CN102048941B - Quality control method of children-welfare tablets serving as Chinese medicinal preparation - Google Patents
Quality control method of children-welfare tablets serving as Chinese medicinal preparation Download PDFInfo
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- CN102048941B CN102048941B CN200910071120XA CN200910071120A CN102048941B CN 102048941 B CN102048941 B CN 102048941B CN 200910071120X A CN200910071120X A CN 200910071120XA CN 200910071120 A CN200910071120 A CN 200910071120A CN 102048941 B CN102048941 B CN 102048941B
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Abstract
The invention relates to a quality control method of children-welfare tablets serving as a Chinese medicinal preparation. The method comprises the following steps of: performing microscopical identification; identifying whether a prescription of the children-welfare tablets comprises whiteflower hogfennel root, bitter orange, red orange, vine root, divaricate saposhnikovia root and naringin which serve as comparison substances or not by a thin layer chromatography and detecting the naringin content of the prescription of the children-welfare tablets by a liquid chromatography; and testing the mercuric sulfide content of cinnabar in the prescription of the children-welfare tablets by a potentiometric titration method. Based on the original standard of a test method, a microscopical identification method is provided for cinnabar, figwirt root, pinellia tuber, balloonflower root, incised notopterygium rhizome, gambir plant, vine root, liquoric root, divaricate saposhnikovia root and cornu bubali concentrated powder; a thin layer identification method is provided for whiteflower hogfennel root, bitter orange, vine root and divaricate saposhnikovia root in the prescription; a content test method for red orange and bitter orange is drawn up by taking naringin as a quantitative index; by a modified quality standard, the controllability over the quality standard of the children-welfare tablets is enhanced, and the inherent quality and the curative effect of a product are further ensured; and the standard plays an important role in promoting production marketing, enhancing market competitiveness of the product and ensuring medication safety of a patient.
Description
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 XIAOER JINDAN.
Background technology
XIAOER JINDAN is made up of Cinnabaris, dried tangerine peel, Bulbus Fritillariae Ussuriensis, Arisaema Cum Bile, Radix Peucedani, Radix Scrophulariae, the Rhizoma Pinelliae (clearly), Folium Isatidis, Caulis Akebiae, Radix Platycodonis, Herba Schizonepetae, Rhizoma Et Radix Notopterygii, Cacumen Tamaricis, Radix Rehmanniae, Fructus Aurantii (parched with bran), Radix Paeoniae Rubra, Ramulus Uncariae Cum Uncis, Radix Puerariae, Fructus Arctii (stir-fry), Rhizoma Gastrodiae, Radix Glycyrrhizae, windproof, Borneolum Syntheticum, Pulvis Cornus Bubali Concentratus, Cornu Saigae Tataricae, Herba Menthae; Method for preparing: above 20 Six-elements; The Cornu Saigae Tataricae file is ground into fine powder; Pulvis Cornus Bubali Concentratus, Borneolum Syntheticum are ground into fine powder, and Cinnabaris water flies into impalpable powder; 22 flavors such as all the other Bulbus Fritillariae Ussuriensiss are ground into fine powder, sieve; With powder facing-ups such as Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus, Borneolum Syntheticum, Cinnabaris fine powder and Bulbus Fritillariae Cirrhosaes; Sieve; Mixing, every 100g powder add refined honey 120～140g and process big honeyed pills, promptly get; Major function: dispelling pathogenic wind and eliminating phlegm, heat clearing away is relieving convulsion, is used for infantile common cold fever, nasal obstruction watery nasal discharge, cough and asthma, laryngopharynx swelling and pain, hyperpyrexia and infantile convulsion.
Though still there is not the international standard of plant medicine at present in the world; The trend of Chinese medicine standard but the south east asia of the U.S., European Union, China and tradition outlet Chinese medicine is improved; In the case, the standard that needs to propose to be fit to China's product quality is to adapt to international standard, and it is historical that China has the Chinese medicine in thousands of years to use; Countries in the world are many Chinese medicine standards with reference to China in working out corresponding plant amedica target level of product quality, so quality standard perfect, that improve Chinese medicine is more extremely urgent.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, a kind of method of quality control of Chinese medicine preparation XIAOER JINDAN 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 realize through following technical scheme:
A kind of method of quality control of Chinese medicine preparation XIAOER JINDAN, step is:
(1) microscopical identification;
(2) the former control medicinal material of acting like a bully, thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain the Radix Peucedani composition;
(3) being control medicinal material with the Fructus Aurantii, is reference substance with the naringin, and thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain the Fructus Aurantii composition;
(4) being control medicinal material with the Radix Puerariae, is reference substance with the puerarin, and thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain the Radix Puerariae composition;
(5) with windproof be control medicinal material, 5-O-methyl-visamminol is a reference substance, and thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain windproof composition;
(6) with the naringin be reference substance, liquid chromatography detects the content of naringin in the XIAOER JINDAN prescription;
(7) adopt potentiometric titration, measure the content of cinnabar in the XIAOER JINDAN prescription Cinnabaris.
