CN115201398B - Quality detection method for radix seu herba Kadsurae Longipedunculatae, extract and preparation thereof - Google Patents
Quality detection method for radix seu herba Kadsurae Longipedunculatae, extract and preparation thereof Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
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Abstract
The invention discloses a quality detection method of a medicine material of a Chinese yam, an extract and a preparation thereof, which comprises the following steps: (1) preparing a mountain searching tiger control medicinal material solution; (2) preparing a sample solution of the Kadsura longepedunculata; (3) And (3) according to a thin-layer chromatography, sucking the sample solution of the Kadsura longepedunculata and the sample solution of the Kadsura longepedunculata to be spotted on the same silica gel G thin-layer plate, developing with a mixed solution of dimethylbenzene and ethyl acetate as a developing agent, airing and checking. In the quality detection method, thin-layer chromatography is adopted, and the mixed solution of dimethylbenzene and ethyl acetate is used as a developing agent for identification, so that the separation effect is good, spots are round and clear, the specific shift value is moderate, the reproducibility is good, the medicinal materials of the radix polygoni cuspidati and the extracts and preparations thereof can be effectively identified, and the quality control and the clinical application of the medicinal materials of the radix polygoni cuspidati and the extracts and preparations thereof are facilitated.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicines, in particular to a traditional Chinese medicine preparation, relates to a medicinal material of a mountain searching tiger and extraction thereof quality detection method of the product and preparation.
Background
The Chinese medicinal herb is derived from the Chinese prickly ash Zanthoxylum austrosinense Huang of the Rutaceae plant, is a folk common medicine, is a common medicinal material for Yao medicine and herbal medicine, and has the effects of dispelling wind, removing toxin, removing stasis, relieving swelling, promoting qi circulation and easing pain; it is used for treating venomous snake bite, rheumatalgia, stomach ache, toothache, sprain and contusion, fracture, common cold, etc.
The Chinese medicine "Qishan Tiger" is a main raw material of Shuanghu Zhongtongning (tincture), and is carried in the annex of Guangxi Chinese medicine Standard and Chinese medicine Chengfang preparation "by Ministry of health, the text of the quality standard of Chinese medicine in places and countries is not carried yet, and belongs to the" reverse hanging variety ". The Chinese medicinal materials of Kadsura longepedunculata are recorded in the works of Chinese plant Zhi, chinese Ben Cao, modern Ben Cao gang mu, bone fracture disease Chinese herbal medicine primary color spectrogram, guangxi Ben Cao Ji, etc., and the related contents of original plant, geographical distribution and medicinal value are briefly described, but the medicinal parts are inconsistent, and the root, stem, root bark and stem bark are all used. At present, the existing standard does not have an identification method and a quality detection standard aiming at the medicinal materials of the radix polygoni multiflori, which are not beneficial to quality assurance and market specification of the medicinal materials of the radix polygoni multiflori.
The present invention has been made in view of this.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a quality detection method for a medicinal material of the radix sophorae flavescentis, an extract and a preparation thereof. The thin-layer chromatography of the invention can effectively identify the medicinal material of the radix polygoni cuspidati and is beneficial to the quality control and clinical application of the medicinal material of the radix polygoni cuspidati.
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that:
the first object of the invention is to provide a quality detection method of a medicinal material of a radix polygoni multiflori, which comprises the following steps:
(1) Preparing a mountain-searching tiger control medicinal material solution;
(2) Preparing a sample solution of the Kadsura longepedunculata;
(3) And (3) according to a thin-layer chromatography, sucking the sample solution of the Kadsura longepedunculata and the sample solution of the Kadsura longepedunculata to be spotted on the same silica gel G thin-layer plate, developing with a mixed solution of dimethylbenzene and ethyl acetate as a developing agent, airing and checking.
