CN115201398A - Quality detection method for medicinal material of caulis et folium piperis longi, extract and preparation thereof - Google Patents
Quality detection method for medicinal material of caulis et folium piperis longi, extract and preparation thereof Download PDFInfo
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- G—PHYSICS
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- 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
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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
- G01N1/34—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
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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
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Abstract
The invention discloses a quality detection method of a Scopolia sinensis Roxb medicinal material and an extract and a preparation thereof, and the quality detection method of the Scopolia sinensis Roxb medicinal material comprises the following steps: (1) preparing a solution of the drug for controlling the saxifraga stolonifera; (2) preparing a solution of the test sample of the tiger searchloes; (3) Dropping control solution and sample solution of radix Seu caulis Parthenocissi Tricuspidatae on the same silica gel G thin layer plate by thin layer chromatography, developing with mixed solution of xylene and ethyl acetate as developing agent, air drying, and inspecting. In the quality detection method, the thin-layer chromatography is adopted, and the xylene-ethyl acetate mixed solution is used as a developing solvent for identification, so that the separation effect is good, the spots are round and clear, the specific shift value is moderate, the reproducibility is good, the radix et caulis Opuntiae Dillenii medicinal material, the extract and the preparation thereof can be effectively identified, and the quality control and the clinical application of the radix et caulis Opuntiae Dillenii medicinal material, the extract and the preparation thereof are facilitated.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a quality detection method for a drug of caulis et folium piperis longi, an extract of the drug and a preparation of the drug.
Background
The Scopolia sinensis is derived from Zanthoxylum australense Huang of Rutaceae, is a folk common medicine, is a medicinal material commonly used by Yao medicine and herbal medicine, and has the effects of dispelling pathogenic wind, removing toxic substances, removing blood stasis, relieving swelling, promoting qi circulation and relieving pain; it can be used for treating venomous snake bite, rheumatalgia, gastralgia, toothache, sprain, contusion, fracture, and common cold.
The Scopolia sinensis is a main raw material of Shuanghu Zhongtongning (tincture), is collected in the appendix of Guangxi traditional Chinese medicine standards and traditional Chinese medicine patent preparations of the Ministry of health, has no collection of local and national traditional Chinese medicine quality standards, and belongs to an inverted hanging variety. The Bingshan tiger is recorded in the writings of Chinese plant record, chinese materia Medica, modern compendium of materia Medica, chinese herbal medicine original chromatogram of bone injury, selection of Guangxi materia Medica and the like, and the related contents of original plants, geographical distribution, medicinal value and the like are briefly described, but medicinal parts are not consistent, and roots, stems, root barks and stem barks are all used. At present, the existing standard does not have an identification method and a quality detection standard aiming at the medicines of the Scopolia crassipes, and is not beneficial to the quality assurance and the market specification of the medicine of the Scopolia crassipes.
The present invention has been made in view of this situation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a quality detection method for the medicinal material of the tiger, the extract thereof and the preparation thereof. The thin-layer chromatography provided by the invention can effectively identify the drug substance of the Scopolia sinensis, and is beneficial to the quality control and clinical application of the drug substance of the Scopolia sinensis.
In order to solve the technical problems, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a quality detection method of the drug Scopolia sinensis, which comprises the following steps:
(1) Preparing a solution of the Scopolia sinensis control medicinal material;
(2) Preparing a solution of the test sample of the tiger hunters;
(3) Dropping control solution and sample solution of radix Seu caulis Parthenocissi Tricuspidatae on the same silica gel G thin layer plate by thin layer chromatography, developing with mixed solution of xylene and ethyl acetate as developing agent, air drying, and inspecting.
The properties of the medicinal materials of the tiger: the root is cylindrical, slightly curved, and has few branches. The surface is dark yellowish brown to dark brown, has fine longitudinal lines, can be seen as nearly circular or elliptical skin hole-like transverse protrusions, the stem is cylindrical, the surface is grey brown to dark brown, and has skin holes and tuba shaped skin thorn, and the center of the cross section can be seen as a medulla part. The sliced piece is in the form of oblique slice or irregular slice, the bark part is easily separated from the wood part, the wood part is yellow white to yellowish, concentric ring lines can be seen, and the medulla part is white or hollow. Is hard and hard. Light smell, bitter taste. At present, the existing standard does not have an identification method and a quality detection standard for the drug Scopolia sinensis, which are not beneficial to the quality assurance and the market specification of the drug Scopolia sinensis.
