28 ℃, and the maximum effect-toxicity ratio of the prepared aconite is 49.359. Considering the feasibility of the actual process, the parameters are adjusted to be integers, namely the rehydration rate is 45%, the steaming time is 2h, the drying temperature is 70 ℃, the processing temperature is 150 ℃, and the prediction result is 47.721. Through 5 verification tests (table 4) under the conditions (the rehydration rate is 45%, the steaming time is 2h, the drying temperature is 70 ℃, and the processing temperature is 150 ℃), the effect-toxicity ratio of the prepared aconite main body tablet is 47.138, which is similar to the predicted value of the model, and the model is reasonable and effective. The annex is shown in figure 8.
TABLE 45 verification test results
Figure BDA0003340401460000131
2.4 measurement results of sample content in control group
The measurement results of the alkaloid content of the control group samples are shown in Table 5.
TABLE 5 alkaloid content of control samples
Figure BDA0003340401460000132
Figure BDA0003340401460000141
As can be seen from Table 5, compared with the control sample, the processed radix Aconiti lateralis Preparata with alkaloid content of diester-type alkaloid of 0.409% and monoester-type alkaloid of 0.043% can be reduced to 0.004%, the monoester-type alkaloid can be increased to 0.196%, the toxicity and potency ratio is 47.318, and the total alkaloid content is 44.199% of the dry radix Aconiti lateralis Preparata. Compared with steamed aconite, although the content of the total alkaloid is 71.133 percent, the effect-toxicity ratio is more than 2 times; compared with Heishui tablet, the content of total alkaloid is 160.375 percent, and the effect-toxicity ratio is 23 times of that of the Heishui tablet; compared with the traditional radix aconiti preparata slice, the content of the total alkaloid is 244.803 percent, and the effect-toxicity ratio is 15 times higher; compared with the hot-sand dried aconite, the content of the total alkaloid is 97.382 percent, and the effect-toxicity ratio is more than 21 times.
2.5 determination of moisture, total Ash and acid insoluble Ash
The measurement results of moisture, total ash and acid-insoluble ash of the prepared processed pieces and black flakes and the conventional processed pieces are shown in table 6.
TABLE 6 moisture, total Ash and acid insoluble Ash content of the test and control samples
Sample (I) Moisture (%) Total ash (%) Acid-insoluble ash (%)
The invention relates to a firecracker accessory piece 6.485 3.185 0.169
Steamed slice 7.514 3.647 0.127
Traditional black flake 6.537 9.424 1.346
Black smooth sheet firecracker 5.447 10.487 1.594
Sand-heated dry accessory piece 4.527 3.156 0.675
In addition to water, china pharmacopoeia 2020 edition provides requirements for total ash content and acid insoluble ash content of the processed aconite, the water content is required to be not more than 15%, the total ash content is not more than 6%, and the acid insoluble ash content is not more than 1%, the water content of the processed aconite in the invention is 6.485%, the total ash content is 3.185%, and the acid insoluble ash content is 0.169%, the new edition of pharmacopoeia is met, compared with the traditional black flabels and black flabels, the water content is equivalent, and the total ash content and the acid insoluble ash content are obviously reduced; compared with the sand-scalding dry tablet, the acid-insoluble ash content is obviously reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (4)

1. A preparation method of a high-efficiency toxicity ratio radix Aconiti lateralis Preparata comprises the following steps:
moistening the dried radix Aconiti lateralis with water to obtain moistened radix Aconiti lateralis;
steaming the thoroughly moistened accessory pieces to obtain steamed accessory pieces;
drying the steamed sliced aconite to obtain dried sliced aconite;
parching the dried radix Aconiti lateralis, and obtaining the processed radix Aconiti lateralis after the surface changes color and swells;
the rehydration rate of the thoroughly moistened aconite is 35-65%;
the steaming time is 1.5 to 2.7 hours;
the steaming temperature is 100 to 105 ℃;
the drying temperature is 55 to 85 ℃;
the stir-frying temperature is 130 to 165 ℃.
2. The method for preparing a dry aconite according to claim 1, wherein the method for preparing the dry aconite comprises the steps of: cleaning fresh radix Aconiti lateralis, slicing, oven drying or air drying to obtain dried radix Aconiti lateralis.
3. The method of claim 2, wherein the temperature of the drying does not exceed 50 ℃.
4. The method of claim 1, wherein the wetting-through process comprises spraying water onto the dried coupon.
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