And said microscopical identification is observed for XIAOER JINDAN being put microscopically: the dark brownish red of irregular fine particle, and glossy, the edge furvous; Stone cell yellowish-brown or colourless, rectangle like, similar round or out-of-shape, the about 94 μ m of diameter; The needle-like calcium oxalate crystal bunchy, long 100～144 μ m are present in the mucilage cell or are dispersed in; Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance; Oil pipe contains pale brown color secretions, the about 100 μ m of diameter; Calcium oxalate sand crystal is present in the parenchyma cell, and crystal cell connection is sometimes embarked on journey; The fiber bunchy, peripheral cell contains prism of calcium oxalate, forms crystalline cellulose, and the wall lignify of crystal cell thickens; Parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose; Oil pipe contains golden yellow secretions, the about 30 μ m of diameter; Irregular fragment canescence or lark are had gloss slightly, and there is the taupe brown pigment granule on the surface, and irregular lengthwise crack is arranged.
And said thin layer chromatography differentiates that the method for the Radix Peucedani composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add kieselguhr 3g, porphyrize adds chloroform 40ml, and supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds chloroform 2ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Radix Peucedani control medicinal material 1g, add chloroform 15ml, process control medicinal material solution with above-mentioned need testing solution method for preparing;
(3) thin layer condition and result: the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 4 μ l; Put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate=3: 1 is developing solvent, launches; Take out, dry, put under the ultra-violet lamp 365nm and inspect; Inspect in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on whether show the fluorescence speckle of same color, and then confirm to supply whether to contain the Radix Peucedani composition in the test agent.
And said thin layer chromatography differentiates that the method for the Fructus Aurantii composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add methanol 30ml, supersound process 30 minutes; Filter, the filtrating evaporate to dryness, residue adds water 20ml makes dissolving; Extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Fructus Aurantii control medicinal material 1g, add methanol 15ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds methanol 1ml makes dissolving, as control medicinal material solution;
(3) preparation of reference substance solution: get the naringin reference substance, add methanol and process the solution that every 1ml contains 1mg, as reference substance solution;
(4) thin layer condition and result: the thin layer chromatography test, draw above-mentioned need testing solution and control medicinal material solution 10 μ l, reference substance solution 4 μ l, put in same silica gel G F respectively
254On the lamellae, with ethyl acetate: butanone: ethanol=12: 5: 1 is developing solvent, launches; Take out, dry, spray is with 5% aluminum chloride alcoholic solution; Heating; Put ultra-violet lamp 254nm down and ultra-violet lamp 365nm inspect, inspect in the test sample chromatograph with control medicinal material and the corresponding position of reference substance chromatograph on whether show the speckle and the fluorescence speckle of same color, and then whether contain Fructus Aurantii and tangerine composition in definite sample.
And said thin layer chromatography differentiates that the method for the Radix Puerariae composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add methanol 30ml, supersound process 30 minutes; Filter, the filtrating evaporate to dryness, residue adds water 20ml makes dissolving; Extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Radix Puerariae control medicinal material 1g, add methanol 15ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds methanol 1ml makes dissolving, as control medicinal material solution;
(3) reference substance solution preparation: get the puerarin reference substance, add methanol and process the solution that every ml contains 1mg, as reference substance solution;
(4) thin layer condition and result: the thin layer chromatography test, draw above-mentioned need testing solution, each 10 μ l of control medicinal material solution, reference substance solution 4 μ l; Put respectively on same silica gel g thin-layer plate, with chloroform: methanol: water=7: 2.5: 0.25 is developing solvent, launches; Take out; Dry, put under the ultra-violet lamp 365nm and inspect, inspect in the test sample chromatograph with control medicinal material and the corresponding position of reference substance chromatograph on whether show the fluorescence speckle of same color.
And said thin layer chromatography differentiates that the step of the windproof composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add kieselguhr 3g, porphyrize adds acetone 40ml, and supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get windproof control medicinal material 1g, add acetone 10ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as control medicinal material solution;
(3) preparation of reference substance solution: get the 5-O-methyl-visamminol reference substance, add methanol and process the solution that every 1ml contains 1mg, as reference substance solution;
(4) thin layer condition and result: the thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put in same silica gel G F respectively
254On the lamellae; With chloroform: methanol=4: 1 is developing solvent, launches, and takes out; Dry; Put under the ultra-violet lamp 254nm and inspect, inspect in the test sample chromatograph with control medicinal material and the corresponding position of reference substance chromatograph on whether show the speckle of same color, and then confirm to supply whether to contain windproof composition in the test agent.
