CN110664953B - Processing method of radix stemonae - Google Patents
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Abstract
The invention discloses a processing method of radix stemonae, which effectively improves the content of effective components, namely radix stemonae alkaloid components, in honey-fried radix stemonae by moistening radix stemonae slabs and molasses fermentation liquor solution and adding cane molasses into honey, thereby ensuring the cough relieving activity of the honey-fried radix stemonae, reducing the toxic and side effects of the radix stemonae, ensuring that the radix stemonae is safer and more effective in clinical use, further improving the quality and the effect of the honey-fried radix stemonae, reducing the production cost and having simple preparation process.
Description
Technical Field
The invention belongs to the field of medicines, relates to a method for processing a traditional Chinese medicinal material, and particularly relates to a method for processing radix stemonae.
Background
The radix Stemonae is dried root tuber of Stemonae radix Stemonae sessilifolia (Miq.) Miq, Stemonae radix Stemonae japonica (BL) Miq, or Stemonae radix Stemonae Lour, and is mainly produced in Shandong, Jiangsu, Anhui, Hunan, Guangxi, Yunnan, Hubei, etc. Sweet, bitter and slightly warm, enters lung meridian, and has the effects of moistening lung, descending qi, relieving cough, killing parasites and killing lice. Can be used for treating chronic cough, pulmonary tuberculosis cough, and cough; it is used for treating head louse, body louse, enterobiasis, and pudendal pruritus. Honey radix Stemonae has effects of moistening lung and relieving cough, and can be used for treating deficiency-type cough. The processed radix stemonae product and the processing method thereof are more, the honey is mainly used for stir-frying at present in clinical application, the crude radix stemonae product has little toxicity, and the irritation to the stomach can be relieved after being processed by honey, and the honey-fried product is usually used for treating chronic cough. Modern researches show that honey-fried radix stemonae has better cough relieving effect than that of raw products. The stemona sessilifolia has the best effect of relieving cough in different varieties of stemona sessilifolia, so the stemona sessilifolia is taken as a research object in the invention. The alkaloid in the stemona root mainly plays roles of relieving cough and relieving cough, wherein stemonine is a representative active ingredient, but researches show that the content of the main alkaloid ingredient playing the cough relieving activity is low after the stemona root is processed by honey, and the quality and the effect of the stemona root processed by honey are difficult to ensure.
Cane molasses, also known as syrup, is a thick liquid left after sugar production from sugar cane juice squeezed by sugar industry through heating, neutralization, precipitation, filtration, concentration, crystallization and other processes, and is one of the byproducts of sugar factories. The cane molasses has complex components, comprises protein, vitamins, organic acid and some metal ions, has high sugar content which generally accounts for 30-50 percent, and is a common raw material in the fermentation, feed, food and building industries.
The inventor aims at the research of processing radix stemonae, researches on various processing methods of radix stemonae are carried out, and the inventor finds that the addition of molasses fermentation liquor solution and cane molasses during the processing of radix stemonae with honey can effectively improve the content of alkaloid components of the processed radix stemonae and improve the cough relieving effect of the radix stemonae.
Disclosure of Invention
The invention aims to provide a method for processing radix stemonae in the prior art aiming at the problem that the content of main alkaloid components which play a role in relieving cough activity after radix stemonae is processed with honey is low, the method can effectively improve the content of the alkaloid components of radix stemonae processed with honey, and the effect of relieving cough is improved, and the preparation process is simple.
The technical scheme of the invention is as follows:
a processing method of radix stemonae comprises the following steps:
t1, taking fresh stemona roots, cleaning and airing;
t2, taking a clean stemona medicinal material, and slicing into thick slices;
t3, uniformly stirring the stemona tuber slabs and the molasses fermentation liquor solution, and moistening at normal temperature;
and T4, putting the moistened radix stemonae into a preheated stir-frying container, and adding honey water for processing to obtain the radix stemonae tea.