Characteristics of the medicinal materials of the wild tiger: the root is cylindrical, slightly curved, and has few branches. The surface is dark yellow brown to dark brown, has thin longitudinal lines, is seen as a nearly round or oval shaped transverse protuberance in the shape of a keyhole, the stem is cylindrical, the surface is gray brown to tan, the keyhole and the drum Ding Zhuangpi are penetrated, and the medulla is seen in the center of the section. The slicing person is in a bevel cutting sheet or an irregular sheet shape, the leather part is easy to separate from the wood part, the wood part is yellow-white to light yellow, concentric ring patterns are visible, and the pith part is white or hollow. Hard. Light smell and bitter taste. At present, the existing standard does not have an identification method and a quality detection standard aiming at the medicinal materials of the radix polygoni multiflori, which are not beneficial to quality assurance and market specification of the medicinal materials of the radix polygoni multiflori.
The quality detection method for the medicinal materials of the tiger adopts a thin-layer chromatography method, uses a dimethylbenzene-ethyl acetate mixed solution as a developing agent for identification, has good separation effect, round and clear spots, moderate specific shift value and good reproducibility, can effectively identify the medicinal materials of the tiger, and is favorable for quality control and clinical application of the medicinal materials of the tiger.
Further scheme, in the developing agent in the step (3), the volume ratio of the dimethylbenzene to the ethyl acetate is 12-18:1;
Preferably, the volume ratio of xylene to ethyl acetate is 15:1.
In the invention, experiments are carried out on a plurality of developing agents, and the invention discovers that when dimethylbenzene and ethyl acetate with the volume ratio of 12-18:1 are adopted as the developing agents, the separation effect is good, the spots are round and clear, the specific shift value is moderate, and the repeatability is good. The separation effect is best when xylene and ethyl acetate in a volume ratio of 15:1 are used as developing agents.
Further, in step (3), the amount of spotting is 8 to 15. Mu.l, preferably 10 to 15. Mu.l.
The invention discovers that the pattern is clear and the spots are obvious when the sample application amount is 8-15 mu l according to the investigation results of different sample application amounts, and the sample application amount is suitable.
In a further scheme, in the step (3), the glass is developed under the conditions of the temperature of 10-35 ℃ and the relative humidity of 35-90%, and is inspected under an ultraviolet lamp of 365 nm.
The method can be developed under the conditions of 10-35 ℃ and 35-90% of relative humidity, and has good applicability and durability.
In a further scheme, in the step (1), the preparation method of the mountain searching tiger control medicinal material solution comprises the following steps: taking a reference medicinal material of the radix sophorae flavescentis, adding ethanol, carrying out ultrasonic treatment, filtering, evaporating filtrate to dryness, and adding methanol into residues to dissolve the residues to prepare a reference medicinal material solution.
Preferably, 1g of the reference medicinal material of the radix sophorae regulator is taken, 20mL of ethanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, the filtrate is evaporated to dryness, and 1mL of methanol is added into residues to dissolve the residues to be used as a reference medicinal material solution.
In a further scheme, in the step (2), the preparation method of the sample solution of the medicinal material of the Kadsura longepedunculata comprises the following steps: taking a proper amount of powder of the medicinal materials of the radix sophorae flavescentis, adding ethanol, carrying out ultrasonic treatment, filtering, evaporating filtrate to dryness, and adding methanol into residues to dissolve the residues to obtain a sample solution.
Aiming at the preparation methods of the reference substance and the sample, the invention carries out relevant investigation on the types of the extraction solvent and the constant volume solvent, and compares three methods of 65% ethanol extraction-methanol constant volume "," 65% ethanol extraction-65% ethanol constant volume "," ethanol extraction-methanol constant volume ", and the like. As a result, the test sample solution prepared by the method of ethanol extraction and methanol constant volume has the advantages of good solubility, low viscosity, easy sample application and clear spots.
Preferably, 1g of the powder of the radix sophorae regulator is taken, 20ml of ethanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, the filtrate is evaporated to dryness, and 1ml of methanol is added into residues to dissolve the residues to be used as a test solution.
Further, the method comprises measuring extract by hot dipping method in alcohol-soluble extract measuring method, and using 65% ethanol as solvent, not less than 3.0%.