The invention provides a quality detection method of a Scopolia sinensis Roxb medicinal material, which adopts thin-layer chromatography and takes a dimethylbenzene-ethyl acetate mixed solution as a developing solvent for identification, has good separation effect, round and clear spots, moderate specific shift value and good reproducibility, can effectively identify the Scopolia sinensis Roxb medicinal material, and is beneficial to quality control and clinical application of the Scopolia sinensis Roxb medicinal material.
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, a plurality of developing agents are tested, and the results show that when dimethylbenzene and ethyl acetate with the volume ratio of 12-18: 1 are used as the developing agents, the separation effect is good, spots are round and clear, the specific displacement value is moderate, and the reproducibility is good. When xylene and ethyl acetate in a volume ratio of 15:1 are used as developing agents, the separation effect is best.
In a further embodiment, in step (3), the amount of spot is 8 to 15. Mu.l, preferably 10 to 15. Mu.l.
According to the invention, the investigation result of different sample amounts shows that when the sample amount is 8-15 mu l, the map is clear, the spots are obvious, and the sample amount is a proper sample amount.
In the further scheme, in the step (3), the film is developed under the conditions that the temperature is 10-35 ℃ and the relative humidity is 35-90 percent, and the film is inspected under a 365nm ultraviolet lamp.
The method can be developed under the conditions of 10-35 ℃ of temperature 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 solution of the drug for controlling the tiger comprises the following steps: adding ethanol into control medicinal material of caulis et folium piperis longi, ultrasonic treating, filtering, evaporating filtrate, dissolving residue with methanol, and making into control medicinal solution.
Preferably, 1g of the control drug of the saxifraga crassocarpa is taken, 20mL of ethanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, filtrate is evaporated to dryness, and 1mL of methanol is added to residues to dissolve the residues to be used as a control drug solution.
In a further scheme, in the step (2), the preparation method of the test solution of the drug of the Scopolia sinensis comprises the following steps: taking appropriate amount of radix Scopoliae sinensis powder, adding ethanol, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue with methanol to obtain sample solution.
Aiming at the preparation methods of the reference substance and the test substance, the invention carries out related 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. The result shows that the solution of the test sample prepared by the method of ethanol extraction-methanol constant volume has good solubility, low viscosity, easy sample application and clear spots.
Preferably, 1g of the medicinal material powder of the caulis et folium piperis longi is taken, 20ml of ethanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, 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 comprises extract determination, which is determined by hot dipping method in alcohol-soluble extract determination method, using 65% ethanol as solvent, and is not less than 3.0%.
The major chemical components reported in the saxifraga crassosii are fat-soluble components, and are mostly separated from low-polarity solvent extract such as hexane, petroleum ether, chloroform, ethyl acetate and the like. The externally applied preparation 'Shuanghu Zhongtongning' in orthopedics and traumatology takes the tiger moseri as one of the main raw materials and adopts 65 percent ethanol as a percolation extraction solvent. Therefore, the same batch of samples are selected, ethanol and 65% ethanol are used as extraction solvents, the cold soaking method and the hot soaking method are respectively used for examining the extraction effect, and the comparative test result shows that the extract content of the 65% ethanol hot soaking method is the highest.
Further, the method also comprises the steps of checking moisture, total ash and acid insoluble ash;
preferably, the moisture is not more than 14.0%, the total ash is not more than 5.0%, and the acid-insoluble ash is not more than 1.0%.
The second purpose of the invention is to provide a quality detection method of the extract or the preparation of the tiger searchloes, which comprises the following steps:
(1) Preparing a test solution of the extract or preparation of the tiger moschata;
(2) Preparing a solution of the drug for controlling the tiger;
(3) And (3) performing thin-layer identification on the test solution of the anemone rivularis extract or the preparation and the control solution of the anemone rivularis according to the thin-layer chromatography in the quality detection method of any scheme or the combination scheme.
In a further scheme, the preparation of the radix Seu caulis Parthenocissi Tricuspidatae is Shuanghuzhongtongning, and the preparation method of the test solution comprises the following steps:
collecting 20ml of the product, placing in a separating funnel, extracting with chloroform 20ml under shaking, collecting chloroform solution, evaporating to dryness, and dissolving the residue with 1ml of methanol to obtain sample solution.
