CN102038892A - Quality control method for traditional Chinese medicinal preparation of galactagogue pills - Google Patents

Abstract

The invention relates to a quality control method for a traditional Chinese medicinal preparation of galactagogue pills, which comprises the following steps of: firstly, performing microscopical identification; secondly, identifying whether a prescription of the galactagogue pills contains costustoot, Chinese angelica, szechuan lovage rhizome and astragalus components by adopting thin layer chromatography; and finally, measuring the content of white paeony root in the prescription of the galactagogue pills by taking paeoniflorin as a reference substance through high performance liquid chromatography. In the detection method, on the basis of the original standard of the first volume of Chinese patent medicines in Drug Standards Issued by Ministry of Public Health, a thin layer identification detection method for a reference medicinal material and a reference substance is increased, and a method for measuring the content by the high performance liquid chromatography is formulated. The revised quality standard control method improves the controllability of the quality standard of the galactagogue pills, further ensures the inherent quality and treatment effect of a product, and has important significance for promoting product sales, improving the market competitiveness of the product and ensuring the medication safety of the patient.

Description

The method of quality control of Chinese medicine preparation lactogenic ball

Technical field

The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, especially a kind of method of quality control of Chinese medicine preparation lactogenic ball.

Background technology

Lactogenic ball main component is: the Radix Astragali, Radix Angelicae Sinensis, the Radix Paeoniae Alba, Radix Rehmanniae Preparata, Rhizoma Chuanxiong, Radix Rhapontici, Fructus Hordei Germinatus, Cornu Cervi Degelatinatum, Semen Vaccariae, Squama Manis, the Radix Aucklandiae, Medulla Tetrapanacis, and preparation method: above 12 flavors are ground into fine powder, sieve, mixing, every 100g powder adds refined honey 110～130g, make big honeyed pills, that is major function: help gas to enrich blood, active, stimulating milk secretion, be used for the deficiency of both QI and blood in puerperal, galactostasis, the milk rareness, the clinical puerperal hypogalactia of being used for belongs to insufficiency of vital energy and blood, mammary gland impassable patient.Existing quality standard statement: this product is brown to tan big honeyed pills; Sweet, little hardship of distinguishing the flavor of, this simple description is difficult to well differentiate medicine.

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.

Summary of the invention

The objective of the invention is to overcome the deficiencies in the prior art part, a kind of method of quality control of Chinese medicine preparation lactogenic ball that can the qualitative and quantitative analysis ingredient is provided, 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:

A kind of method of quality control of Chinese medicine preparation lactogenic ball, step is:

(1) microscopical identification;

(2) be reference substance with dehydrocostuslactone and costunolide, thin layer chromatography differentiates in the lactogenic ball prescription whether contain the Radix Aucklandiae;

(3) be control medicinal material with Radix Angelicae Sinensis and Rhizoma Chuanxiong, thin layer chromatography differentiates in the lactogenic ball prescription whether contain Radix Angelicae Sinensis and Rhizoma Chuanxiong;

(4) with the astragaloside be reference substance, thin layer chromatography differentiates in the lactogenic ball prescription whether contain the Radix Astragali;

(5) with the peoniflorin be reference substance, high-efficient liquid phase technique is measured the Radix Paeoniae Alba content in the lactogenic ball prescription.

And described microscopical identification is: put microscopically and observe: amorphous fragment is near colourless or faint yellow, and similar round not of uniform size or oval cavity are arranged, and the fragment edge is often uneven; The fiber bunchy or loose from, how cataclasm, wall thickness, there is longitudinal crack on the surface, two ends fragment into broom shape or more truncate; The epidermis cell file is often by 1 long cell and 2 alternate connections of short cell, long cell wall thickness, wavy bending, lignify; Plant skin epidermis fragment rufous or yellowish-brown, cell surface is seen anticlinal wall and is thickened, and star horn shape or dark wavy bending are made zyklopisch and arranged.

