CN102028839A - Quality control method of Chinese medicinal preparation for regulating menstruation in Department of Obstetrics and Gynecology - Google Patents
Quality control method of Chinese medicinal preparation for regulating menstruation in Department of Obstetrics and Gynecology Download PDFInfo
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Abstract
The invention relates to a quality control method of a Chinese medicinal preparation for regulating menstruation in Department of Obstetrics and Gynecology. The method comprises the following steps of: (1) identifying a character; (2) identifying papaya by a thin layer chromatography; (3) identifying dark plum fruit by the thin layer chromatography; (4) identifying white paeony root by the thin layer chromatography; and (5) measuring the white paeony root by a high-efficiency liquid phase method. Quality standard of dampness removing pills is enhanced and perfected, the character and microscopical characteristic of the dampness removing pills are modified, thin layer identification and inspection method for the papaya, the dark plum fruit and the white paeony root in a prescription is increased and the white paeony root content in the prescription is measured by taking paeoniflorin as a comparison product by a high-efficiency liquid phase chromatography; due to the modified quality standard, the controllability of the quality standard of the dampness removing pills is enhanced and inherent quality and curative effect of the product are further ensured; moreover, the method plays an important role in promoting product sales, increasing the market competition of the product and ensuring the medicament taking safety of patients.
Description
Technical field
The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, the regulating menstruation of especially a kind of gynecological is with the method for quality control of the wet ball that disappears of Chinese medicine preparation.
Background technology
The wet ball that disappears is made up of eight flavor Chinese medicines such as Radix Rehmanniae Preparata, Radix Rehmanniae, Radix Glehniae, the Rhizoma Atractylodis Macrocephalae, the Radix Paeoniae Alba, Fructus Mume, Fructus Chaenomelis and Rhizoma Cyperi.Preparation method is above eight flavors, is ground into fine powder, and mixing sieves, and every 100g powder adds refined honey 100～120g and makes big honeyed pills, promptly.The wet ball that disappears has enriching yin and nourishing kidney, invigorating spleen and reinforcing stomach, inducing diuresis and reducing edema effect.Be usually used in treating nourishing kidney-yin, Simple Obesity due to wet the Sheng, edema, and disease such as menoxenia are the conventional Chinese medicine preparations of gynecological's regulating menstruation.
Wet disappear ball by the department of Chinese medicine expert of Hospital No.1 Attached to Tianjin Traditional Chinese Medicine College use traditional Chinese medicine theory and for many years clinical experience develop in conjunction with determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs.This product is agreed to produce " Tianjin drug standard " nineteen ninety version, " the 20 in Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation " (standard No.: recorded WS3-B-4024-98) through the reply in 1984 of Tianjin health bureau.The wet ball that disappears is the exclusive kind that Tianjin Zhongxin Pharmaceutical Group Co produces.
Along with constant development of economy, Chinese medicine is subjected to the more understanding of common people and attractes attention.Chinese medicine is to grow up under traditional instruction of Chinese Medicine theory, and mostly raw material is natural materials such as bark and grass roots, mineral, animal, wide material sources, complicated component.This has just determined the particularity of Chinese medicine safety standards, and the safety standards problem becomes the difficult problem that Chinese medicine enters the international market too.The trend of Chinese medicine standard though the present international standard of still not having plant medicine in the world, the south east asia of the U.S., European Union and China's tradition outlet Chinese medicine are improved.In the case, the standard that more will propose to be fit to China's product quality to be adapting to international standard, and Chinese medicine in state-owned thousands of years use history, countries in the world are also many Chinese medicine standards with reference to China in working out corresponding plant amedica target level of product quality.Quality standard perfect, that improve Chinese medicine has become extremely urgent thing more.
During thin layer chromatography (TLC) is differentiated control medicinal material determine more and more be used in the Chinese medicine preparation, owing to the restriction of reference substance or select reasons such as reference substance is exclusive inadequately, the chromatograph contrast of often selecting for use control medicinal material to differentiate as TLC.
High performance liquid chromatography (HPLC) has fast, sensitive, separation efficiency advantages of higher, in TCD identification, after adopting HPLC method separation characteristic composition, carrying out structural analysis and quantitative analysis with UV-detector (UV) or mass detector (MS), is the effective ways of thoroughly evaluating quality.Just there are 59 kinds of medical materials and 50 kinds of Chinese patent medicines to adopt the HPLC methods to identify in one one of the Chinese Pharmacopoeia (version in 2000), study but also constantly there is human HPLC method that other Chinese medicine is identified with component analysis.
