CN116850231B - Method for processing radix rehmanniae with Bulbus Lilii - Google Patents

Method for processing radix rehmanniae with Bulbus Lilii Download PDF

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CN116850231B
CN116850231B CN202310746604.XA CN202310746604A CN116850231B CN 116850231 B CN116850231 B CN 116850231B CN 202310746604 A CN202310746604 A CN 202310746604A CN 116850231 B CN116850231 B CN 116850231B
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radix rehmanniae
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王君明
巫晓慧
何庆文
刘鸣昊
张飞
龙冰玉
段雅倩
秦玲玉
宋玲玲
王彦嵋
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Henan University of Traditional Chinese Medicine HUTCM
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Abstract

The invention relates to a method for processing radix rehmanniae by lily, which can effectively solve the problems of enhancing the effects of nourishing yin, clearing heat and stopping bleeding of radix rehmanniae and increasing the effects of tranquillization, relieving cough and eliminating phlegm of radix rehmanniae, and the method comprises the steps of adding water into lily decoction pieces for decoction for 3 times, concentrating to obtain lily water decoction with the mass concentration of 0.50-0.83 g/mL, uniformly stirring radix rehmanniae and lily at a mass fraction ratio of 100:15-25, moistening until the medicine is thoroughly soaked, processing and drying the moistened radix rehmanniae pieces to obtain a finished product; the invention selects medicinal and edible traditional Chinese medicine lily to prepare the dried rehamnnia root for the first time, aims to innovatively develop the dried rehamnnia root prepared by lily as decoction pieces, and the prepared product can enhance the effects of nourishing yin, clearing heat and stopping bleeding of the dried rehamnnia root, also increases the effects of soothing the nerves, relieving cough and eliminating phlegm of the dried rehamnnia root, enhances the effects of the dried rehamnnia root and the pertinence of the medicament, expands the selection range and the adaptation range of the dried rehamnnia root decoction pieces, and improves the accuracy and the high efficiency of the dried rehamnnia root in clinical application.

Description

Method for processing radix rehmanniae with Bulbus Lilii
Technical Field
The invention relates to the technical field of traditional Chinese medicine processing, in particular to a method for processing radix rehmanniae by using lily as an auxiliary material.
Background
Rehmannia is fresh or dried root tuber of rehmannia Rehmannia glutinosa Libosch, which is a figwort plant, is mainly produced in Henan province, is one of four well-known Chinese medicines, has extremely high medicinal value, is especially favored by radix rehmanniae with the effects of clearing heat and cooling blood, nourishing yin and promoting the production of body fluid, contains radix rehmanniae in many classical formulas (such as lily rehmannia decoction, honey-fried licorice root decoction, radix stephaniae tetrandrae rehmannia decoction and the like) of the Yisheng Zhang Zhongjing, and is often used as an important medicine or a monarch drug in the formulas. The new decoction pieces prepared by the characteristics of radix rehmanniae are extremely rare from the teaching materials such as the current 2020 edition of Chinese pharmacopoeia, national and provinces of processing standards, chinese medicine processing science and the like. Although the Tangchen Tibetan ware "herbal picking up and losing" has recorded radix rehmanniae Preparata for the first time, however, the drug property, efficacy and main treatment of radix rehmanniae Preparata have been changed fundamentally, the efficacy of radix rehmanniae is mainly sweet and cold nourishing yin and clearing heat, and the efficacy of radix rehmanniae Preparata is changed into sweet and warm blood replenishing and essence replenishing, and radix rehmanniae Preparata and radix rehmanniae have been two distinct traditional Chinese medicines; even if the prepared rehmannia root is available, the prepared rehmannia root is still limited, the legal prepared rehmannia root is very scarce, the prepared rehmannia root is an important medicine composition in a plurality of prescriptions (such as lily and rehmannia root soup and other secondary prescriptions), the clinical medicine requirement on the prepared rehmannia root is huge, the diseases are often complicated and changeable, and the pertinence of the clinical medicine requirement on the prepared rehmannia root for patients with different symptoms of different diseases is different, but the prepared rehmannia root cannot supply more prepared products suitable for different medicine pertinence requirements of patients with different diseases due to the lack of the prepared products, so the selectivity, the accuracy and the high efficiency of the prepared rehmannia root in clinical application are severely limited, and the industrialized application process of the prepared rehmannia root is restricted. The processing is one of the characteristics of the traditional Chinese medicine, and can play a plurality of roles of synergism, attenuation and the like on the traditional Chinese medicine through the aspects of 'mutual concoction is processed' to enhance curative effect, and 'mutual aversion is processed' to reduce toxicity and the like. The lily is dried fleshy scaly leaves of lily plant Paeonia ostii Lilium lancifolium thunder, lily Lilium brownii F.E.Brownvar.virdulum Baker or Lilium pumilum DC, is a medicinal and edible traditional Chinese medicine, has the effects of nourishing yin, moistening lung, clearing heart fire and soothing nerves, and is mainly used for treating yin deficiency, dry cough, cough with blood, dysphoria, palpitation, insomnia and dreaminess, absentmindedness and other symptoms. Lily and radix rehmanniae belong to a typical drug pair with the mutual synergy, which is seen in a spot from the secondary scene name Fang Baige and Shang Bianke, which lays a theoretical foundation for the 'mutual assistance' of lily for the preparation of radix rehmanniae. However, so far, no report has been made on the processing of radix rehmanniae by lily "the same materials" at home and abroad.