And described thin layer chromatography differentiates that the step of the Radix Aucklandiae in the lactogenic ball prescription is:

1. the preparation of need testing solution: get lactogenic ball sample 2 balls, shred, add chloroform 30ml, supersound process 30 minutes filters, and residue is standby, and filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution;

2. the preparation of reference substance solution: remove hydrogen constuslactone reference substance, costunolide reference substance, add chloroform respectively and make the solution that every 1ml contains 0.5mg, in contrast product solution;

3. thin layer condition and result: thin layer chromatography test, draw each 2～6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=5: 1 is developing solvent, launches, take out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing, detect in the need testing solution chromatograph on the speckle displacement of reference substance, whether to show identical speckle, and then determine whether contain Radix Aucklandiae composition for test agent.

And the Radix Angelicae Sinensis in the described thin layer chromatography discriminating lactogenic ball prescription and the step of Rhizoma Chuanxiong composition are:

1. the preparation of need testing solution: get the need testing solution in the Radix Aucklandiae discriminating;

2. the preparation of control medicinal material solution: get Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, add chloroform 20ml, supersound process 10 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution;

3. thin layer condition and result: thin layer chromatography test, draw need testing solution and each 2～4 μ l of above-mentioned control medicinal material in the Radix Aucklandiae discriminating, put respectively on same silica gel g thin-layer plate, with normal hexane: ethyl acetate=4: 1 is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp 365nm and inspect, detect in the need testing solution chromatograph on the speckle displacement of reference substance, whether to show identical speckle, and then determine whether contain Radix Angelicae Sinensis and Rhizoma Chuanxiong composition for test agent.

And described thin layer chromatography differentiates that the step of the astragalus root components in the lactogenic ball prescription is:

1. the preparation of need testing solution: get the residue in the Radix Aucklandiae discriminating, add 1% sodium hydrate methanol solution 50ml, refluxed 1 hour, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, extract twice with water saturated n-butyl alcohol jolting, each 30ml merges n-butyl alcohol liquid, extract 2 times with the ammonia solution jolting, each 25ml discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution;

2. the preparation of reference substance solution: get the astragaloside reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution;

3. thin layer condition and result: thin layer chromatography test, draw each 2～6 μ l of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: methanol: lower floor's solution of water=13: 7: 2 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to the speckle colour developing, put respectively under daylight and the ultra-violet lamp 365nm and inspect, detect in the need testing solution chromatograph on the speckle displacement of reference substance, whether to show identical speckle, and then determine whether contain astragalus root components for test agent.

And described employing high-efficient liquid phase technique is a reference substance with the peoniflorin, and the method for measuring Radix Paeoniae Alba content in the lactogenic ball prescription is:

1. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Mobile phase: acetonitrile: 0.1% phosphoric acid solution=18: 82, the detection wavelength is 230nm, column temperature: 40 ℃, flow velocity: 1.0ml/ minute, number of theoretical plate calculates by the peoniflorin peak should be not less than 5000;

2. the preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 60 μ g,, and detects chromatogram that is;

3. the preparation of need testing solution: it is an amount of to get lactogenic ball sample, shreds, and gets about 2g, the accurate title, decide, and the accurate Diluted Alcohol 25ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, centrifugal 10 minutes, get supernatant, filter, get subsequent filtrate, that is, and detect chromatogram;

4. detect and result's mensuration: precision is drawn reference substance solution, need testing solution and is used respectively 10 μ l of solvent respectively, injects chromatograph of liquid, mensuration; In the lactogenic ball prescription, the Radix Paeoniae Alba accounts for 9.8% of prescription total amount, adding refined honey 110g by every 100g fecula in the preparation calculates, every gram sample contains Radix Paeoniae Alba fecula 46.5mg approximately, with reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, every g sample contains peoniflorin and should be 0.74mg, and starch calculates by 80% rate of transform, and the every g of this product contains the Radix Paeoniae Alba with peoniflorin C ₂₃H ₂₈O ₁₁Meter must not be less than 0.59mg, with reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, contains the Radix Paeoniae Alba with peoniflorin C so content limit is formulated for every ball ₂₃H ₂₈O ₁₁Meter must not be less than 5.31mg.