The wet ball initial quality standard statement that disappears: " put microscopically and observe for getting this product: contain gelatinizing starch grain parenchyma cell; single loose from or fragmentation; be similar round, ellipse or irregular shape; be full of the starch grain of gelatinizing; wall can be examined sometimes and see; calcium oxalate cluster crystal diameter 11～24～35 μ m, accidental prismatic crystal.It is unicellular that nonglandular hair mostly is greatly, straight or bend to sickle shaped, fallow, often is full of the burgundy thing in the cell ".For the method for quality control of this kind, obviously ten minutes is fuzzy and not enough.The description of part Chinese medicine microscopical identification features such as the Fructus Mume and the Radix Paeoniae Alba is only arranged in original standard, for quality control standard, be nowhere near, should add control medicinal material and reference substance foundation as the thin layer chromatography identification of test method.The assay item that does not have the index components of the discriminating of feature medical material and reflection medicine inherent quality can't effectively guarantee the inherent quality of product aborning, and drug effect also can not get guaranteeing.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, provide a kind of can the regulating menstruation of qualitative and quantitative gynecological with the method for quality control of the wet ball that disappears of Chinese medicine preparation, this method has that detection means is simple, the testing result characteristic of accurate.
The objective of the invention is to be achieved through the following technical solutions:
The regulating menstruation of a kind of gynecological is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and step is:
(1) character identification;
(2) differentiate Fructus Chaenomelis: adopting thin layer chromatography is control medicinal material with the Fructus Chaenomelis, differentiates in the wet ball prescription that disappears whether contain the Fructus Chaenomelis composition;
(3) differentiate Fructus Mume: adopting thin layer chromatography is control medicinal material with the Fructus Mume, differentiates in the wet ball prescription that disappears whether contain the Fructus Mume composition;
(4) differentiate the Radix Paeoniae Alba: adopting thin layer chromatography is reference substance with the peoniflorin, differentiates in the wet ball prescription that disappears whether contain Radix Paeoniae Alba composition;
(5) measure the Radix Paeoniae Alba: adopting high-efficient liquid phase technique is reference substance with the peoniflorin, measures the Radix Paeoniae Alba content in the wet ball prescription that disappears.
And described character identification is:
1. character description is: the big honeyed pills of pitchy, sweet, little acid of distinguishing the flavor of;
2. putting microscopically observes: the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing, and the secretory cell similar round contains fallowly to rufous secretions, and its peripheral cell is made radial arrangement; The fibre bundle rufous, fiber finer, diameter 8～10 μ m.
And described thin layer chromatography differentiates that the method for Fructus Chaenomelis is:
1. the ball sample that disappears of will wetting is made need testing solution;
2. getting Fructus Chaenomelis is that control medicinal material is made control medicinal material solution;
3. the preparation of negative sample solution;
4. thin layer chromatography detects: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio toluene: ethyl acetate: formic acid=5: 1: 0.1 be that developing solvent launches, and spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear;
5. interpretation of result: lamellae put under the ultra-violet lamp 365nm wavelength inspect, determine whether contain the Fructus Chaenomelis composition in the test agent.
And described thin layer chromatography differentiates that the method for Fructus Mume is:
1. get the remaining medicinal residues of Fructus Chaenomelis discriminating and make need testing solution;
2. get the Fructus Mume control medicinal material and make control medicinal material solution;
3. the preparation of negative sample solution;
4. thin layer chromatography detects: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio toluene: ethyl acetate: formic acid=5: 3: 1 be that developing solvent launches, and spray is with 5% vanillin sulfuric acid solution solution, be heated to speckle develop the color clear;
5. interpretation of result: analyze the position of the speckle of same color on the silica gel thin-layer plate, determine whether contain the Fructus Mume composition in the test agent.
And described thin layer chromatography differentiates that the method for the Radix Paeoniae Alba is:
1. get the remaining medicinal residues of Fructus Mume discriminating and make need testing solution;
2. get the peoniflorin reference substance, add ethanol and make reference substance solution;
3. the preparation of negative sample solution;
4. thin layer chromatography detects: get 1., 2., 3. solution on same silica gel thin-layer plate, with the volume ratio chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is that developing solvent launches, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing;
5. interpretation of result: analyze the position of the speckle of same color on the silica gel thin-layer plate, determine whether contain Radix Paeoniae Alba composition in the test agent.