Disclosure of Invention
Aiming at the situation, the invention aims to overcome the defects of the prior art, and the invention aims to provide a method for processing the dried rehamnnia root by using the lily, which can effectively solve the problems of enhancing the effects of nourishing yin, clearing heat and stopping bleeding of the dried rehamnnia root and increasing the effects of soothing nerves, relieving cough and eliminating phlegm of the dried rehamnnia root.
The technical scheme of the invention is that the method for processing the radix rehmanniae by using the lily comprises the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. decocting lily decoction pieces with water with the weight and volume of 12 times of that of the lily decoction pieces for 3 times each time, decocting for 30 minutes each time, mixing filtrates, and concentrating to obtain lily water decoction with the mass concentration of 0.50-0.83 g/mL; the weight and volume refer to solids in g and liquids in mL;
c. taking the radix rehmanniae decoction pieces in the step a, adding the lily water decoction in the step b, mixing evenly the radix rehmanniae and the lily at a mass fraction ratio of 100:15-25, and moistening until the decoction is completely soaked (about 5 h);
d. c, processing and drying the moistened radix rehmanniae slices in the step to obtain a finished product;
the processing and drying are parching with slow fire, or lyophilizing at-80deg.C.
The invention selects medicinal and edible traditional Chinese medicine lily to prepare the dried rehamnnia root for the first time, aims to innovatively develop the dried rehamnnia root prepared by lily as decoction pieces, and the prepared product can enhance the effects of nourishing yin, clearing heat and stopping bleeding of the dried rehamnnia root, also increases the effects of soothing the nerves, relieving cough and eliminating phlegm of the dried rehamnnia root, enhances the effects of the dried rehamnnia root and the pertinence of the medicines, expands the selection range and the indication range of the dried rehamnnia root decoction pieces, meets the requirements of different medicine pertinence of patients with different illness states, improves the accuracy and the high efficiency of the dried rehamnnia root in clinical application, develops the medicinal value and the commercial value of the dried rehamnnia root, and has remarkable economic and social benefits.
Detailed Description
The following describes specific embodiments and specific cases of the present invention in detail with reference to examples.
The invention, in its practice, can be illustrated by the following examples
Example 1
The invention discloses a method for processing radix rehmanniae by using lily, which comprises the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 15.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction (30 mL) with the concentration of 0.50 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, and uniformly stirring, and moistening (about 5 h) until the decoction is completely permeated;
d. c, placing the dried rehmannia root slices in the step c in a frying pan, frying with slow fire (4 min,100 ℃) until the sections of the dried rehmannia root are brown-yellow to black or black, drying in a baking oven at 60 ℃ after the sections are slightly focused, taking out, and cooling.
Example 2
The invention discloses a method for processing radix rehmanniae by using lily, which comprises the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 20.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of about 0.67 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, and uniformly stirring, and moistening (about 5 h) until the decoction is completely permeated;
d. c, placing the dried rehmannia slices in the step c in a frying pan, frying with slow fire until the sections of the dried rehmannia slices are brown to black or black, and drying in a 60 ℃ oven after slightly focusing the sections of the dried rehmannia slices, taking out and cooling.