Advantage of the present invention and good effect are:

1, detection method of the present invention is on the basis of first primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, increased the thin layer identification of test method of control medicinal material and reference substance, formulate high performance liquid chromatography and carried out the method for assay, revised quality standard control method, improved the controllability of lactogenic ball quality standard, further guarantee product inherent quality and curative effect, to promoting production marketing, increase the competitiveness of product in market, guaranteeing that patient's drug safety is significant.

2, the present invention is with reference to " method such as one one of Chinese pharmacopoeia version in 2005 has increased the microscopical identification method of Squama Manis, the Radix Astragali, Fructus Hordei Germinatus, Semen Vaccariae in the prescription; Increased the thin layer discrimination method of Radix Angelicae Sinensis and Rhizoma Chuanxiong, the Radix Aucklandiae and the Radix Astragali; With the peoniflorin is reference substance, has formulated the content assaying method of the Radix Paeoniae Alba, and revised quality standard has improved the quality control of medicine, can check out counterfeit drug and substandard drug more exactly, and the modernization of Chinese medicine and Chinese medicine are gone abroad to be significant.

Description of drawings

Fig. 1 inspects figure for the chromatogram on the self-control lamellae of the present invention in detecting for the test agent Radix Aucklandiae under the chromatographic condition that experiment is set, be followed successively by from left to right: dehydrocostuslactone reference substance (middle inspection institute, lot number: 11525-200404), costunolide reference substance (middle inspection institute, lot number: 11524-200503), Radix Aucklandiae control medicinal material (middle inspection institute, lot number: 120921-200506), sample 1 (lot number: 200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), negative control;

Fig. 2 " is inspecting figure under the chromatographic condition that Chinese pharmacopoeia version in 2005 is an one for the chromatogram on the self-control lamellae of the present invention in detecting for the test agent Radix Aucklandiae, be followed successively by from left to right: negative control, sample 1 (lot number: 200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), remove Radix Aucklandiae control medicinal material (middle inspection institute), Radix Aucklandiae control medicinal material (middle inspection institute);

Fig. 3 inspects figure for the present invention in detecting for the Radix Aucklandiae in the test agent on commercially available plate (Yantai product), be followed successively by from left to right: negative control, sample 1 (lot number: 200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), dehydrocostuslactone reference substance (middle inspection institute), costunolide reference substance (middle inspection institute);

Fig. 4 inspects figure for Radix Angelicae Sinensis in the test agent and Rhizoma Chuanxiong for the present invention under ultra-violet lamp (365nm), be followed successively by from left to right: negative control, sample 1 (lot number: 200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), Radix Angelicae Sinensis and Rhizoma Chuanxiong control medicinal material (middle inspection institute, lot number: 120927-200512), (middle inspection institute, lot number: 120917-200503);

Fig. 5, Fig. 6 are respectively the thin-layer chromatogram of the present invention in detecting for the Radix Astragali in the test agent and inspect figure under daylight and ultra-violet lamp 365nm, be followed successively by from left to right: sample 1 (lot number: 200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), astragaloside reference substance (middle inspection institute, lot number: 110781-200512), negative control;

Fig. 7 is reference substance figure spectrogram in the Radix Paeoniae Alba liquid chromatographic detection of the present invention;

Fig. 8 is test sample figure spectrogram in the Radix Paeoniae Alba liquid chromatographic detection of the present invention;

Fig. 9 is negative sample collection of illustrative plates in the Radix Paeoniae Alba liquid chromatographic detection 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 Chinese medicine preparation lactogenic ball, the step of its method is:

(1) microscopical identification:

This product is a starch, " Chinese pharmacopoeia one one of version in 2005 waits related content in reference, microscopic features to Squama Manis, the Radix Astragali, Fructus Hordei Germinatus, Semen Vaccariae in the prescription are described, putting the microscopic examination specific descriptions is: " amorphous fragment is near colourless or faint yellow; similar round not of uniform size or oval cavity are arranged, fragment edge often uneven (Squama Manis).The fiber bunchy or loose from, how cataclasm, wall thickness, there is longitudinal crack on the surface, two ends fragment into broom shape or more truncate (Radix Astragali).The epidermis cell file is often by 1 long cell and 2 alternate connections of short cell, long cell wall thickness, wavy bending, lignify (Fructus Hordei Germinatus).Plant skin epidermis fragment rufous or yellowish-brown, cell surface is seen anticlinal wall and is thickened, and star horn shape or dark wavy bending are made zyklopisch and arranged (Semen Vaccariae).