The main chemical components reported in the Kadsura longepedunculata are mostly fat-soluble components, and are mostly separated from low-polarity solvent extracts such as hexane, petroleum ether, chloroform, ethyl acetate and the like. The external prescription preparation for orthopedics department is prepared from one of main raw materials of Kadsura japonica, and 65% ethanol as a percolation extraction solvent. Therefore, the same batch of samples are selected, ethanol and 65% ethanol are used as extraction solvents, extraction effect investigation of a cold leaching method and a hot leaching method is respectively carried out, and comparison test results show that the extract content of the 65% ethanol hot leaching method is highest.
Further aspects also include moisture, total ash, and acid insoluble ash checks;
Preferably, the moisture is no more than 14.0%, the total ash is no more than 5.0%, and the acid insoluble ash is no more than 1.0%.
The second object of the present invention is to provide a quality detection method of a extract or preparation of a Kadsura longepedunculata, comprising:
(1) Preparing a sample solution of a Kadsura longepedunculata extract or preparation;
(2) Preparing a mountain-searching tiger control medicinal material solution;
(3) And carrying out thin-layer identification on the sample solution of the extract or the preparation of the Kadsura longepedunculata and the contrast medicinal material solution of the Kadsura longepedunculata according to the thin-layer chromatography in the quality detection method according to any scheme or combination scheme.
In a further scheme, the preparation of the Qishan tiger is Shuanghu gall ning, and the preparation method of the test solution comprises the following steps:
extracting 20ml of the product with chloroform 20ml of shaking in a separating funnel, separating chloroform solution, evaporating to dryness, and dissolving the residue with 1ml of methanol to obtain sample solution.
Further, the preparation method of the mountain searching tiger control medicinal material solution comprises the following steps: taking 1g of a reference medicinal material of the radix sophorae flavescentis, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 20ml of 55% ethanol into residues to dissolve, placing into a separating funnel, shaking and extracting with 20ml of chloroform, separating chloroform liquid, evaporating to dryness, and adding 1ml of methanol into residues to dissolve to obtain the reference medicinal material solution.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects:
1. In the quality detection method, thin-layer chromatography is adopted, and the mixed solution of dimethylbenzene and ethyl acetate is used as a developing agent for identification, so that the separation effect is good, spots are round and clear, the specific shift value is moderate, the reproducibility is good, the medicinal herb of the radix polygoni cuspidati can be effectively identified, and the quality control and clinical application of the medicinal herb of the radix polygoni cuspidati are facilitated.
2. The invention searches the preparation method of the sample solution and other conditions such as sample application amount in the thin layer chromatography through a large number of experiments, and determines the preparation method and the thin layer chromatography conditions of the optimal sample solution, so that the quality detection method has good durability and good reproducibility, and can effectively identify the medicinal materials of the radix polygoni cuspidati.
3. In addition, the invention further improves the quality detection method of the Qishan tiger extract and the preparation, is beneficial to the quality control of the Qishan tiger preparation, and is especially beneficial to the quality control of the Shuanghu gall Ning preparation.
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. It is evident that the drawings in the following description are only examples, from which other drawings can be obtained by a person skilled in the art without the inventive effort. In the drawings:
FIG. 1 is a thin-layer chromatogram of 10 Xueshanhu medicinal materials in example 1 of the present invention;
FIG. 2 is a thin layer chromatogram of example 2 of the present invention using n-hexane-ethyl acetate-acetic acid (9:3:0.1) as a developing agent;
FIG. 3 is a thin layer chromatogram of example 2 of the present invention using xylene-ethyl acetate (15:1) as the developing agent;
FIG. 4 is a thin layer chromatogram of example 3 of the present invention using method 1;
FIG. 5 is a thin layer chromatogram of example 3 of the present invention using method 2;
FIG. 6 is a thin layer chromatogram of example 3 of the present invention using method 3;
FIG. 7 is a thin layer chromatogram of different spotting amounts in example 4 of the present invention;
FIG. 8 is a thin layer chromatogram under the conditions of group 1 employed in example 5 of the present invention;
FIG. 9 is a thin layer chromatogram under the conditions of group 2 employed in example 5 of the present invention;
FIG. 10 is a thin layer chromatogram under the conditions of group 3 employed in example 5 of the present invention;
FIG. 11 is a thin layer chromatogram under the conditions of group 4 employed in example 5 of the present invention;
FIG. 12 is a thin layer chromatogram under the conditions of group 5 employed in example 5 of the present invention;
FIG. 13 is a thin layer chromatogram under the conditions of group 6 employed in example 5 of the present invention;
FIG. 14 is a thin layer chromatogram under the conditions of set 7 employed in example 5 of the present invention;
FIG. 15 is a thin layer chromatogram under the conditions of group 8 employed in example 5 of the present invention;
FIG. 16 is a thin-layer chromatogram of quality detection of a Shuanghu Zhongtongning preparation in example 7 of the present invention.