Example 3
The invention discloses a method for processing radix rehmanniae by using lily, which comprises the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 25.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of about 0.83 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, and uniformly stirring, and moistening (about 5 h) until the decoction is completely permeated;
d. c, placing the dried rehmannia slices in the step c in a frying pan, frying with slow fire until the sections of the dried rehmannia slices are brown to black or black, and drying in a 60 ℃ oven after slightly focusing the sections of the dried rehmannia slices, taking out and cooling.
Example 4
The invention discloses a method for processing radix rehmanniae by using lily, which comprises the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 15.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction (30 mL) with the concentration of about 0.50 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, and uniformly stirring, and moistening (about 5 h) until the decoction is completely permeated;
d. and c, freeze-drying the dried rehmannia root slices in the step c at the temperature of minus 80 ℃ in a freeze dryer, and taking out to obtain the dried rehmannia root slices.
Example 5
a. Taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 20.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of about 0.67 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, and uniformly stirring, and moistening (about 5 h) until the decoction is completely permeated;
d. and c, freeze-drying the dried rehmannia root slices in the step c at the temperature of minus 80 ℃ in a freeze dryer, and taking out to obtain the dried rehmannia root slices.
Example 6
The invention discloses a method for processing radix rehmanniae by using lily, which comprises the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 25.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of about 0.83 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, and uniformly stirring, and moistening (about 5 h) until the decoction is completely permeated;
d. and c, freeze-drying the dried rehmannia root slices in the step c at the temperature of minus 80 ℃ in a freeze dryer, and taking out to obtain the dried rehmannia root slices.
The invention selects the medicinal and edible traditional Chinese medicine lily to prepare the dried rehmannia root for the first time, the prepared preparation enhances the effects of nourishing yin, clearing heat and stopping bleeding of the dried rehmannia root, increases the effects of soothing the nerves, relieving cough and eliminating phlegm of the dried rehmannia root, enhances the effects and the pertinence of the medicament of the dried rehmannia root, changes the active ingredients of the dried rehmannia root decoction pieces, expands the selection range and the adaptation range of the dried rehmannia root decoction pieces so as to meet the requirements of different medicament pertinence of patients with different illness states and different symptoms, and obtains good beneficial technical effects through experiments, and related experimental data are as follows:
1. experimental materials
1.1 laboratory animals
ICR mice, male, SPF grade, 16-18 g body mass, supplied by Jinan Pengyue laboratory animal Breeding Co., ltd. [ SCXK (Lu) 20220006].
1.2 Experimental drugs
According to the embodiments 1-6 of the invention, the dried rehmannia root decoction pieces prepared from lily are obtained.
2. The prepared radix rehmanniae decoction pieces of Bulbus Lilii have effects of nourishing yin, clearing heat, tranquilizing, relieving cough, eliminating phlegm, and stopping bleeding.
2.1 grouping and administration of animals
After the adaptive breeding of 90 male ICR mice for one week, the mice were randomly divided into 9 groups, 10 groups and 1 blank group, (2) radix rehmanniae group, (3) lily decoction group, (4) example 1, (5) example 2, (6) example 3, (7) example 4, (8) example 5, (9) example 6, and the like according to the mass. The dried rehmannia root, the lily water decoction and dried rehmannia root decoction pieces processed by different lily are dissolved in 0.5% sodium carboxymethyl cellulose solution, and are subjected to gastric administration by a dosage of 2g/kg, a blank control group is subjected to administration of an equal volume of 0.5% sodium carboxymethyl cellulose solution for 1 time/d, the continuous gastric administration is carried out for 14 days, and the observation or measurement of the effects of nourishing yin, clearing heat, soothing nerves, relieving cough, eliminating phlegm and stopping bleeding of the dried rehmannia root special processed product is respectively carried out after the last administration for 1 hour.
2.2 detection of indicators related to nourishing yin and clearing heat
2.2.1 Water intake
Mice were tested for water intake on day 14 of dosing. Each mouse was placed individually in cages with 1 water bottle per cage, and the water intake of the mice was tested and calculated for 12 h.