In a further scheme, the preparation method of the solution of the drug for controlling the tiger comprises the following steps: collecting control drug of caulis et folium piperis longi 1g, adding ethanol 20ml, ultrasonic treating for 30 min, filtering, evaporating filtrate to dryness, dissolving residue with 55% ethanol 20ml, placing in separating funnel, extracting with chloroform 20ml under shaking, collecting chloroform solution, evaporating to dryness, dissolving residue with methanol 1ml, and making into control drug solution.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. in the quality detection method, the thin-layer chromatography is adopted, and the xylene-ethyl acetate mixed solution is used as a developing solvent for identification, so that the separation effect is good, the spots are round and clear, the specific shift value is moderate, the reproducibility is good, the medicine material of the Ranunculus ternatus can be effectively identified, and the quality control and the clinical application of the medicine material of the Ranunculus ternatus are facilitated.
2. The invention searches other conditions such as the preparation method of the test solution, the spot sample amount in the thin-layer chromatography and the like through a large number of experiments, and determines the most suitable preparation method and thin-layer chromatography conditions of the test solution, so that the quality detection method has good durability and good reproducibility, and can effectively identify the drug substance of the tiger.
3. In addition, the invention further improves the quality detection method of the extract and the preparation of the Scopolia sinensis Roxb, is beneficial to the quality control of the Scopolia sinensis Roxb preparation, and is particularly beneficial to the quality control of the Shuanghutongning preparation.
The following describes 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, 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 without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a thin layer chromatogram of 10 Tiger species in example 1 of the present invention;
FIG. 2 is a thin layer chromatogram using n-hexane-ethyl acetate-acetic acid (9: 3: 0.1) as a developing solvent in example 2 of the present invention;
FIG. 3 is a thin layer chromatogram using xylene-ethyl acetate (15: 1) as a developing solvent in example 2 of the present invention;
FIG. 4 is a thin layer chromatogram obtained by the method 1 in example 3 of the present invention;
FIG. 5 is a thin layer chromatogram obtained by the method 2 in example 3 of the present invention;
FIG. 6 is a thin layer chromatogram of example 3 according to the present invention;
FIG. 7 is a thin layer chromatogram of different spot sizes in example 4 of the present invention;
FIG. 8 is a thin layer chromatogram under the conditions of group 1 used in example 5 of the present invention;
FIG. 9 is a thin layer chromatogram under the conditions of group 2 used in example 5 of the present invention;
FIG. 10 is a thin layer chromatogram under the conditions of group 3 used in example 5 of the present invention;
FIG. 11 is a thin layer chromatogram under the conditions of group 4 used in example 5 of the present invention;
FIG. 12 is a thin layer chromatogram under the conditions of group 5 used in example 5 of the present invention;
FIG. 13 is a thin layer chromatogram under the conditions of group 6 used in example 5 of the present invention;
FIG. 14 is a thin layer chromatogram under the conditions of group 7 used in example 5 of the present invention;
FIG. 15 is a thin layer chromatogram under the conditions of group 8 used in example 5 of the present invention;
fig. 16 is a thin layer chromatogram for quality detection of the Shuanghu Zhongtongning preparation in example 7 of the invention.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
Zanthoxylum bungeanum zang, which is a small arbor or shrub, is mainly produced in Guangxi Guilin, tian and other places, cocklebur, melted water and other places, the south of Anhui, zhejiang, jiangxi, fujian, the southwest of Hubei, hunan and the northern of Guangdong.
The samples collected and the results of the identification in the present invention are shown in Table 1.
TABLE 1 Saisha sample information and identification results
Instruments and reagents
The instrument comprises the following steps: CAMAG REPROSTAR 3 thin layer chromatography imager (Switzerland Karma); GF-200 analytical balance (Japan AND Co.); BUG40-06 ultrasonic cleaner (Shanghai Binten Co.).
Reagent: caulis et folium piperis longi reference medicinal material (China institute for food and drug inspection, lot No. 121385-201201); thin layer chromatography silica gel G thin layer plate (Qingdao ocean chemical Co., ltd., batch No. 20170808); all the organic reagents are analytically pure; the water is purified water (self-made).