Further, in the processing method of radix stemonae, the thickness of the thick slice in the step T2 is 2-3 mm.
Further, in the processing method of radix stemonae, the molasses fermentation liquid solution in the step T3 is molasses fermentation liquid with the weight percentage of 3-8%; the molasses fermentation liquor can be cane molasses, beet molasses or corn molasses which are obtained through microbial fermentation.
Further, in the processing method of radix stemonae, the moistening time in the step T3 is 2-4 h.
Further, in the processing method of radix stemonae, the honey water in the step T4 is a mixed solution of honey, cane molasses and water, and the weight ratio of the honey to the cane molasses to the water is 1: 1-2.
Further, the stemona processing method comprises the step of processing the stemona with honey water in the step T4, wherein the ratio of the honey water to the stemona thick slices is 1: 1.
Further, the processing method of radix stemonae is characterized in that the processing temperature in the step T4 is 110-130 ℃.
Further, the processing method of radix stemonae is characterized in that the processing time in the step T4 is 10-20 min.
Compared with the prior art, the invention has the following beneficial effects:
the radix stemonae thick slices and the molasses fermentation liquid solution are moistened and the cane molasses is added into the honey, so that the content of the effective components, namely the alkaloid components of the radix stemonae, in the honey-fried stemona is effectively improved, and the molasses fermentation liquid and the cane molasses contain various active substances and nutritional components, so that the cough relieving activity of the honey-fried radix stemonae is improved, the toxic and side effects of the radix stemonae are reduced, the radix stemonae is safer and more effective to be clinically used, and the quality and the effect of the honey-fried radix stemonae are further improved. Because the processing process adopts the molasses with low price, the production cost can be reduced by more than half.
Detailed Description
The invention is further described with reference to specific examples, without limiting the scope of protection and the scope of application of the invention:
research on stemonine content and drug effect in radix Stemonae by one or more different processing methods
1 materials and instruments
1.1 reagents and drugs
Hydrochloric acid (AR, national drug group chemical agents ltd, 20160301); ammonia (AR, chemical agents ltd 20160901); chloroform (AR, national chemical group 20150811); yellow wine (Zhenjiang Hengshun wine industry, LLC 20180328); the methanol and the acetonitrile are both chromatographically pure; radix Stemonae (Guangxi Guilin Gongcheng, identified as Stemona tuberosa of Stemonaceae, Bai genus by professor of Kagao Liao lunar Liang, Chinese medicine identification and research laboratory of Guangxi traditional Chinese medicine university).
The SPF-level Kunming mouse has half male and female, 6-8 weeks old, 18-22 g weight, is provided by Yise laboratory animal technology, Inc. of Changchun city, and has a qualification number of SCXK (Ji) 2016-0003, and is approved by the medical ethics committee of the affiliated hospital of Guangxi medical university and then subjected to animal experiments, and has an approval number of NM-LL-2016-11-12-07.
1.2 instruments
An electric heating constant temperature water bath kettle (Shanghai Qixin scientific instruments Co., Ltd. HWS-26); an ultrasonic cleaner (KQ 3200B ultrasonic instruments Co., Ltd., Kunshan); an infrared thermometer (CWH 600, Asahi science and technology Co., Ltd., Sichuan); a circulating water type vacuum pump (Zhengzhou great wall science and industry Co., Ltd., SHB-B95); high performance liquid chromatography (Agilent 1260); a water purifier (UPT-I/II economic type of Sichuan Yopu super pure science and technology Limited); an infrared light wave furnace (Elite electric Shenzhen, Inc. CW 2002-Z).
2 methods and results
2.1 measurement of content
2.1.1 chromatographic conditions
The column was a Shim-pack VP-ODS column (250 mm. times.4.6 mm); the mobile phase is acetonitrile-water, and gradient elution is carried out for 0-2 min (40%), 2-30 min (60%) and 30-45 (40%); the flow rate is 1.0ml min < -1 >; the column temperature is 30 ℃; the detection wavelength is 254 nm; the amount of the sample was 20. mu.L.