2.2.2 anal temperature
Anal temperature measurements were made on day 14 of dosing, respectively. During measurement, the mouse is firstly grabbed, the anus is exposed, the mercury head of the thermometer is dipped with a small amount of lubricating liquid and then is gently and slowly inserted into the anal orifice of the mouse, the depth is about 1cm, and the temperature count value is read and recorded after the 'tic' sound prompt is heard.
2.2.3 Cold and Hot plate experiments
Maintaining the laboratory temperature (23+/-2) DEG C, and setting the temperature of a bottom plate of an automatic temperature control system: the low temperature plate is 20 ℃ and the high temperature plate is 39 ℃. On the 14 th day of administration, each group of mice is sequentially placed in each channel on the cold and hot plate under a quiet environment, the trend of the cold and hot temperature areas of the cold and hot plates is monitored by a camera to move, and finally the residence proportion of the hot areas of the mice is obtained.
2.2.4 serum cAMP, cGMP, T, T4, na + -ATP、Ca 2+ Assay of ATPase level
All mice were collected with eyes and blood, left standing at room temperature for 2 hours, centrifuged at 4℃and 3500r/min for 10min, and the upper serum was separated and the levels of mouse serum cAMP, cGMP, T and T4 were measured according to the kit instructions, respectively.
2.3 determination of tranquilization index (sleep experiment)
Abdominal injection of sodium pentobarbital (55mg.kg) -1 ) Sleep was induced and mice were observed for sleep latency (time from injection of pentobarbital sodium to appearance of mice over-reflection for more than 1 min), and mice over-reflection time for more than 1min was the standard for falling asleep. The total sleep time of the mice (the total time from the onset of sleep to the recovery of wakefulness) was recorded simultaneously.
2.4 determination of cough-relieving efficacy-related index (Ammonia water cough-inducing experiment)
The 500mL beaker is reversely buckled on a desktop provided with qualitative filter paper of 10cm multiplied by 10cm, 0.1mL of concentrated ammonia water is sucked by a 1mL syringe and injected on the filter paper, after natural volatilization for 30s, the filter paper is rapidly extracted, and the filter paper is put into a mouse to be tested. And (3) observing that the mice have the symptoms of abdominal muscle contraction, chest constriction and large mouth opening and are accompanied by cough sounds as the judgment basis of the cough, and recording the cough times of the mice within 2 minutes.
2.5 determination of the relevant index of the phlegm-eliminating efficacy (tracheal phenol Red excretion experiment)
Mice were intraperitoneally injected with 0.01mg.g of 5% phenol red physiological saline solution -1 . Taking the tracheal tissue with the same length from the thyroid cartilage of the mouse to the tracheal branch, placing the tracheal tissue into a centrifuge tube containing 2mL of physiological saline, adding 0.1mL of 0.5% sodium bicarbonate solution, performing ultrasonic treatment for 15min and soaking for 24h, centrifuging for 15min at 3000r/min, and taking supernatant. Absorbance at 546nm was measured, and the phenol red standard curve y=0.1018x+0.0455, r was substituted 2 Mice tracheal phenol red excretion (final results are expressed as concentrations) were calculated separately = 0.9992.
2.6 measurement of hemostatic index (tail-cutting method blood time test)
Placing the mice in a fixer, cutting the mice at a position 0.5cm away from the tip of the tail of the mice by using surgical scissors, starting timing when blood overflows by itself, and adsorbing blood drops once every 30 seconds by using filter paper until the blood stops naturally (no blood stain exists when the filter paper is sucked), namely the bleeding time.
3. Results
3.1 experiments for reinforcing yin-nourishing and heat-clearing efficacy of dried rehmannia root decoction pieces processed by lily
Abnormal increases in mouse water intake, serum cAMP, cAMP/cGMP, T3, T4 enzyme levels and decreased cGMP levels are generally indicative of the yin deficiency pattern of mice, while decreases in water intake, serum cAMP, cAMP/cGMP, T3, T4 levels and increases in cGMP levels are indicative of the yin-nourishing efficacy of the drug. Compared with radix rehmanniae, the radix rehmanniae decoction pieces prepared by the lily can lower the serum cAMP, cAMP/cGMP, T3 and T4 levels of mice and raise the cGMP levels, which proves that the yin nourishing efficacy of the radix rehmanniae decoction pieces prepared by the lily is enhanced. The results are shown in tables 1 and 2.