It should be noted that these drawings and the written description are not intended to limit the scope of the inventive concept in any way, but to illustrate the inventive concept to those skilled in the art by referring to the specific embodiments.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments will be clearly and completely described with reference to the accompanying drawings in the embodiments of the present invention, and the following embodiments are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
Ling nan Zanthoxylum bungeanum Zanthoxylum austrosinense Huang is a small arbor or shrub, mainly produced in Guangxi Guilin, tian and so on, cangwu, thawed water and so on, in the south of Anhui, zhejiang, jiangxi, fujian, hubei southwest, hunan and Guangdong.
The samples collected in the present invention and the identification results are shown in table 1.
TABLE 1 search for mountain tiger sample information and identification results
Instrument and reagent
Instrument: CAMAG REPROSTAR 3 thin layer chromatography imager (swiss kama); GF-200 analytical balance (japan AND corporation); BUG40-06 ultrasonic cleaner (Shanghai Birenshi Co.).
Reagent: the mountain-searching tiger contrast medicinal material (Chinese food and drug verification institute, lot 121385-201201); thin layer chromatography silica gel G thin layer plate (Qingdao ocean chemical Co., ltd., lot number: 20170808); the organic reagents are all analytically pure; the water was purified (homemade).
Example 1 thin layer identification of mountain-searching tiger medicinal material
(1) Preparing a mountain searching tiger control medicinal material solution:
Taking 1g of a reference medicinal material of the radix sophorae flavescentis, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to prepare a reference medicinal material solution.
(2) Preparing a sample solution of the Kadsura longepedunculata:
Taking 1g of the powder of the medicinal material of the radix sophorae flavescentis to be measured, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a sample solution.
(3) According to thin layer chromatography (China pharmacopoeia 2015 edition four general rule 0502), sucking 10-15 μl of each of the above two solutions, respectively spotting on the same silica gel G thin layer plate, spreading with xylene-ethyl acetate (15:1) as developing agent, spreading distance of 8cm, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
Chromatographic conditions: silica gel G thin layer prefabricated plate, manufacturer: qingdao ocean chemical Co., ltd., lot number: 20170808
Specification of: 10cm by 20cm
Dot-like spotting, spotting amount: 1 and 12 were spotted in an amount of 15. Mu.l, and 1-5, 7-11 were spotted in an amount of 10. Mu.l;
Temperature: 27 ℃; relative humidity: 60 percent of
Developing agent: xylene-ethyl acetate (15:1)
The chromatogram results are shown in FIG. 1, wherein the lanes are: SSH-1,2.SSH-2,3.SSH-3,4.SSH-4,5.SSH-5,6. Control, 7.SSH-6,8.SSH-7,9.SSH-8, 10.SSH-9, 11.SSH-10, 12. Control. The marked A is a yellow fluorescent spot, and the marked B is a green fluorescent spot.
From the results, 2 fluorescence main spots with the same color appear on the positions corresponding to the chromatogram of the reference medicinal material in the chromatogram of the test sample, which indicates that the test sample and the reference medicinal material are the same medicinal material. 10 batches of the Kadsura longepedunculata are inspected according to the method, and fluorescent spots with the same color are displayed on the positions corresponding to the chromatogram of the reference medicinal material in the chromatogram of the test sample.