Example 1 thin layer identification of Scopolia sinensis
(1) Preparing a solution of the tiger huntingh control medicinal materials:
collecting control medicinal material 1g, adding ethanol 20ml, ultrasonic treating for 30 min, filtering, evaporating filtrate, dissolving residue with methanol 1ml, and making into control medicinal material solution.
(2) Preparing a solution of the test sample of the Scopolia crassipes:
taking 1g of the powder of the medicinal material of the caulis et folium piperis longi to be detected, 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) Performing thin layer chromatography (0502 of the four parts of the pharmacopoeia 2015 edition) test, sucking 10-15 μ l of the above two solutions respectively, dropping on the same silica gel G thin layer plate, developing with xylene-ethyl acetate (15: 1) as developing agent, spreading for 8cm, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
Chromatographic conditions are as follows: silica gel G thin-layer precast slab, manufacturer: qingdao ocean chemical Co., ltd, batch number: 20170808
Specification: 10cm x 20cm
Dot spotting, spot amount: the spotting amount of 1 and 12 is 15. Mu.l, and the spotting amount of 1-5, 7-11 is 10. Mu.l;
temperature: 27 ℃; relative humidity: 60 percent of
Developing agent: xylene-ethyl acetate (15
The chromatogram results are shown in fig. 1, wherein the lanes are: 1.SSH-1,2.SSH-2,3.SSH-3,4.SSH-4,5.SSH-5,6, control drug, 7.SSH-6,8.SSH-7,9.SSH-8, 10.SSH-9, 11.SSH-10, 12 control drug. The label A is yellow fluorescent spot and B is green fluorescent spot.
As can be seen from the results, 2 main fluorescent spots with the same color are displayed on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference materials, which indicates that the test solution and the reference material are the same materials. The 10 batches of the Selaginella crassifolia are examined by the method, and fluorescent spots with the same color are displayed on the chromatogram of the test solution at the positions corresponding to the chromatogram of the reference medicinal material.
EXAMPLE 2 examination of chromatographic conditions
Using the method of example 1, two different polarity development systems of n-hexane-ethyl acetate-acetic acid (9.
Chromatographic conditions 1:
silica gel G thin-layer precast slab, manufacturer: qingdao ocean chemical Co., ltd, batch number: 20170808,
specification: 10cm x 10cm
Dot spotting, spot amount: 1 is 15 mul, 2-4 is 10 mul; temperature: 28 ℃; relative humidity: 61 percent of
Developing agent: n-hexane-ethyl acetate-acetic acid (9.
The chromatogram results are shown in FIG. 2, wherein 1, 2.SSH-1, SSH-2, SSH-3A, yellow fluorescent spot B, green fluorescent spot of the control drug.
Chromatographic conditions 2:
silica gel G thin-layer precast slab, manufacturer: qingdao ocean chemical Co., ltd, batch number: 20170808
Specification: 10cm x 10cm
Dot spotting, spot amount: 1 is 15 mul, 2-4 is 10 mul; temperature: 28 ℃; relative humidity: 60 percent of
Developing agent: xylene-ethyl acetate (15
The chromatogram result is shown in FIG. 3, wherein 1, 2.SSH-1.SSH-2.SSH-3A, yellow fluorescent spot B, green fluorescent spot of the control drug
As a result: proved by 10 batches of medicinal materials, the dimethylbenzene-ethyl acetate (15).
EXAMPLE 3 examination of the method of preparing a test solution
The types of the extraction solvent and the constant volume solvent are relatively investigated, and the 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. Specific conditions are shown in table 2.
TABLE 2
As a result, the test solution prepared by the method of ethanol extraction-methanol constant volume has good solubility, low viscosity, easy sample application and clear spots. Preparing a control medicinal material solution from the caulis et folium piperis longi control medicinal material by the same method, and spotting the control medicinal material solution and different batches of test sample solutions on the same silica gel G plate for inspection, wherein the results are all in accordance with the regulations.
Example 4 spotting amount investigation
And (3) carrying out different point sample amount inspection on the test solution and the reference medicinal material solution, and obtaining the result that when the point sample amount is 10-15 mu l, the map is clear, the spots are obvious, and the point sample amount is the proper point sample amount.