(2) adopting thin layer chromatography, is reference substance with dehydrocostuslactone and costunolide, differentiates the Radix Aucklandiae composition in the lactogenic ball prescription.

1. the preparation of need testing solution: get lactogenic ball sample 2 balls, shred, add chloroform 30ml, supersound process 30 minutes filters, and residue is standby, and filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution;

2. the preparation of reference substance solution: remove hydrogen constuslactone reference substance, costunolide reference substance, add chloroform respectively and make the solution that every 1ml contains 0.5mg, in contrast product solution;

3. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that the Radix Aucklandiae, make pill, make negative sample solution by above-mentioned need testing solution preparation method again by the technology of former medicine;

4. thin layer condition and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 2～6 μ l of above-mentioned four kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=5: 1 is developing solvent, launch, take out, dry, spray is with 2% vanillin sulfuric acid solution, it is clear to be heated to the speckle colour developing, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.Negative sample is noiseless, the results are shown in Figure 1, once adopted " the thin layer chromatography condition test of a middle Radix Aucklandiae medical material of Chinese pharmacopoeia version in 2005 in addition, the dehydrocostuslactone speckle is not concentrated as a result, see Fig. 2, adopt the lamellae of other brands, with cyclohexane extraction: acetone=5: 1 is the developing solvent repeated trials, good reproducibility is seen Fig. 3.

(3) adopting thin layer chromatography, is control medicinal material with Radix Angelicae Sinensis, Rhizoma Chuanxiong, differentiates Radix Angelicae Sinensis and Rhizoma Chuanxiong composition in the lactogenic ball prescription.

1. the preparation of need testing solution: get the need testing solution in the Radix Aucklandiae discriminating;

2. the preparation of control medicinal material solution: get Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, add chloroform 20ml, supersound process 10 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution;

3. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Radix Angelicae Sinensis and Rhizoma Chuanxiong, make pill, make negative sample solution by above-mentioned need testing solution preparation method again by the technology of former medicine;

4. thin layer condition and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 2～4 μ l of need testing solution, above-mentioned control medicinal material and negative sample solution in the Radix Aucklandiae discriminating, put respectively on same silica gel g thin-layer plate, with normal hexane: ethyl acetate=4: 1 is developing solvent, launch, take out, dry, put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color, the negative sample contrast is noiseless, the results are shown in Figure 4.

(4) adopting thin layer chromatography, is reference substance with the astragaloside, differentiates astragalus root components in the lactogenic ball prescription.

1. the preparation of need testing solution: get the residue in the Radix Aucklandiae discriminating, add 1% sodium hydrate methanol solution 50ml, reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, extract twice with water saturated n-butyl alcohol jolting, each 30ml merges n-butyl alcohol liquid, extract 2 times with the ammonia solution jolting, each 25ml discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution;

2. the preparation of reference substance solution: get the astragaloside reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution;

3. negative sample formulations prepared from solutions: by the prescription proportioning, get other flavour of a drug except that the Radix Astragali, make pill, make negative sample solution by above-mentioned need testing solution preparation method again by the technology of former medicine;

4. thin layer condition and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 2～6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: methanol: lower floor's solution of water=13: 7: 2 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle or the fluorescence speckle of same color respectively, negative sample solution is noiseless as a result, wherein: inspect figure under the daylight and see Fig. 5, ultra-violet lamp (365nm) is inspected figure and is seen Fig. 6, through observing, can obtain same effect.

(5) adopting high-efficient liquid phase technique, is reference substance with the peoniflorin, measures the content of the Radix Paeoniae Alba in the prescription lactogenic ball.