TABLE 1 dried rehmannia root decoction pieces processed with Lily the index of yin deficiency of mice before and after intervention (level of water intake, T3, T4)
Note that: the radix rehmanniae group was compared with the blank control group, * P<0.05, ** P<0.01; comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
TABLE 2 Dihuang decoction pieces prepared from Lily before and after intervention with mouse yin deficiency index (serum cAMP, cGMP, cAMP/cGMP)
Note that: the radix rehmanniae group was compared with the blank control group, * P<0.05, ** P<0.01; comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
abnormal rise of the anal temperature of the mice and abnormal reduction of the proportion of the hot area in cold and hot plate experiments generally represent internal fever of the mice, and the reduction of the anal temperature level of the mice and the rise of the proportion of the heat-transfer area by the medicine can reflect the heat-clearing efficacy of the medicine. Compared with radix rehmanniae, the radix rehmanniae decoction pieces prepared from lily can lower the anal temperature of mice and raise the proportion of hot areas, which proves that the heat-clearing efficacy of the radix rehmanniae decoction pieces prepared from lily is enhanced. The results are shown in Table 3.
TABLE 3 changes in internal Heat index (anal temperature, hot zone ratio) of mice before and after Lily processed decoction pieces of radix rehmanniae
Note that: the radix rehmanniae group was compared with the blank control group, * P<0.05, ** P<0.01; comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
3.2 experiment of increasing tranquillizing drug effect of decoction pieces of radix rehmanniae processed by Lily
The sleep time latency of the mice is increased and the sleep time is reduced, so that the insomnia state can be reflected, and the sleep latency of the mice can be reduced or the sleep time of the mice can be increased after administration, so that the nerve soothing effect of the drug can be reflected. The invention proves that the prepared rehmannia root decoction pieces of lily can reduce the sleep latency of mice or increase the sleep time of mice more than the rehmannia root. And the drug effect increase rate of the dried rehmannia root decoction pieces (example 1 to example 6) prepared by lily over the sleep latency period is 34.0%, 46.5%, 20.6%, 13.5%, 26.8%, 21.1% in sequence compared with dried rehmannia root; the drug effect increase rates of the dried rehmannia root decoction pieces (examples 1 to 6) prepared from lily over the sleeping time are 34.3%, 36.0%, 28.7%, 34.5%, 32.0% and 30.8% in order compared with dried rehmannia root. The prepared rehmannia root decoction pieces of lily have the effect of soothing nerves. The results are shown in Table 4.
TABLE 4 sleep latency and sleep duration of mice before and after Lily-processed decoction pieces of radix rehmanniae
Note that: comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
3.3 experiment of decoction pieces of dried rehmannia root processed with Lily to increase cough-relieving efficacy
The ammonia water cough-inducing experiment is a common experiment for testing the cough-relieving efficacy of drugs. After administration, the cough-relieving effect of the drug is reflected if the cough-relieving times caused by ammonia water of mice can be reduced. The invention proves that the prepared rehmannia root decoction pieces of lily can reduce the cough frequency of mice more than the rehmannia root, and the drug effect rising rate of the prepared rehmannia root decoction pieces of lily (example 1 to example 6) is 42.3 percent, 52.9 percent, 30.5 percent, 36.7 percent, 38.8 percent and 42.7 percent compared with the rehmannia root. The above description shows that the decoction pieces of radix rehmanniae processed by Bulbus Lilii have antitussive effect. The results are shown in Table 5.
TABLE 5 cough times with Ammonia in mice before and after Lily processed radix rehmanniae decoction pieces are intervened
Note that: comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
3.4 experiment of increasing phlegm eliminating efficacy of decoction pieces of radix rehmanniae processed with Lily
The tracheal phenol red excretion test is a common test for testing the expectorant efficacy of drugs. After administration, if the expelling amount of the tracheal phenol red of the mice can be promoted, the phlegm eliminating effect of the medicine is reflected. The invention proves that the prepared rehmannia root decoction pieces of lily can promote the excretion of the mouse tracheal phenol red more than the rehmannia root, and the drug effect rising rate of the prepared rehmannia root decoction pieces of lily (examples 1 to 6) is 104.5 percent, 93.0 percent, 110.0 percent, 96.2 percent, 185.3 percent and 219.3 percent compared with the rehmannia root. The dried rehmannia root decoction pieces prepared from lily have the effect of eliminating phlegm. The results are shown in Table 6.