Chromatographic conditions are as follows: silica gel G thin-layer precast slab, manufacturer: qingdao ocean chemical Co., ltd, lot number: 20170808
Specification: 10cm x 20cm
Dot-like spotting; temperature: 31 ℃; relative humidity: 59 percent of
Developing agent: xylene-ethyl acetate (15
The results are shown in FIG. 7, where:
1-4 reference medicinal materials with sample amount of 5 μ l, 10 μ l, 15 μ l, 20 μ l
SSH-1, sample size 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
SSH-2, spot sizes of 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
SSH-3, spot size 5. Mu.l, 10. Mu.l, 15. Mu.l, 20. Mu.l
A. Yellow fluorescent spot b.
EXAMPLE 5 durability test examination
The development effects of the thin-layer plates provided by three factories such as Qingdao ocean chemical factories, national drug groups, MERCK and the like are investigated, different development temperatures and relative humidities are investigated, and the results show that the durability of the method is good.
The groups 1 to 3 adopt thin-layer precast slabs provided by different manufacturers, and the groups 4 to 8 all adopt silica gel G thin-layer precast slabs of the same batch of Qingdao ocean chemical industry Co., ltd, and tests are carried out at different development temperatures and relative humidities.
The results show that the results of the thin-layer chromatography identification method are basically consistent by adopting the thin-layer prefabricated plates provided by different manufacturers and under different temperatures and relative humidities, and the method has good durability.
Example 6 other examinations of Saxifraga herbs
1. The water content was measured by a water content measuring method (0832 second method in the fourth pharmacopoeia 2015 edition).
The results of the moisture determination of 10 samples of the medicinal material of the tiger were shown in table 2, wherein the highest value was 12.3%, the lowest value was 6.7% and the average value was 9.0%, and the moisture limit was determined to be not more than 14.0% considering that the main production area of the product was south and the medicinal material was affected by humid climatic conditions during transportation and storage.
TABLE 3
| Sample (I) | Moisture (%) | Sample (I) | 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. The measurement was carried out according to the total ash measurement method (the four-part general rule 2302 of the Chinese pharmacopoeia 2015 edition).
The results of total ash measurements on 10 samples of this product are shown in Table 4, in which the maximum value is 4.68%, the minimum value is 0.64%, and the average value is 2.37%, and the total ash limit is defined as not exceeding 5.0% according to the measurement results.
TABLE 4
| Sample(s) | Total ash (%) | Sample (I) | 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. The acid-insoluble ash is measured by the acid-insoluble ash measurement method (the four-part general rule 2302 of the Chinese pharmacopoeia 2015 edition).
The results of the measurement of acid-insoluble ash on 10 samples of this product are shown in Table 5, in which the maximum value is 0.79%, the minimum value is 0.10%, and the average value is 0.27%, and the limit of acid-insoluble ash is defined as not exceeding 1.0% according to the measurement results.
TABLE 5
| Sample (I) | Acid-insoluble ash (%) | Sample (I) | 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 the method for measuring lead, cadmium, arsenic, mercury and copper (appendix 2321 in the fourth part of the 2015 edition of Chinese pharmacopoeia).
The limit of heavy metals and harmful elements disclosed in the general rules of the verification of 0212 medicinal materials and decoction pieces in the fourth part 2015 of the Chinese pharmacopoeia to be revised by the State Committee of pharmacopoeia is that lead is less than 5mg/kg, cadmium is less than 1mg/kg, arsenic is less than 2mg/kg, mercury is less than 0.2mg/kg and copper is less than 20mg/kg.
The heavy metal and harmful element measurement is carried out on 10 batches of samples of the product, wherein the highest value is 1.51mg/kg of lead, 0.350mg/kg of cadmium, 0.210mg/kg of arsenic, 0.0170mg/kg of mercury and 5.11mg/kg of copper, and the lowest value is 0.28mg/kg of lead, 0.033mg/kg of cadmium, no arsenic detection, no mercury detection and 1.70mg/kg of copper. The inspection results of multiple batches of samples show that the contents of heavy metals and harmful elements in the tigers are low.