2.1.2 preparation of the solution
2.1.2.1 reference preparation
Precisely weighing appropriate amount of radix Stemonae tuberose reference substance, dissolving in methanol, diluting to desired volume, shaking, and filtering with 0.22 μm microporous membrane to obtain the final product (each 1mL contains about 1mg of radix Stemonae tuberose).
2.1.2.2 preparation of test article
Precisely weighing 5g of the processed product prepared under the item 2.2, placing the processed product in a conical flask with a plug, precisely adding 50mL of 95% methanol, ultrasonically extracting for 1h, filtering, evaporating to dryness in a water bath, dissolving the residue in 25mL of 4% hydrochloric acid, performing suction filtration, adjusting the pH of the filtrate to 9-10 by adding ammonia water, transferring the filtrate to a separating funnel for extraction, performing rotary drying, dissolving the residue in methanol, fixing the volume to 2mL, and filtering through a 0.22 mu m microporous membrane to obtain the product.
2.1.3 methodology investigation
2.1.3.1 Linear relationship investigation
Precisely measuring 1.0mL of the tuberostemonine reference substance solution into a 1, 5, 10, 20, 50 and 100mL volumetric flask, adding methanol to a constant volume to a scale, and shaking up. Respectively measuring according to chromatographic conditions under the item of '2.1.1', taking the sample amount (mug) as a horizontal coordinate (X) and the peak area as a vertical coordinate (Y), drawing a standard curve, performing regression analysis, and calculating a regression equation and a correlation coefficient. The experiment result shows that the linear range of the stemonine Y-638.92X-425.83 and r-0.9991 is 20-500 mu g, which indicates that the linear range is good.
2.1.3.2 precision test
Precisely sucking 20 μ L of control solution under the term "2.1.2.1", and repeatedly injecting sample under the chromatographic condition under the term "2.1.1" for 6 times, wherein the integral value RSD of the tuberostemonine peak area is 2.68%, which indicates that the instrument precision is good.
2.1.3.3 repeatability test
According to the preparation of the test solution under the item 2.1.2.2, 6 parts of the test solution are respectively prepared, 20 mu L of the prepared test solution is precisely absorbed, the sample injection is carried out according to the chromatographic condition under the item 2.1.1, and the RSD value of the mass fraction of the tuberostemonine is 1.93 percent.
2.1.3.4 stability test
Precisely sucking 20 μ L of the test solution prepared under the item "2.1.2.2", injecting samples at 0, 2, 4, 6, 8, 14, and 16h under the chromatographic condition of the item "2.1.1", and determining that the stability is good within 16 h. The RSD of the integrated value of the peak area of the tuberostemonine is 2.71%.
2.1.3.5 sample recovery test
Precisely weighing 6 parts of the same radix stemonae processed product, each part is about 2.5g, placing the same radix stemonae processed product into a conical flask with a plug, precisely adding a proper amount of reference substances, and preparing a test solution under the item '2.1.2.2'; measured according to the chromatographic conditions under the term "2.1.1". The average recovery rate of the tuberostemonine is 97 percent and the RSD is 2.5 percent.
2.1.3.6 determination of samples
The content of the tuberostemonine is calculated according to the chromatographic condition measurement under the item of 2.1.1, and the result is shown in table 1.
2.2 preparation of different Stemona processed products
In order to ensure the representativeness of the sample and the reliability of the test result, the stemona sessilifolia raw product after being cut is randomly sampled and processed according to the following processing technology.
2.2.1 Honey roasting (traditional method)
Taking a pure stemona medicinal material with the thickness of 0.2-0.3 mm, processing the medicinal material with honey and water ratio of 10:10 at 120 ℃ for 20min, taking out, cooling and storing for later use.