1. chromatographic condition: with reference to " relevant content assaying method of Chinese pharmacopoeia version in 2005 is formulated, and is filler with octadecylsilane chemically bonded silica; Mobile phase: acetonitrile: 0.1% phosphoric acid solution=18: 82; The detection wavelength is 230nm; Column temperature: 40 ℃; Flow velocity: 1.0ml/ minute, number of theoretical plate calculates by the peoniflorin peak should be not less than 5000;

2. the preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 60 μ g,, the results are shown in Figure 7 that is;

3. the preparation of need testing solution: it is an amount of to get lactogenic ball sample, shreds, and gets about 2g, the accurate title, decide, and the accurate Diluted Alcohol 25ml that adds claims to decide weight, supersound process (power 240W, frequency 45kHz) 30 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with Diluted Alcohol, centrifugal (3000 rev/mins) 10 minutes get supernatant, filter, get subsequent filtrate, that is, the results are shown in Figure 8;

4. the preparation of negative sample solution: get the medical material of respectively distinguishing the flavor of by prescription, make pill, by 2. need testing solution preparation method, make negative sample solution again, the results are shown in Figure 9 by the technology of former medicine except that the Radix Paeoniae Alba;

5. detect and result's mensuration: precision is drawn reference substance solution, need testing solution, negative sample solution and is used respectively 10 μ l of solvent respectively, injects chromatograph of liquid, mensuration; In the lactogenic ball prescription, the Radix Paeoniae Alba accounts for 9.8% of prescription total amount, adding refined honey 110g by every 100g fecula in the preparation calculates, every gram sample contains Radix Paeoniae Alba fecula 46.5mg approximately, with reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, every g sample contains peoniflorin and should be 0.74mg, and starch calculates by 80% rate of transform, and the every g of this product contains the Radix Paeoniae Alba with peoniflorin (C ₂₃H ₂₈O ₁₁) meter, must not be less than 0.59mg, with reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, contains the Radix Paeoniae Alba with peoniflorin (C so content limit is formulated for every ball ₂₃H ₂₈O ₁₁) meter, must not be less than 5.31mg.

Claims (6)

1. the method for quality control of a Chinese medicine preparation lactogenic ball, it is characterized in that: the step of its method is:

(1) microscopical identification;

(2) be reference substance with dehydrocostuslactone and costunolide, thin layer chromatography differentiates in the lactogenic ball prescription whether contain the Radix Aucklandiae;

(3) be control medicinal material with Radix Angelicae Sinensis and Rhizoma Chuanxiong, thin layer chromatography differentiates in the lactogenic ball prescription whether contain Radix Angelicae Sinensis and Rhizoma Chuanxiong;

(4) with the astragaloside be reference substance, thin layer chromatography differentiates in the lactogenic ball prescription whether contain the Radix Astragali;

(5) with the peoniflorin be reference substance, high-efficient liquid phase technique is measured the Radix Paeoniae Alba content in the lactogenic ball prescription.

2. the method for quality control of Chinese medicine preparation lactogenic ball according to claim 1, it is characterized in that: described microscopical identification is: put microscopically and observe: amorphous fragment is near colourless or faint yellow, similar round not of uniform size or oval cavity are arranged, and the fragment edge is often uneven; The fiber bunchy or loose from, how cataclasm, wall thickness, there is longitudinal crack on the surface, two ends fragment into broom shape or more truncate; The epidermis cell file is often by 1 long cell and 2 alternate connections of short cell, long cell wall thickness, wavy bending, lignify; Plant skin epidermis fragment rufous or yellowish-brown, cell surface is seen anticlinal wall and is thickened, and star horn shape or dark wavy bending are made zyklopisch and arranged.

3. the method for quality control of Chinese medicine preparation lactogenic ball according to claim 1 is characterized in that: described thin layer chromatography differentiates that the step of the Radix Aucklandiae in the lactogenic ball prescription is:

1. the preparation of need testing solution: get lactogenic ball sample 2 balls, shred, add chloroform 30ml, supersound process 30 minutes filters, and residue is standby, and filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution;

2. the preparation of reference substance solution: remove hydrogen constuslactone reference substance, costunolide reference substance, add chloroform respectively and make the solution that every 1ml contains 0.5mg, in contrast product solution;

3. thin layer condition and result: thin layer chromatography test, draw each 2～6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=5: 1 is developing solvent, launches, take out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing, detect in the need testing solution chromatograph on the speckle displacement of reference substance, whether to show identical speckle, and then determine whether contain Radix Aucklandiae composition for test agent.