TABLE 6 production of radix rehmanniae characteristics New decoction pieces Pre-and post-intervention mouse tracheal phenol Red excretion
Note that: comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
3.5 experiment for enhancing hemostatic efficacy of decoction pieces of radix rehmanniae processed with Lily
The tail cutting method is a common experiment for testing the hemostatic effect of the medicine. After administration, the bleeding time of the tail part of the mice can be shortened, and the hemostatic effect of the medicine is reflected. The invention proves that the bleeding time of the tail part of a mouse can be shortened more than the dried rehmannia root decoction pieces prepared from the lily, and the drug effect increasing rate of the dried rehmannia root decoction pieces prepared from the lily (example 1 to example 6) is 23.1 percent, 38.2 percent, 43.2 percent, 32.5 percent, 26.7 percent and 49.6 percent compared with the dried rehmannia root. The above description shows that the decoction pieces of radix rehmanniae processed by Bulbus Lilii have enhanced hemostatic effect. The results are shown in Table 7.
TABLE 7 dried rehmannia root decoction pieces prepared from Lily bulb before and after intervention for bleeding time of tip of mouse tail
Note that: the radix rehmanniae group was compared with the blank control group, * P<0.05, ** P<0.01; comparing the decoction pieces of radix rehmanniae processed by Bulbus Lilii with radix rehmanniae group, # P<0.05, ## P<0.01。
3.6 experiments for measuring the contents of catalpol, dihuang Gangoside D, wang Baige glycoside A and Wang Baige glycoside B in the dried rehmannia root decoction pieces processed by the lily
3.6.1 chromatographic conditions
Wang Baige glycoside a, wang Baige glycoside B chromatographic conditions: a Stablebond Analytical chromatographic column (4.6X105 mm,5 μm) with acetonitrile-0.1% phosphoric acid (18:82) as mobile phase was used, the detection wavelength was 312nm, the flow rate was 1.0mL/min, the column temperature was 30deg.C, and the sample injection amount was 10. Mu.l.
Referring to the catalpol chromatographic conditions in the 2020 edition of Chinese pharmacopoeia: methanol-0.1% phosphoric acid (1:99) is used as a mobile phase, the detection wavelength is 210nm, the flow rate is 1.0mL/min, the column temperature is 30 ℃, and the sample injection amount is 10 mu l.
Referring to the chromatographic condition of the rehmannia glycoside D in the "Chinese pharmacopoeia" of 2020 edition: methanol-0.1% phosphoric acid (1:99) is used as a mobile phase, the detection wavelength is 203nm, the flow rate is 1.0mL/min, the column temperature is 30 ℃, and the sample injection amount is 10 mu l.
3.6.2 preparation of control solution
Accurately weighing appropriate amounts of Wang Baige glycoside A and Wang Baige glycoside B, placing in a 10mL brown volumetric flask, adding 80% methanol solution to obtain a solution with concentration of 0.1 mg.mL -1 Is a control solution of (a).
Precisely weighing catalpol reference substance, placing in 10mL brown volumetric flask, adding flow match to obtain 2.0 mg.mL -1 Is a control solution of (a).
Precisely weighing a proper amount of a rehmannia glycoside D reference substance, placing the reference substance into a 10mL brown volumetric flask, and adding 25% methanol solution to prepare 0.2 mg.mL -1 Is a control solution of (a).
Preparation of 3.6.3 sample solution
Referring to the "Chinese pharmacopoeia" of 2020 edition, 2.0g of dried rehmannia root decoction pieces processed by lily are precisely weighed, placed in a round bottom flask, 50mL of methanol is added, the weighed weight is heated, refluxed and extracted for 1.5h, cooled, then weighed again, the reduced weight is complemented by methanol, shaking up, filtering, precisely weighing 10mL of subsequent filtrate, concentrating to near dryness, dissolving residues by mobile phase, transferring to a 10mL measuring flask, diluting to scale by mobile phase, shaking up, and passing through a 0.22 mu m microporous filter membrane for measuring catalpol.