EXAMPLE 2 investigation of chromatographic conditions
A comparison of two different polarity development systems, n-hexane-ethyl acetate-acetic acid (9:3:0.1) and xylene-ethyl acetate (15:1), was performed using the procedure of example 1.
Chromatographic condition 1:
silica gel G thin layer prefabricated plate, manufacturer: qingdao ocean chemical Co., ltd., lot number: 20170808,
Specification of: 10cm x 10cm
Dot-like spotting, spotting amount: 1 is 15 μl,2-4 is 10 μl; temperature: 28 ℃; relative humidity: 61%
Developing agent: n-hexane-ethyl acetate-acetic acid (9:3:0.1).
The chromatographic results are shown in FIG. 2, wherein 1. The control medicinal material is 2.SSH-1.SSH-2.SSH-4.SSH-3A. Yellow fluorescent spot B. Green fluorescent spot.
Chromatographic condition 2:
Silica gel G thin layer prefabricated plate, manufacturer: qingdao ocean chemical Co., ltd., lot number: 20170808
Specification of: 10cm x 10cm
Dot-like spotting, spotting amount: 1 is 15 μl,2-4 is 10 μl; temperature: 28 ℃; relative humidity: 60 percent of
Developing agent: xylene-ethyl acetate (15:1)
The chromatographic results are shown in FIG. 3, wherein 1. Control medicine 2.SSH-1.SSH-2.SSH-4.SSH-3A. Yellow fluorescent spot B. Green fluorescent spot
Results: through the verification of 10 batches of medicinal materials, the separation effect of dimethylbenzene-ethyl acetate (15:1) is good, spots are round and clear, the specific shift value is moderate, and the repeatability is good.
Example 3 investigation of sample solution preparation methods
The types of the extraction solvent and the constant volume solvent are inspected in a correlation manner, and three methods of 65% ethanol extraction-methanol constant volume "," 65% ethanol extraction-65% ethanol constant volume "," ethanol extraction-methanol constant volume "and the like are compared. The specific conditions are shown in Table 2.
TABLE 2
As a result, the test sample solution prepared by the method of ethanol extraction-methanol constant volume has good solubility, low viscosity, easy sample application and clear spots. And (3) preparing a reference medicinal material solution by using the same method as the reference medicinal material of the Kadsura longepedunculata, and checking the reference medicinal material solution and the sample solution of different batches on the same silica gel G plate, wherein the results are in accordance with the regulations.
Example 4 sample application amount investigation
And (3) examining different sample application amounts of the sample solution and the control medicinal material solution, wherein when the sample application amount is 10-15 mu l, the pattern is clear, the spots are obvious, and the sample application amount is suitable.
Chromatographic conditions: silica gel G thin layer prefabricated plate, manufacturer: qingdao ocean chemical Co., ltd., lot number: 20170808
Specification of: 10cm by 20cm
Dot-shaped sample application; temperature: 31 ℃; relative humidity: 59%
Developing agent: xylene-ethyl acetate (15:1)
The results are shown in fig. 7, wherein:
1-4. Control drug, sample application amount 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
SSH-1, spotting amounts of 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
SSH-2, spotting amounts of 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
SSH-3, spotting amounts of 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
A. yellow fluorescent spot b. Green fluorescent spot.
Example 5 durability test investigation
The unfolding effects of the thin layer plates provided by three factories such as Qingdao ocean chemical factories, national drug groups and MERCK are examined, and the results of the examination of different unfolding temperatures and relative humidity show that the method has good durability.
The thin-layer precast slabs provided by different manufacturers are adopted in the groups 1-3, and the silica gel G thin-layer precast slabs in the same batch of Qingdao ocean chemical industry Co., ltd. Are adopted in the groups 4-8, and the tests are carried out at different unfolding temperatures and relative humidities.
The results show that the thin-layer chromatography identification method provided by different manufacturers is basically consistent with the thin-layer precast slab provided by different manufacturers and under different temperatures and relative humidities, and the method has good durability.