And the method that described high-efficient liquid phase technique is measured the Radix Paeoniae Alba is:
1. the setting of liquid phase chromatogram condition;
2. the preparation of standard solution;
3. the preparation of need testing solution;
4. the preparation of negative sample solution;
5. measure Radix Paeoniae Alba chromatogram;
6. interpretation of result: can calculate the content that obtains the Radix Paeoniae Alba in the wet ball that disappears according to chromatogram.
Advantage of the present invention and good effect are:
1, detection method of the present invention is revised character and microscopical identification on the basis of the 20 primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, has increased the thin layer identification of test method of control medicinal material and reference substance; And formulated the method that high performance liquid chromatography is carried out assay.
2, the present invention's thin layer chromatography of increasing control medicinal material, reference substance in the detection method of the wet ball that disappears is differentiated and inspection item such as high performance liquid chromatogram discriminating, the quality control that more helps Chinese medicine preparation, thereby check out counterfeit drug and substandard drug more exactly, go abroad significant for the modernization of Chinese medicine and Chinese medicine.
3, the present invention has carried out raising, perfect to the quality standard of the wet ball that disappears, on the primary standard basis, the character and the microscopical identification feature of the wet ball that disappears have been revised, increased the thin layer identification of test method of Fructus Chaenomelis, Fructus Mume and the Radix Paeoniae Alba in the prescription, with the peoniflorin is reference substance, has formulated the content that adopts Radix Paeoniae Alba in the high effective liquid chromatography for measuring prescription; Revised quality standard having improved the controllability of the wet ball quality standard that disappears, and further guarantees product inherent quality and curative effect, and to promoting production marketing, increase the competitiveness of product in market, guaranteeing that patient's drug safety is significant.
Description of drawings
It is the figure that inspects under the 365nm ultra-violet lamp for Fructus Chaenomelis in the test agent at daylight and wavelength that Fig. 1 and Fig. 2 are respectively the present invention, wherein, band is followed successively by from left to right among Fig. 1 and Fig. 2: 1. need testing solution 1 (lot number: 200601), 2. need testing solution 2 (lot number: 200602), 3. need testing solution 3 (lot number: 200603), 4. Fructus Chaenomelis control medicinal material, 5. Fructus Chaenomelis negative sample.
Fig. 3 inspects figure for Fructus Mume in the test agent for the present invention under daylight; Wherein band is followed successively by from left to right: 1. need testing solution 1 (lot number: 200601), 2. need testing solution 2 (lot number: 200602), 3. need testing solution 3 (lot number: 200603), 4. Fructus Mume control medicinal material, 5. Fructus Mume negative sample.
Fig. 4 inspects figure for the Radix Paeoniae Alba in the test agent for the present invention under daylight, wherein band is followed successively by from left to right: 1. need testing solution 1 (lot number: 200601), 2. need testing solution 2 (lot number: 200602), 3. need testing solution 3 (lot number: 200603), 4. peoniflorin reference substance (middle inspection institute), 5. Radix Paeoniae Alba negative sample.
Fig. 5 is the liquid chromatogram of peoniflorin reference substance of the present invention (middle inspection institute);
Fig. 6 is the liquid chromatogram of the present invention for test agent;
Fig. 7 is the liquid form and aspect collection of illustrative plates of Radix Paeoniae Alba negative sample of the present invention.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The method of quality control of the wet ball that disappears of the Chinese medicine preparation of a kind of gynecological regulating menstruation, the step of its method is:
(1) character identification:
Character description is: the wet ball that disappears is the big honeyed pills of pitchy; Sweet, little acid of distinguishing the flavor of.Putting microscopically observes: the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing (Radix Rehmanniae Preparata).The secretory cell similar round contains fallowly to rufous secretions, and its peripheral cell is made radial arrangement; The fibre bundle rufous, fiber finer, diameter 8～10 μ m (Rhizoma Cyperi).
(2) thin layer chromatography is differentiated Fructus Chaenomelis: adopting thin layer chromatography, is control medicinal material with the Fructus Chaenomelis, differentiates Fructus Chaenomelis in the wet ball prescription that disappears.