5. Extract of plant
The main chemical components reported by the saxifrage are fat-soluble components, and are mostly separated from low-polarity solvent extraction liquid such as hexane, petroleum ether, chloroform, ethyl acetate and the like. The externally applied preparation 'Shuanghu Zhongtongning' in orthopedics and traumatology takes the tiger moseri as one of the main raw materials and adopts 65 percent 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 soaking method and extraction effect investigation of a hot soaking method are respectively carried out, and a comparison test result shows that the extract content of the 65% ethanol hot soaking method is the highest, and the result is shown in table 6. Therefore, it was confirmed that the measurement was carried out by a hot dipping method under the item of alcohol-soluble extract measurement method (the four-part rule 2201 of the Chinese pharmacopoeia 2015 edition) using 65% ethanol as a solvent.
TABLE 6
| Solvent extraction process | Extract (%) |
| Hot dipping method of ethanol | 4.2 |
| Hot dipping in 65% ethanol | 6.5 |
| Cold soaking method with 65% ethanol | 4.8 |
Extract test on 10 samples of the product has the results 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 not less than 3.0% in consideration of the source difference of medicinal materials.
TABLE 7
| Sample (I) | Extract mean (%) | Sample (I) | 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 testing method of Tiger Saussureae preparation
The Shuanghutongyangning is a Chinese patent medicine prepared from radix anemones Raddeanae, radix Rhododendri Anthopogonidis, radix Aconiti Kusnezoffii, rhizoma arisaematis, rhizoma Pinelliae, camphora and Mentholum, and can be prepared by the existing method.
The embodiment provides a quality detection method of Shuanghutongning, which comprises the following specific steps:
(1) Preparing a solution of the tiger huntingh control medicinal materials:
collecting control drug of caulis et folium piperis longi 1g, adding ethanol 20ml, ultrasonic treating for 30 min, filtering, evaporating filtrate to dryness, dissolving residue with 55% ethanol 20ml, placing in separating funnel, extracting with chloroform 20ml under shaking, collecting chloroform solution, evaporating to dryness, dissolving residue with methanol 1ml, and making into control drug solution.
(2) Preparing a test solution of Shuanghu gall powder:
taking 20ml of the double-tiger pain relieving medicine to be detected, placing the medicine in a separating funnel, shaking and extracting by using 20ml of trichloromethane, separating trichloromethane liquid, evaporating to dryness, and adding 1ml of methanol into residues to dissolve the residues to be used as a test solution.
(3) Negative control solutions lacking saxifraga crassifolia were prepared:
taking 20ml of negative control sample lacking caulis et folium piperis longi, placing in a separating funnel, extracting with chloroform 20ml under shaking, collecting chloroform solution, evaporating to dryness, and dissolving residue with 1ml of methanol to obtain negative control solution.
The negative control sample lacking the Scopolia sinensis is prepared from the root of Rhododendron dauricum, the raw radix Aconiti Kusnezoffii, the raw rhizoma arisaematis, the raw pinellia ternate, the camphor and the menthol, compared with the Shuanghu Zhongtongning test sample, the Scopolia sinensis raw medicinal materials are not added, and the prescription dosage and the preparation method of other medicinal materials are the same as those of the Shuanghu Zhongtongning test sample.
(4) Performing thin layer chromatography (0502 of the four parts of the pharmacopoeia 2015 edition) test, sucking 3-9 μ l of the above three solutions, respectively dropping on the same silica gel G thin layer plate, developing with xylene-ethyl acetate (15: 1) as developing agent, spreading for 8cm, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
(5) Chromatographic conditions are as follows: silica gel G thin-layer precast slab, manufacturer: national pharmaceutical group chemical reagents limited, batch number: 20171123 specification: 10cm x 20cm
(6) Dot spotting, spot amount: 1. the sample application amount of 3-5 is 3 mul, and the sample application amount of 2 is 9 mul;
(7) Temperature: 21 ℃; relative humidity: 78 percent of
(8) Developing agent: xylene-ethyl acetate (15
(9) The chromatogram results are shown in fig. 16, in which 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 Huzhongtongning samples, and the part marked A is a green fluorescent spot.
(10) From the chromatogram results, it can be seen that 1 main fluorescent spot with the same color is displayed on the corresponding position of the chromatogram of the test sample of Shuanghutongning, and the negative control has no interference, which indicates that the characteristic component is from the Scopolia sinensis. The 3 batches of Shuanghutongning are tested according to the method, and fluorescent spots with the same color are displayed on the chromatogram of the test solution at the positions corresponding to the chromatogram of the reference solution.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A quality detection method of the drug Scopolia sinensis is characterized by comprising the following steps:
(1) Preparing a solution of the drug for controlling the tiger;
(2) Preparing a solution of the test sample of the tiger hunters;
(3) Dropping control solution and sample solution of radix Seu caulis Parthenocissi Tricuspidatae on the same silica gel G thin layer plate by thin layer chromatography, developing with mixed solution of xylene and ethyl acetate as developing agent, air drying, and inspecting.