Referring to the "Chinese pharmacopoeia" of 2020 edition, 1.0g of dried rehmannia root decoction pieces processed by lily is precisely weighed, placed in a conical flask with a plug, 25mL of 25% methanol is precisely added, weighed, subjected to ultrasonic treatment (power 400W, frequency 50 kHz) for 1h, cooled, weighed again, complemented with the reduced weight by 25% methanol, shaken uniformly, filtered and passed through a microporous filter membrane of 0.22 μm for measuring the rehmannia root glycoside D.
Precisely weighing about 2.0g of crude rehmannia decoction piece powder processed by lily, placing the crude rehmannia decoction piece powder into a round-bottomed flask, adding 50mL of 80% methanol, weighing, heating, refluxing and extracting for 1.5h, cooling, weighing again, supplementing the reduced weight with methanol, shaking uniformly, filtering, and taking the subsequent filtrate to pass through a 0.22 mu m microporous filter membrane for measuring Wang Baige glycoside A and Wang Baige glycoside B.
3.6.4 linear relationship investigation
Precisely absorbing appropriate amount of catalpol reference substance solution, placing into 10mL brown volumetric flask, adding 80% methanol, dissolving to constant volume to scale, and preparing into 0.05, 0.25, 0.5, 1, 2, 3mg·mL respectively -1 According to the chromatographic condition under the condition of 3.6.1, taking the catalpol peak area as an ordinate (Y) and the catalpol mass concentration as an abscissa (X), and drawing a standard curve to obtain a linear regression equation: y=3610.7x+74.203, r 2 = 0.9996, indicating that catalpol is 0.05-3 mg.mL -1 The linear relationship is good.
Precisely sucking a proper amount of rehmannia glycoside D reference substance solution, placing into a 10mL brown volumetric flask, adding 25% methanol to dissolve, and fixing volume to scale to obtain a solution with mass concentrations of 0.0625, 0.125, 0.25, 0.5, and 1mg·mL respectively -1 Sampling according to the chromatographic condition under 3.6.1 items, drawing a standard curve by taking the peak area of the rehmannia glycoside D as an ordinate (Y) and the mass concentration of the rehmannia glycoside D as an abscissa (X), and obtaining a linear regression equation: y= 3012.1X-10.349, r 2 =0.9999, indicating that catalpol is between 0.0625 and 1 mg.mL -1 The linear relationship is good.
Precisely sucking a proper amount of Wang Baige glycoside A reference substance solution, placing into a 10mL brown volumetric flask, adding 80% methanol, dissolving to volume to scale, and preparing into 0.00625, 0.0125, 0.025, 0.05, and 0.1mg·mL respectively -1 According to the chromatographic conditions under 3.6.1 items, taking Wang Baige glycoside A peak area as an ordinate (Y) and Wang Baige glycoside A mass concentration as an abscissa (X), and drawing a standard curve to obtain a linear regression equation: y=18147x+2.0115, r 2 =0.9995, indicating that catalpol is between 0.00625 and 0.1 mg.mL -1 The linear relationship is good.
Precisely sucking a proper amount of Wang Baige glycoside B reference substance solution, placing into a 10mL brown volumetric flask, adding 80% methanol to dissolve, and fixing volume to scale to obtain a solution with mass concentrations of 0.00625, 0.0125, 0.025, 0.05 and 0.1 mg.mL respectively -1 According to the chromatographic conditions under 3.6.1 items, taking Wang Baige glycoside B peak area as an ordinate (Y) and Wang Baige glycoside B mass concentration as an abscissa (X), and drawing a standard curve to obtain a linear regression equation: y=25239X-11.929, r 2 =0.9998, indicating that catalpol is between 0.00625 and 0.1 mg.mL -1 The linear relationship is good.
3.6.5 assay
The results show that the content of catalpol and rehmanniae radix glycoside D in lily processed radix rehmanniae decoction pieces (example 1-example 6) is reduced, but Wang Baige glycoside A and Wang Baige glycoside B components are added. The results are shown in Table 8.