1. the preparation of need testing solution: according to the literature, contain the acid soap glycoside in the Fructus Chaenomelis, as ursolic acid etc., so adopt ether to test in the test as extracting solvent.Get wet ball 1 ball that disappears, shred, add kieselguhr 2.5g, grind well, the supersound process twice that adds diethyl ether, each 30ml, each 10 minutes, filter, merging filtrate, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Fructus Chaenomelis control medicinal material 1g, the supersound process twice that adds diethyl ether is shone medical material solution in pairs with legal system.
3. the preparation of negative sample solution: by the prescription proportioning, get prescription medical material 4g (except the Fructus Chaenomelis), it is an amount of to add refined honey, and the 30ml that adds diethyl ether is according to method for making preparation on the 20 primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, as negative control solution.
4. thin layer detects: the photograph thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution and negative sample solution each 10 μ l, control medicinal material solution 6 μ l, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=5: 1: 0.1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing.
5. interpretation of result: the testing result of the wet ball test sample that disappears of different production batch is seen Fig. 1 and Fig. 2.Under the daylight, in the test sample chromatograph, with the corresponding position of Fructus Chaenomelis control medicinal material chromatograph on, show the speckle of same color, negative sample is noiseless; Put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of Fructus Chaenomelis control medicinal material chromatograph on, show the fluorescence speckle of same color, negative sample is also noiseless, shows for test agent to contain the Fructus Chaenomelis composition.
(3) thin layer chromatography is differentiated Fructus Mume: adopting thin layer chromatography, is control medicinal material with the Fructus Mume, differentiates Fructus Mume in the wet ball prescription that disappears.
1. the preparation of need testing solution: get the medicinal residues after Fructus Chaenomelis is differentiated a following ether extraction, add ethyl acetate 40ml, reflux 30 minutes is put coldly, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: other gets Fructus Mume control medicinal material 1g, adds ethyl acetate 20ml, shines medical material solution in pairs with legal system.
3. the preparation of negative sample solution: by the prescription proportioning, get prescription medical material 4g (except the Fructus Mume), it is an amount of to add refined honey, and the 30ml that adds diethyl ether is again according to method for making preparation on the 20 primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, as negative sample solution.
4. thin layer detects: the photograph thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=5: 3: 1 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing
5. interpretation of result: the testing result of the wet ball test sample that disappears of different production batch is seen Fig. 3.In the test sample chromatograph, with the corresponding position of Fructus Mume reference substance chromatograph on, show the speckle of same color, negative sample is noiseless.Show for test agent and contain the Fructus Mume composition.
(4) thin layer chromatography is differentiated the Radix Paeoniae Alba: adopting thin layer chromatography is reference substance with the peoniflorin, differentiates the Radix Paeoniae Alba in the wet ball prescription that disappears.
1. the preparation of need testing solution: get the medicinal residues under the Fructus Mume discriminating item, add water saturated n-butyl alcohol 40ml, supersound process 60 minutes filters, and n-butyl alcohol liquid evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.
2. the preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.
3. the preparation of negative sample solution: by the prescription proportioning, get prescription medical material 4g (except the Radix Paeoniae Alba), it is an amount of to add refined honey, according to method for making preparation on the 20 primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, as negative sample solution.
4. thin layer detects: draw each 6 μ l of above-mentioned three kinds of solution according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing.
5. interpretation of result: the testing result of the wet ball test sample that disappears of different production batch is seen Fig. 4.In the test sample chromatograph, with the corresponding position of peoniflorin reference substance chromatograph on, show the speckle of same color, negative sample is noiseless.Show that test sample contains Radix Paeoniae Alba composition;
(5) high-efficient liquid phase technique is measured the Radix Paeoniae Alba: adopting the Radix Paeoniae Alba in the wet ball prescription that disappears of high-efficient liquid phase technique mensuration, is reference substance with the peoniflorin.
1. the setting of liquid phase chromatogram condition: with reference to " relevant assay method of Chinese pharmacopoeia version in 2005 determines that detecting wavelength is 230nm.With the octadecylsilane chemically bonded silica is filler; With oxolane: phosphate buffer (1/15mol/L sodium dihydrogen phosphate-1/15mol/L disodium phosphate soln (5: 1))=15: 85 is a mobile phase; Number of theoretical plate calculates by the peoniflorin peak should be not less than 3000.