2. The method for detecting the quality of the Scopolia sinensis Roxb medicinal material as claimed in claim 1, wherein in the developing solvent of step (3), the volume ratio of xylene to ethyl acetate is 12-18: 1;
preferably, the volume ratio of xylene to ethyl acetate is 15: 1.
3. The method for detecting the quality of the Scopolia sinensis Roxb medicinal material as claimed in claim 1 or 2, wherein in step (3), the amount of spotting is 8-15 μ l; preferably 10-15. Mu.l.
4. The method according to any one of claims 1 to 3, wherein in step (3), the product is developed at a temperature of 10-35 deg.C and a relative humidity of 35-90%, and inspected under 365nm ultraviolet light.
5. The method for detecting the quality of the drug substance of the Scopolia sinensis as claimed in any one of claims 1 to 4, wherein in the step (1), the preparation method of the solution of the drug substance of the Scopolia sinensis comprises: collecting caulis et folium piperis longi control, adding ethanol, ultrasonic treating, filtering, evaporating filtrate to dryness, and dissolving residue with methanol to obtain caulis et folium piperis longi control solution;
preferably, 1g of the control drug of the Scopolia sinensis is taken, 20mL of ethanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, filtrate is evaporated to dryness, and 1mL of methanol is added to residues to dissolve the residues to obtain the solution of the control drug of the Scopolia sinensis.
6. The method for detecting the quality of the Scopolia sinensis Roxb medicinal material according to any one of claims 1-5, wherein the preparation method of the Scopolia sinensis Roxb medicinal material test solution in the step (2) comprises: taking appropriate amount of radix Scopoliae sinensis powder, adding ethanol, ultrasonic treating, filtering, evaporating filtrate, and dissolving residue with methanol to obtain sample solution;
preferably, 1g of the medicinal material powder of the caulis et folium piperis longi is taken, 20ml of ethanol is added, ultrasonic treatment is carried out for 30 minutes, filtration is carried out, filtrate is evaporated to dryness, and 1ml of methanol is added into residues to dissolve the residues to be used as a test solution.
7. The method for detecting the quality of the Tiger duct herb according to any one of claims 1 to 6, further comprising the step of measuring the extract by hot dipping in an alcohol-soluble extract measuring method using 65% ethanol as a solvent, which is not less than 3.0%.
8. The method for detecting the quality of the Scopolia sinensis Rehd as claimed in any one of claims 1 to 7, further comprising the steps of examining moisture, total ash and acid-insoluble ash;
preferably, the moisture content does not exceed 14.0%; the total ash content is not more than 5.0%, and the acid insoluble ash content is not more than 1.0%.
9. A quality detection method of the Tilapia lappa extract or the preparation is characterized by comprising the following steps:
(1) Preparing a test solution of the extract or the preparation of the tiger huntington;
(2) Preparing a solution of the drug for controlling the tiger;
(3) The quality control method according to any one of claims 1-8, wherein thin-layer chromatography is used for thin-layer identification of the solution of the extract or preparation of Scopolia sinensis Roxb.
10. The quality detection method according to claim 9, wherein the preparation of the radix Seu caulis Parthenocissi Tricuspidatae is Bischofumeclite, and the preparation method of the test solution comprises: collecting 20ml of the product, placing in a separating funnel, extracting with chloroform 20ml under shaking, collecting chloroform solution, evaporating to dryness, and dissolving the residue with 1ml of methanol to obtain sample solution;
the preparation method of the solution of the Scopolia sinensis reference medicinal material comprises the following steps: collecting control drug of caulis et folium piperis longi 1g, adding ethanol 20ml, ultrasonic treating for 30 min, filtering, evaporating filtrate to dryness, dissolving residue with 55% ethanol 20ml, placing in separating funnel, extracting with chloroform 20ml under shaking, collecting chloroform solution, evaporating to dryness, dissolving residue with methanol 1ml, and making into control drug solution.
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