2.2.2 Honey roasting (only adding cane molasses)
Taking 0.2-0.3 mm thick radix stemonae, adding honey water and radix stemonae medicinal material into honey water in a ratio of 1:1:2, processing at 120 deg.C for 20min, taking out, cooling, and storing for use.
2.2.3 Honey roasting (method of the invention)
Taking a clean stemona sessilifolia medicinal material with the thickness of 0.2-0.3 mm, adding 5% of cane molasses fermentation liquor, uniformly stirring, moistening for 2h at normal temperature, adding honey water and stemona sessilifolia medicinal material in a ratio of 1:1, processing for 20min at 120 ℃, taking out, cooling and storing for later use.
2.3 results
The content of the active ingredient of the stemona tuberosa is increased after the stemona tuberosa is processed, and the stemona tuberosa alkali content measured by different processed products is from high to low: honey roasting (the method of the invention) > honey roasting (only cane molasses is added) > honey roasting (the traditional method) > raw product. The results are shown in Table 1.
TABLE 1 Stemona tuberosa L.content of Stemona tuberosa L.processed products
3 observing the effect of the drug before and after processing
The Kunming mouse is half male and female, and water is not forbidden for 12 h. Placed in a 250mL beaker. A cotton ball is placed in a watch glass with the diameter smaller than that of the beaker, a screen is covered on the cotton ball, 0.3mL of ammonia water is injected into the cotton ball, and the beaker is quickly inverted so that the ammonia water stimulates the mouse to cause cough. The strong contraction of the abdominal muscles of animals is taken as the standard, and the mouth opening and the exhalation are performed simultaneously. 100 mice qualified for initial screening of induced cough are judged to be 100 within 1min if the cough frequency is more than or equal to 3, and are randomly divided into 10 groups, 10 mice/group and half of males and females. Group 1 is physiological saline group, positive drug group (codeine 6 mg. kg)-1) High and low dose group (0.5 g.20 g) of radix Stemonae crude drug-1，0.25g·20g-1) The high and low dose group (0.5 g.20 g) of radix Stemonae honey-fried product (the method of the invention)-1，0.25g·20g-1) High and low dose (0.5 g.20 g) for radix Stemonae honey-fried (only cane molasses is added)-1，0.25g·20g-1) High and low dose (0.5g 20 g) group of radix Stemonae honey-fried (traditional method) products-1，0.25g·20g-1) 10 groups of mice were fasted for 8h before administration, water was prohibited for 2h, and the mice were continuously administered for 3d, and tested 1h after the last administration. Mice were stimulated with ammonia to elicit coughing as per the above method. The latency of each group of mice and the number of coughs in the mice within 3min were observed and recorded. The results are shown in Table 2.
TABLE 2 cough incubation period and cough frequency of mice in each experimental group
Note: compared with the blank control group, P is less than 0.05, P is less than 0.01, and P is less than 0.05 when compared with honey-fried products, honey-fried products (only cane molasses) and honey-fried products (the method of the invention) in the same dosage.
The effect of each experimental group on cough latency and cough frequency in mice is shown in table 2. The experimental results show that compared with the blank group, each experimental group can prolong the cough incubation period of the mice and reduce the cough frequency. The honey-fried products (the method of the invention) and the honey-fried products (only cane molasses is added) have significant differences from the honey-fried products (the traditional method), which shows that the cough relieving effect of the radix stemonae tuberose after processing is enhanced, and the cough relieving effect of the radix stemonae tuberose is further improved by adding the molasses fermentation liquor and the cane molasses.
Investigation of the second and third honey-roasting processes
1. Single factor test
1.1 concentration selection of molasses fermentation broth
In the test, the concentrations of 1%, 3%, 5%, 8% and 10% cane molasses fermentation liquor are compared, and after being moistened for 2h at normal temperature, honey water and stemona root medicinal materials are added into the honey water in a ratio of 1:1:2, wherein the honey water comprises honey, cane molasses and purified water, and the mixture is processed at 120 ℃ for 20min, and the stemonine content is taken as a research index. As a result, 3%, 5% and 8% of molasses fermentation liquor have higher tuberostemonine content, so 3-8% of molasses fermentation liquor is selected.