2. the preparation of standard solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds Diluted Alcohol and makes the solution that every 1ml contains 0.1mg, promptly.Liquid chromatographic detection the results are shown in Figure 5;
3. the preparation of need testing solution: it is an amount of to get the wet ball that disappears, and shreds, and gets 2g, the accurate title, decide, and the accurate Diluted Alcohol 50ml that adds claims to decide weight, supersound process (power 280W, frequency 33kHz) 60 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with Diluted Alcohol, centrifugal (rotating speed is that per minute 3000 changes) 5 minutes gets supernatant, with 0.45 μ m filtering with microporous membrane, get subsequent filtrate, promptly.Liquid chromatographic detection the results are shown in Figure 6.
4. the preparation of negative sample solution: get other each flavor by prescription, make sample, by above-mentioned need testing solution preparation method, make negative sample solution again according to method for making on the 20 primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation except that the Radix Paeoniae Alba.By same chromatographic condition analysis, negative sample is not seen chromatographic peak at the corresponding retention time of peoniflorin place again.The result shows that negative sample is noiseless to detecting.Liquid chromatographic detection the results are shown in Figure 7.
5. measure: accurate respectively molten each the 10 μ l of reference substance solution, need testing solution and negative sample that draw, inject chromatograph of liquid, measure, promptly.
6. interpretation of result: can determine to contain peoniflorin in the test agent by retention time.With reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, and every g sample contains peoniflorin and should be 0.97mg.Can calculate according to chromatogram to obtain content of paeoniflorin in the wet ball that disappears, this content and state-promulgated pharmacopoeia compare, and whether can judge for the Radix Paeoniae Alba content of test agent qualified, and then the quality of the wet ball that disappears of judgement different manufacturers, different batches.In the wet ball prescription that disappears of this laboratory sample, the Radix Paeoniae Alba accounts for 12.74% of prescription total amount, adding refined honey 110g by every 100g fecula in the preparation calculates, every g sample contains the Radix Paeoniae Alba and should be 60.7mg, in view of the wet ball that disappears is a starch, according to Chinese Pharmacopoeia Commission's requirement, starch calculates by 80% rate of transform, for every g contains the Radix Paeoniae Alba with peoniflorin (C
23H
28O
11) meter, be 0.78mg, if contain the Radix Paeoniae Alba with peoniflorin (C by every ball
23H
28O
11) meter, should be less than 7.0mg.
Claims (6)
1. gynecological's regulating menstruation is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and it is characterized in that: the step of method is:
(1) character identification;
(2) differentiate Fructus Chaenomelis: adopting thin layer chromatography is control medicinal material with the Fructus Chaenomelis, differentiates in the wet ball prescription that disappears whether contain the Fructus Chaenomelis composition;
(3) differentiate Fructus Mume: adopting thin layer chromatography is control medicinal material with the Fructus Mume, differentiates in the wet ball prescription that disappears whether contain the Fructus Mume composition;
(4) differentiate the Radix Paeoniae Alba: adopting thin layer chromatography is reference substance with the peoniflorin, differentiates in the wet ball prescription that disappears whether contain Radix Paeoniae Alba composition;
(5) measure the Radix Paeoniae Alba: adopting high-efficient liquid phase technique is reference substance with the peoniflorin, measures the Radix Paeoniae Alba content in the wet ball prescription that disappears.
2. a kind of gynecological according to claim 1 regulating menstruation is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and it is characterized in that: described character identification is:
1. character description is: the big honeyed pills of pitchy, sweet, little acid of distinguishing the flavor of;
2. putting microscopically observes: the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing, and the secretory cell similar round contains fallowly to rufous secretions, and its peripheral cell is made radial arrangement; The fibre bundle rufous, fiber finer, diameter 8～10 μ m.
3. a kind of gynecological according to claim 1 regulating menstruation is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and it is characterized in that: described thin layer chromatography differentiates that the method for Fructus Chaenomelis is:
1. the ball sample that disappears of will wetting is made need testing solution;
2. getting Fructus Chaenomelis is that control medicinal material is made control medicinal material solution;
3. the preparation of negative sample solution;
4. thin layer chromatography detects: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio toluene: ethyl acetate: formic acid=5: 1: 0.1 be that developing solvent launches, and spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear;
5. interpretation of result: lamellae put under the ultra-violet lamp 365nm wavelength inspect, determine whether contain the Fructus Chaenomelis composition in the test agent.