Example 6 other examinations of mountain Tiger medicine
1. The inspection water was measured by a water content measuring method (second method of general rule 0832 of chinese pharmacopoeia 2015 edition).
The water content of 10 batches of the medicinal materials of the radix polygoni multiflori is measured, the results are shown in table 2, wherein the highest value is 12.3%, the lowest value is 6.7%, and the average value is 9.0%, and the water content limit is set to be less than 14.0% because the medicinal materials are affected by the humid climate condition to increase in the transportation and storage processes in consideration of the fact that the main production place of the medicinal materials is the south.
TABLE 3 Table 3
| Sample of | Moisture (%) | Sample of | Moisture (%) |
| SSH-1 | 8.4 | SSH-6 | 7.7 |
| SSH-2 | 12.3 | SSH-7 | 9.0 |
| SSH-3 | 11.1 | SSH-8 | 8.3 |
| SSH-4 | 8.3 | SSH-9 | 9.6 |
| SSH-5 | 6.7 | SSH-10 | 8.9 |
2. Measured according to the total ash assay (chinese pharmacopoeia 2015 edition, division 2302).
The total ash content of 10 batches of samples of this product is measured, and the results are shown in Table 4, wherein the highest value is 4.68%, the lowest value is 0.64%, and the average value is 2.37%, and the total ash content limit is set to be less than 5.0% according to the measurement results.
TABLE 4 Table 4
| Sample of | Total ash (%) | Sample of | Total ash (%) |
| SSH-1 | 2.1 | SSH-6 | 0.64 |
| SSH-2 | 3.18 | SSH-7 | 4.68 |
| SSH-3 | 3.25 | SSH-8 | 0.87 |
| SSH-4 | 2.47 | SSH-9 | 0.68 |
| SSH-5 | 3.83 | SSH-10 | 2.04 |
3. Acid insoluble ash was measured according to the acid insoluble ash assay (chinese pharmacopoeia 2015 edition, division 2302).
The acid-insoluble ash content of 10 batches of samples of this product was measured, and the results are shown in Table 5, wherein the maximum value is 0.79%, the minimum value is 0.10%, and the average value is 0.27%, and the acid-insoluble ash content limit is set to not more than 1.0% according to the measurement results.
TABLE 5
| Sample of | Acid insoluble ash (%) | Sample of | Acid insoluble ash (%) |
| SSH-1 | 0.44 | SSH-6 | 0.11 |
| SSH-2 | 0.27 | SSH-7 | 0.79 |
| SSH-3 | 0.17 | SSH-8 | 0.10 |
| SSH-4 | 0.20 | SSH-9 | 0.13 |
| SSH-5 | 0.11 | SSH-10 | 0.34 |
4. Heavy metals and harmful elements are measured according to lead, cadmium, arsenic, mercury and copper measuring method (four appendices 2321 of China pharmacopoeia 2015 edition).
The heavy metal and harmful elements disclosed by the national formulary committee in the "0212 medicinal materials and decoction pieces verification rule" of the four parts of Chinese pharmacopoeia "2015 to be revised are limited to lead not more than 5mg/kg, cadmium not more than 1mg/kg, arsenic not more than 2mg/kg, mercury not more than 0.2mg/kg and copper not more than 20mg/kg.
Heavy metal and harmful elements are measured on 10 batches of samples of the product, wherein the highest value of lead is 1.51mg/kg, cadmium is 0.350mg/kg, arsenic is 0.210mg/kg, mercury is 0.0170mg/kg, copper is 5.11mg/kg, and the lowest value of lead is 0.28mg/kg, cadmium is 0.033mg/kg, arsenic is not detected, mercury is not detected, and copper is 1.70mg/kg. The test results of the samples of a plurality of batches show that the content of heavy metals and harmful elements in the Kadsura longepedunculata is low.