TABLE 8 catalpol, dihuang Gangoside D, wang Baige glycoside A, wang Baige glycoside B content in decoction pieces of radix rehmanniae processed with Bulbus Lilii
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Note that: in comparison with the group of radix rehmanniae, # P<0.05, ## P<0.01。
the experimental data show that the dried rehmannia root decoction pieces prepared by the method have the effects of nourishing yin, clearing heat and stopping bleeding, and the effects of soothing the nerves, relieving cough and eliminating phlegm are proved to be improved, the traditional medicinal value of dried rehmannia root for nourishing yin, clearing heat and stopping bleeding is enhanced, the effect of dried rehmannia root on the indications such as insomnia, cough and phlegm retention is widened, the active ingredients of the dried rehmannia root are changed, the medicinal value of the dried rehmannia root is developed, and the dried rehmannia root decoction pieces have creative contribution for developing new decoction pieces and have remarkable economic and social benefits.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A method for processing radix rehmanniae with lily, which is characterized by comprising the following steps:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. decocting lily decoction pieces with water with the weight and volume of 12 times of that of the lily decoction pieces for 3 times each time, decocting for 30 minutes each time, mixing filtrates, and concentrating to obtain lily water decoction with the mass concentration of 0.50-0.83 g/mL; the weight and volume refer to solids in g and liquids in mL;
c. taking the radix rehmanniae decoction pieces in the step a, adding the lily water decoction in the step b, mixing evenly the radix rehmanniae and the lily at a mass fraction ratio of 100:15-25, and moistening until the decoction is completely permeated;
d. c, processing and drying the moistened radix rehmanniae slices in the step to obtain a finished product;
the processing and drying are parching with slow fire, or lyophilizing at-80deg.C.
2. The method for processing radix rehmanniae with lily according to claim 1, comprising the steps of:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 15.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of 0.50 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, uniformly stirring, and moistening until the decoction is completely permeated;
d. c, placing the dried rehmannia slices in the step c in a frying pan, frying with slow fire until the sections of the dried rehmannia slices are brown to black or black, and drying in a 60 ℃ oven after slightly focusing spots, taking out and cooling.
3. The method for processing radix rehmanniae with lily according to claim 1, comprising the steps of:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 20.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of 0.67 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, uniformly stirring, and moistening until the decoction is completely permeated;
d. c, placing the dried rehmannia slices in the step c in a frying pan, frying with slow fire until the sections of the dried rehmannia slices are brown to black or black, and drying in a 60 ℃ oven after slightly focusing the sections of the dried rehmannia slices, taking out and cooling.
4. The method for processing radix rehmanniae with lily according to claim 1, comprising the steps of:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 25.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of 0.83 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, uniformly stirring, and moistening until the decoction is completely permeated;
d. c, placing the dried rehmannia slices in the step c in a frying pan, frying with slow fire until the sections of the dried rehmannia slices are brown to black or black, and drying in a 60 ℃ oven after slightly focusing the sections of the dried rehmannia slices, taking out and cooling.
5. The method for processing radix rehmanniae with lily according to claim 1, comprising the steps of:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 15.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of 0.50 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, uniformly stirring, and moistening until the decoction is completely permeated;
d. and c, freeze-drying the dried rehmannia root slices in the step c at the temperature of minus 80 ℃ in a freeze dryer, and taking out to obtain the dried rehmannia root slices.
6. The method for processing radix rehmanniae with lily according to claim 1, comprising the steps of:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 20.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of 0.67 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, uniformly stirring, and moistening until the decoction is completely permeated;
d. and c, freeze-drying the dried rehmannia root slices in the step c at the temperature of minus 80 ℃ in a freeze dryer, and taking out to obtain the dried rehmannia root slices.
7. The method for processing radix rehmanniae with lily according to claim 1, comprising the steps of:
a. taking radix rehmanniae decoction pieces, removing impurities for later use;
b. weighing 25.0g of lily decoction pieces, adding water with the weight and volume of 12 times of the lily decoction pieces each time, decocting for 3 times each time for 30 minutes, combining the decoctions, and concentrating to obtain lily water decoction with the concentration of 0.83 g/mL;
c. taking 100g of dried rehmannia root decoction pieces after removing impurities in the step a, adding the lily water decoction in the step b, uniformly stirring, and moistening until the decoction is completely permeated;
d. and c, freeze-drying the dried rehmannia root slices in the step c at the temperature of minus 80 ℃ in a freeze dryer, and taking out to obtain the dried rehmannia root slices.
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