4. a kind of gynecological according to claim 1 regulating menstruation is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and it is characterized in that: described thin layer chromatography differentiates that the method for Fructus Mume is:
1. get the remaining medicinal residues of Fructus Chaenomelis discriminating and make need testing solution;
2. get the Fructus Mume control medicinal material and make control medicinal material solution;
3. the preparation of negative sample solution;
4. thin layer chromatography detects: get 1., 2., 3. solution on same silica gel thin-layer plate, with volume ratio toluene: ethyl acetate: formic acid=5: 3: 1 be that developing solvent launches, and spray is with 5% vanillin sulfuric acid solution solution, be heated to speckle develop the color clear;
5. interpretation of result: analyze the position of the speckle of same color on the silica gel thin-layer plate, determine whether contain the Fructus Mume composition in the test agent.
5. a kind of gynecological according to claim 1 regulating menstruation is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and it is characterized in that: described thin layer chromatography differentiates that the method for the Radix Paeoniae Alba is:
1. get the remaining medicinal residues of Fructus Mume discriminating and make need testing solution;
2. get the peoniflorin reference substance, add ethanol and make reference substance solution;
3. the preparation of negative sample solution;
4. thin layer chromatography detects: get 1., 2., 3. solution on same silica gel thin-layer plate, with the volume ratio chloroform: ethyl acetate: methanol: formic acid=40: 5: 10: 0.2 is that developing solvent launches, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing;
5. interpretation of result: analyze the position of the speckle of same color on the silica gel thin-layer plate, determine whether contain Radix Paeoniae Alba composition in the test agent.
6. a kind of gynecological according to claim 1 regulating menstruation is with the method for quality control of the wet ball that disappears of Chinese medicine preparation, and it is characterized in that: the method that described high-efficient liquid phase technique is measured the Radix Paeoniae Alba is:
1. the setting of liquid phase chromatogram condition;
2. the preparation of standard solution;
3. the preparation of need testing solution;
4. the preparation of negative sample solution;
5. measure Radix Paeoniae Alba chromatogram;
6. interpretation of result: can calculate the content that obtains the Radix Paeoniae Alba in the wet ball that disappears according to chromatogram.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956846A (en) * | 2018-07-27 | 2018-12-07 | 河北中医学院 | A kind of shipi powder freeze-dried powder multiple medicine taste multi information, quick thin-layer identification method |
| CN116735780A (en) * | 2023-07-07 | 2023-09-12 | 江阴天江药业有限公司 | Thin layer identification method and application of papaya or papaya-containing pharmaceutical preparation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939433A (en) * | 2005-09-30 | 2007-04-04 | 北京奇源益德药物研究所 | Quality control of Chinese medicinal compound preparation |
| CN101468122A (en) * | 2007-12-26 | 2009-07-01 | 天津中新药业集团股份有限公司达仁堂制药厂 | Chinese medicinal composition for treating simple obesity and method for preparing the same |
-
2009
- 2009-09-28 CN CN200910070659.3A patent/CN102028839B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939433A (en) * | 2005-09-30 | 2007-04-04 | 北京奇源益德药物研究所 | Quality control of Chinese medicinal compound preparation |
| CN101468122A (en) * | 2007-12-26 | 2009-07-01 | 天津中新药业集团股份有限公司达仁堂制药厂 | Chinese medicinal composition for treating simple obesity and method for preparing the same |
Non-Patent Citations (6)
| Title |
|---|
| 万日义等: "芍药属植物及其制剂中有效成分鉴别和含量测定研究概述", 《海峡药学》 * |
| 单玉荣: "木瓜含量测定方法的研究", 《安徽医药》 * |
| 王文平等: "木瓜中齐墩果酸的分离提取及含量测定", 《食品科学》 * |
| 窦忠花等: "引种木瓜的质量分析", 《山东医药》 * |
| 索菲亚等: "愈溃宁颗粒的质量标准研究", 《中成药》 * |
| 高群等: "丹重搽剂质量标准研究", 《中国药房》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956846A (en) * | 2018-07-27 | 2018-12-07 | 河北中医学院 | A kind of shipi powder freeze-dried powder multiple medicine taste multi information, quick thin-layer identification method |
| CN116735780A (en) * | 2023-07-07 | 2023-09-12 | 江阴天江药业有限公司 | Thin layer identification method and application of papaya or papaya-containing pharmaceutical preparation |
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| CN102028839B (en) | 2015-02-25 |
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