1.2 selection of smoldering time
In the test, 5% cane molasses fermentation liquor is respectively moistened for 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours and 5 hours, honey, cane molasses and purified water are added into honey water according to the proportion of 1:1:2 and the stemona root medicinal material is added into the honey water, the mixture is processed for 20min at the temperature of 120 ℃, and the moistening effect of the medicinal material and the content of the stemonine in the stemona leaves are taken as investigation indexes. As a result, the moistening effect is better when the moistening is carried out for 2-4 h, and the content of the tuberostemonine is higher, so the moistening time is selected to be 2-4 h.
1.3 selection of the amount of sugar cane molasses added
The cane molasses is black in color, sticky and contains a large amount of microorganisms, and the proportion of the microorganisms to the honey affects the quality of the molasses and the appearance and the internal quality of the radix stemonae. In the test, after 5% of cane molasses fermentation liquor is moistened for 2 hours, the weight ratio of honey to cane molasses to water is compared to 1:1:1, 1:2:2 and 1:3:3, and the appearance quality and the sessileine content of the mixed honey juice are considered indexes. The honey, the cane molasses and the water are in a weight ratio of 1:1:1 to 1:2:2, the appearance quality of the honey juice is good, the sessileine content is high, and therefore the weight ratio of the honey to the cane molasses to the water is 1: 1-2.
1.4 selection of processing temperature
In the test, 5% of cane molasses fermentation liquor is moistened for 2h, then honey, cane molasses and purified water are added into honey water in a ratio of 1:1:2 and radix stemonae in a ratio of 1:1, and the honey water is processed for 20min at 100 ℃, 110 ℃, 120 ℃, 130 ℃ and 140 ℃, and the appearance and the stemonine content of the processed sample are used as indexes for investigation. As a result, the sample processed at 110-130 ℃ has better appearance and character and higher content of the tuberostemonine, so the processing temperature is selected to be 110-130 ℃.
1.5 selection of processing time
In the test, 5% of cane molasses fermentation liquor is used for moistening for 2 hours, then honey water and radix stemonae medicinal materials are added into the honey water according to the proportion of 1:1:2, and the mixture is processed at 120 ℃ for different times: 5min, 10min, 15min, 20min, 25min, 30min, and taking appearance and character of the processed sample and tuberostemonine content as examination indexes. As a result, the appearance of the processed sample is better after being processed for 10-20 min, and the content of the tuberostemonine is higher, so the processing temperature is selected to be 10-20 min.
2. Determination of optimum process for roasting with honey
By using L9(34) The orthogonal test method is used for researching the concentration of molasses fermentation liquor, the moistening time, the processing temperature and the processing time by a 4-factor 3 level, and the result is as follows:
TABLE 3 extraction of Condition factor level tables
TABLE 4 radix Stemonae L9 (3) baked with honey4) Results of orthogonal experiments
TABLE 5 variance analysis of radix Stemonae processed with honey
The comprehensive scoring result analysis shows that the factor sequence influencing the honey roasting effect is A & gt C & gt D & gt B, and the preferred horizontal combination result is A2B1C2D3. From the anova results, factor A, C, D had a significant effect (P)<0.05), factor B had no significant effect (P)>0.05). Because the factor B has no obvious influence on the processing effect, the energy conservation is considered, the production efficiency is improved, the large-scale production is convenient, the factor B can be changed into the lowest level, namely, the soaking is carried out for 1 hour, and finally, the optimal processing technology of the honey-fried radix stemonae is preferably selected as A through comprehensive analysis2B1C2D3The method comprises mixing 0.2-0.3 mm thick radix Stemonae with 5% molasses fermentation solution, moistening at room temperature for 2 hr, adding Mel solution, and processing at 120 deg.C for 20 min.