5. Extract of plant
The main chemical components reported in the Kadsura longepedunculata are mostly fat-soluble components, and are mostly separated from low-polarity solvent extracts such as hexane, petroleum ether, chloroform, ethyl acetate and the like. The external prescription preparation for orthopedics department is prepared from one of main raw materials of Kadsura japonica, and 65% ethanol as a percolation extraction solvent. Therefore, the same batch of samples are selected, ethanol and 65% ethanol are used as extraction solvents, extraction effects of a cold leaching method and a hot leaching method are respectively examined, and comparison test results show that the extract content of the 65% ethanol hot leaching method is the highest, and the results are shown in Table 6. It was thus determined that the alcohol-soluble extract was assayed by hot dip method under the term "alcohol-soluble extract assay" (rule 2201 of the fourth edition of chinese pharmacopoeia 2015) using 65% ethanol as solvent.
TABLE 6
| Solvent extraction process | Extract (%) |
| Ethanol hot dip process | 4.2 |
| Hot dipping method with 65% ethanol | 6.5 |
| 65% Ethanol cold soaking method | 4.8 |
The extract was measured on 10 batches of samples of this product, and the results are shown in Table 7, wherein the maximum value is 11.0%, the minimum value is 3.6%, and the average value is 6.4%, and the extract limit is set to not less than 3.0% in consideration of the difference in sources of the medicinal materials.
TABLE 7
| Sample of | Extract mean (%) | Sample of | Extract mean (%) |
| SSH-1 | 6.5 | SSH-6 | 3.6 |
| SSH-2 | 9.4 | SSH-7 | 5.6 |
| SSH-3 | 5.9 | SSH-8 | 4.4 |
| SSH-4 | 8.4 | SSH-9 | 4.4 |
| SSH-5 | 11.0 | SSH-10 | 4.7 |
Example 7 quality detection method of Qishan tiger preparation
The Shuanghu gall ning is a Chinese patent medicine prepared from the Chinese medicinal materials of Chinese forest frog, azalea root, raw aconite root, raw wild aconite root, raw arisaema tuber, raw pinellia tuber, camphor and menthol, and can be prepared by referring to the existing method.
The embodiment provides a quality detection method of Shuanghu gall ning, which comprises the following specific steps:
(1) Preparing a mountain searching tiger control medicinal material solution:
Taking 1g of a reference medicinal material of the radix sophorae flavescentis, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 20ml of 55% ethanol into residues to dissolve, placing into a separating funnel, shaking and extracting with 20ml of chloroform, separating chloroform liquid, evaporating to dryness, and adding 1ml of methanol into residues to dissolve to obtain the reference medicinal material solution.
(2) Preparing a test solution of the Shuanghu gall ning:
taking 20ml of the Shuanghu gall to be measured, placing the Shuanghu gall to be measured into a separating funnel, shaking and extracting with 20ml of chloroform, separating to obtain chloroform liquid, evaporating to dryness, and adding 1ml of methanol into residues to dissolve the residues to be used as a test sample solution.
(3) Negative control solutions were prepared that lacked the tiger of the search mountain:
Taking 20ml of a negative control sample lacking the Kadsura longepedunculata, placing in a separating funnel, shaking and extracting with 20ml of chloroform, separating to obtain chloroform solution, evaporating to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a negative control solution.
The negative control sample lacking the wild tiger is prepared from root of rhododendron, raw radix aconiti kusnezoffii, raw rhizoma arisaematis, raw pinellia ternate, camphor and menthol, and compared with the test sample of the Shuanghu gall, the negative control sample lacking the wild tiger is not added with the wild tiger raw medicinal materials, and the prescription dosage and the preparation method of the other medicinal materials are the same as those of the test sample of the Shuanghu gall.
(4) According to thin layer chromatography (China pharmacopoeia 2015 edition four general rule 0502), sucking 3-9 μl of each of the above three solutions, respectively spotting on the same silica gel G thin layer plate, spreading with xylene-ethyl acetate (15:1) as developing agent, spreading distance of 8cm, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
(5) Chromatographic conditions: silica gel G thin layer prefabricated plate, manufacturer: national drug group chemical reagent Co., ltd., lot number: 20171123 specification: 10cm by 20cm
(6) Dot-like spotting, spotting amount: 1. 3-5 sample application amount is 3 μl, and 2 sample application amount is 9 μl;
(7) Temperature: 21 ℃; relative humidity: 78%
(8) Developing agent: xylene-ethyl acetate (15:1)
(9) The chromatogram results are shown in fig. 16, wherein the lanes are: 1. negative control, 2. Control drug, 3.SHZTN-1,4.SHZTN-2,5.SHZTN-3. Wherein SHZTN-1, SHZTN-2 and SHZTN-3 are 3 batches of double tiger gall medicine samples, and the marked A is a green fluorescent spot.