4. the method for quality control of Chinese medicine preparation lactogenic ball according to claim 1 is characterized in that: the Radix Angelicae Sinensis in the described thin layer chromatography discriminating lactogenic ball prescription and the step of Rhizoma Chuanxiong composition are:

1. the preparation of need testing solution: get the need testing solution in the Radix Aucklandiae discriminating;

2. the preparation of control medicinal material solution: get Radix Angelicae Sinensis and each 0.5g of Rhizoma Chuanxiong control medicinal material, add chloroform 20ml, supersound process 10 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution;

3. thin layer condition and result: thin layer chromatography test, draw need testing solution and each 2～4 μ l of above-mentioned control medicinal material in the Radix Aucklandiae discriminating, put respectively on same silica gel g thin-layer plate, with normal hexane: ethyl acetate=4: 1 is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp 365nm and inspect, detect in the need testing solution chromatograph on the speckle displacement of reference substance, whether to show identical speckle, and then determine whether contain Radix Angelicae Sinensis and Rhizoma Chuanxiong composition for test agent.

5. the method for quality control of Chinese medicine preparation lactogenic ball according to claim 1 is characterized in that: described thin layer chromatography differentiates that the step of the astragalus root components in the lactogenic ball prescription is:

1. the preparation of need testing solution: get the residue in the Radix Aucklandiae discriminating, add 1% sodium hydrate methanol solution 50ml, refluxed 1 hour, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, extract twice with water saturated n-butyl alcohol jolting, each 30ml merges n-butyl alcohol liquid, extract 2 times with the ammonia solution jolting, each 25ml discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution;

2. the preparation of reference substance solution: get the astragaloside reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution;

3. thin layer condition and result: thin layer chromatography test, draw each 2～6 μ l of above-mentioned 2 kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: methanol: lower floor's solution of water=13: 7: 2 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to the speckle colour developing, put respectively under daylight and the ultra-violet lamp 365nm and inspect, detect in the need testing solution chromatograph on the speckle displacement of reference substance, whether to show identical speckle, and then determine whether contain astragalus root components for test agent.

6. the method for quality control of Chinese medicine preparation lactogenic ball according to claim 1 is characterized in that: described employing high-efficient liquid phase technique is a reference substance with the peoniflorin, and the method for measuring Radix Paeoniae Alba content in the lactogenic ball prescription is:

1. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Mobile phase: acetonitrile: 0.1% phosphoric acid solution=18: 82, the detection wavelength is 230nm, column temperature: 40 ℃, flow velocity: 1.0ml/ minute, number of theoretical plate calculates by the peoniflorin peak should be not less than 5000;

2. the preparation of reference substance solution: it is an amount of to get the peoniflorin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 60 μ g,, and detects chromatogram that is;

3. the preparation of need testing solution: it is an amount of to get lactogenic ball sample, shreds, and gets about 2g, the accurate title, decide, and the accurate Diluted Alcohol 25ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight, supply the weight that subtracts mistake with Diluted Alcohol, shake up, centrifugal 10 minutes, get supernatant, filter, get subsequent filtrate, that is, and detect chromatogram;

4. detect and result's mensuration: precision is drawn reference substance solution, need testing solution and is used respectively 10 μ l of solvent respectively, injects chromatograph of liquid, mensuration; In the lactogenic ball prescription, the Radix Paeoniae Alba accounts for 9.8% of prescription total amount, adding refined honey 110g by every 100g fecula in the preparation calculates, every gram sample contains Radix Paeoniae Alba fecula 46.5mg approximately, with reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, every g sample contains peoniflorin and should be 0.74mg, and starch calculates by 80% rate of transform, and the every g of this product contains the Radix Paeoniae Alba with peoniflorin C ₂₃H ₂₈O ₁₁Meter must not be less than 0.59mg, with reference to " content limit calculates under Radix Paeoniae Alba item of Chinese pharmacopoeia version in 2005, contains the Radix Paeoniae Alba with peoniflorin C so content limit is formulated for every ball ₂₃H ₂₈O ₁₁Meter must not be less than 5.31mg.

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