Processing method of radix stemonae, radix stemonae and radix stemonae
Example 1
A processing method of radix stemonae comprises the following steps:
t1, taking a fresh radix stemonae tuberose product, cleaning and airing;
t2, taking the clean radix stemonae tuberose medicinal material, and cutting into pieces with the thickness of 0.2-0.3 mm;
t3, uniformly stirring the stemona tuberosa slices with 3 wt% of beet molasses fermentation liquor solution, and moistening for 4 hours at normal temperature;
and T4, putting the moistened radix stemonae japonica into a preheated frying container, adding honey, cane molasses and water in a weight ratio of 1:1:1 into the mixture of the radix stemonae slabs and the honey water, and processing at 110 ℃ for 20min to obtain the radix stemonae health food.
Example 2
A processing method of radix stemonae comprises the following steps:
t1, taking a fresh product of the vine stemona, cleaning and airing;
t2, taking a medicinal material of the clean and fresh radix stemonae, and cutting into pieces with the thickness of 0.2-0.3 mm;
t3, uniformly stirring the stemona tuberosa slices with 8 wt% of cane molasses fermentation liquor, and moistening for 2 hours at normal temperature;
and T4, putting the moistened stemona sessilifolia into a preheated frying container, adding honey, cane molasses and water in a weight ratio of 1:2:2 into the stemona sessilifolia thick slices and the honey water in a ratio of 1:1, and processing at 130 ℃ for 10min to obtain the stemona sessilifolia health food.
Example 3
A processing method of radix stemonae comprises the following steps:
t1, taking a fresh radix stemonae tuberose product, cleaning and airing;
t2, taking the clean radix stemonae tuberose medicinal material, and cutting into pieces with the thickness of 0.2-0.3 mm;
t3, uniformly stirring the stemona tuberosa slices with a cane molasses fermentation liquid solution with the weight percentage of 5%, and moistening for 2 hours at normal temperature;
and T4, putting the moistened radix stemonae japonica into a preheated frying container, adding honey, cane molasses and water in a weight ratio of 1:1:2 into the mixture of the radix stemonae slabs and the honey water in a ratio of 1:1, and processing at 120 ℃ for 20min to obtain the radix stemonae health food.
Example 4
A processing method of radix stemonae comprises the following steps:
t1, taking a fresh product of the radix stemonae, cleaning and airing;
t2, taking a clean radix stemonae stemona medicinal material, and cutting into pieces with the thickness of 0.2-0.3 mm;
t3, uniformly stirring the stemona sessilifolia slabs and 6 wt% of corn molasses fermentation liquor solution, and moistening for 3 hours at normal temperature;
and T4, putting the moistened radix stemonae sessilifoliae into a preheated frying container, adding honey, cane molasses and water in a weight ratio of 1:2:1 into the radix stemonae sessilifoliae and the honey water in a ratio of 1:1, and processing at 115 ℃ for 15min to obtain the radix stemonae sessilifoliae tea.
Fourthly, content determination of processed stemona roots
The stemonine content of the stemona tuberosa processed products of the above examples 1 to 4 was measured, and the results are shown in table 6.
TABLE 6 Stemona tuberosa alkaloid content of Stemona tuber processed products of various examples
Claims (1)
1. The processing method of the stemona root is characterized by comprising the following steps:
t1, taking fresh stemona roots, cleaning and airing;
t2, taking a clean stemona medicinal material, and cutting into thick slices with the thickness of 2-3 mm;
t3, uniformly stirring the stemona tuber slabs and molasses fermentation liquor with the weight percentage of 3-8%, and moistening for 2-4 h at normal temperature;
t4, putting the moistened radix stemonae into a preheated frying container, adding honey according to the ratio of 1:1 of the honey to the radix stemonae thick slices, and processing at 110-130 ℃ for 10-20 min to obtain the radix stemonae health food; the honey water is a mixed liquid of honey, cane molasses and water, and the weight ratio of the honey to the cane molasses to the water is 1: 1-2.
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