(10) As can be seen from the chromatogram results, in the chromatogram of the test sample of the Shuanghu gall ning, 1 fluorescence main spot with the same color is displayed at the position corresponding to the chromatogram of the reference medicinal material, and the negative reference is undisturbed, so that the characteristic components are derived from the Qishan tiger. 3 batches of Shuanghu gall ning are inspected according to the method, and fluorescent spots with the same color are displayed on the positions corresponding to the chromatogram of the reference medicinal material in the chromatogram of the test sample.
The foregoing description is only illustrative of the preferred embodiment of the present invention, and is not to be construed as limiting the invention, but is to be construed as limiting the invention to any and all simple modifications, equivalent variations and adaptations of the embodiments described above, which are within the scope of the invention, may be made by those skilled in the art without departing from the scope of the invention.
Claims (6)
1. The quality detection method of the medicinal material of the radix polygoni multiflori is characterized by comprising the following steps of:
(1) Preparing a mountain searching tiger control medicinal material solution: taking 1g of a reference medicinal material of the radix sophorae flavescentis, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to prepare a reference medicinal material solution;
(2) Preparing a sample solution of the Kadsura longepedunculata: taking 1g of the powder of the Chinese medicinal materials of the Japanese climbing fern, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a sample solution;
(3) According to thin layer chromatography, absorbing 10-15 μl of each of the control medicinal material solution and the test sample solution of the Kadsura longepedunculata, spotting on the same silica gel G thin layer plate, spreading with mixed solution of xylene and ethyl acetate with volume ratio of 15:1 as developing agent at 10-35deg.C and relative humidity of 35-90%, air drying, and inspecting under 365nm ultraviolet lamp.
2. The method for detecting the quality of a medicinal material of a mountain-hu as claimed in claim 1, further comprising the step of measuring the extract, according to a hot dipping method in an alcohol-soluble extract measuring method, using 65% ethanol as a solvent, not less than 3.0%.
3. The quality detection method of a medicinal material of a radix et rhizoma recited in claim 1 or 2, further comprising checking for moisture, total ash, and acid insoluble ash.
4. The method for detecting the quality of a medicinal material of the Chinese yam according to claim 3, wherein the water content is not more than 14.0%; the total ash content is not more than 5.0% and the acid insoluble ash content is not more than 1.0%.
5. A quality detection method of a Qishan tiger extract or preparation is characterized by comprising the following steps:
(1) Preparing a sample solution of a Kadsura longepedunculata extract or preparation;
(2) Preparing a mountain-searching tiger control medicinal material solution;
(3) Thin layer chromatography in the quality control method according to any one of claims 1 to 4 is used for thin layer identification of sample solution of herba Sagittariae Sagittifoliae extract or preparation and herba Sagittariae Sagittifoliae control medicinal material solution.
6. The quality inspection method according to claim 5, wherein the preparation of the Qihan tiger is Shuanghu gall ning, and the preparation method of the test solution comprises the following steps: placing 20ml of the product in a separating funnel, shaking and extracting with 20ml of chloroform, separating chloroform solution, evaporating to dryness, and dissolving the residue with 1ml of methanol to obtain sample solution;
The preparation method of the mountain-searching tiger control medicinal material solution comprises the following steps: taking 1g of a reference medicinal material of the radix sophorae flavescentis, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 20ml of 55% ethanol into residues to dissolve, placing into a separating funnel, shaking and extracting with 20ml of chloroform, separating chloroform liquid, evaporating to dryness, and adding 1ml of methanol into residues to dissolve to obtain the reference medicinal material solution.
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