And said is reference substance with the naringin, and the method that liquid chromatography detects the content of naringin in the prescription is:
(1) chromatographic condition: use octadecylsilane chemically bonded silica to be filler; Mobile phase: methanol: water: phosphoric acid=35: 65: 0.05; Column temperature: 35 ℃; Flow velocity: 1ml/min; Detect wavelength: 283nm, number of theoretical plate calculates by the naringin peak and is not less than 3000;
(2) preparation of reference substance solution: it is an amount of to get the naringin reference substance, and accurate the title decides, and adds methanol and processes the solution that every 1ml contains naringin reference substance 0.1mg, shakes up, and promptly gets, and the accurate 10 μ l that draw inject chromatograph of liquid and detect;
(3) preparation of need testing solution: it is an amount of to get the XIAOER JINDAN sample, shreds, and gets 2.5g, and accurate the title decides, and puts in the tool plug conical flask; The accurate methanol 50ml that adds claims to decide weight, and supersound process 30 minutes is put cold; Claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol; Get subsequent filtrate, promptly get, the accurate 10 μ l that draw inject chromatograph of liquid and detect;
(4) formulation of content limit
In the XIAOER JINDAN sample, Fructus Aurantii accounts for 4.17% of prescription total amount, concocts; These article are starch, and dried tangerine peel also contains a small amount of naringin in the side elsewhere, takes all factors into consideration; The naringin rate of transform is calculated by 100% in the Fructus Aurantii; Every 1g contains naringin must not be less than 0.72mg, if calculate according to every ball, contains naringin and must not be less than 1.1mg.
And, said employing potentiometric titration, the method for measuring the content of cinnabar in the XIAOER JINDAN prescription Cinnabaris is:
(1) cinnabar assay in the Cinnabaris
Get the about 0.1g of Cinnabar, totally 6 parts, the accurate title, decide, and puts in the 100ml conical flask; Add sulphuric acid 10ml and potassium nitrate 1.5g, heating makes dissolving, puts coldly, adds water 50ml; Add 1% potassium permanganate solution to showing pink, drip 2% copperas solution again to red color disappeared, with ammonium thiocyanate volumetric solution 0.1047mol/L titration; Every 1ml ammonium thiocyanate volumetric solution 0.1mol/L is equivalent to the cinnabar HgS of 11.63mg, and the meansigma methods of content is 97.48%, and RSD is 0.92%;
(2) confirming of test sample processing method: it is an amount of to get the XIAOER JINDAN sample, shreds, and gets 2g, and accurate the title decides; Put in the 100ml conical flask, add sulphuric acid 20ml, potassium nitrate 2g, heating makes into milky; Put coldly, add water 40ml, drip 1% potassium permanganate solution to showing pink with the degree of being that do not disappear in 2 minutes; Drip 2% copperas solution again to red color disappeared, with ammonium thiocyanate volumetric solution 0.1mol/L titration, every 1ml ammonium thiocyanate volumetric solution 0.1mol/L is equivalent to the cinnabar (HgS) of 11.63mg;
(3) content limit confirms
In the prescription; Cinnabaris accounts for 4.83% of prescription total amount, must not be less than 96.0% regulation according to pharmacopeia to Cinnabaris Containing Sulfur hydrargyrum, and XIAOER JINDAN sample Containing Sulfur hydrargyrum theoretical amount should be 46.38mg/g; In view of these article are big honeyed pills; Fluctuate according to ± 15%, per 1 ball of XIAOER JINDAN sample contains Cinnabaris in cinnabar HgS, should be 60～80mg.
Advantage of the present invention and good effect are:
Detection method of the present invention has increased the microscopical identification method of Cinnabaris in the prescription, Radix Scrophulariae, the Rhizoma Pinelliae, Radix Platycodonis, Rhizoma Et Radix Notopterygii, Ramulus Uncariae Cum Uncis, Radix Puerariae, Radix Glycyrrhizae, windproof and Pulvis Cornus Bubali Concentratus on the primary standard basis; Radix Peucedani, Fructus Aurantii, Radix Puerariae and windproof thin layer discrimination method in the prescription have been increased; With the naringin is quantitative target; Formulated the content assaying method of tangerine and Fructus Aurantii; Revised quality standard; Improved the controllability of XIAOER JINDAN quality standard, further guaranteed 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.
Description of drawings
Fig. 1 supplies the thin-layer chromatogram of Radix Peucedani in the test agent to inspect figure at ultra-violet lamp (365nm) for the present invention; Be followed successively by from left to right: sample 1 (lot number: E518001), sample 2 (lot number: E518002), sample 3 (lot number: 200603); Radix Peucedani control medicinal material (middle inspection institute), negative sample;
Fig. 2, Fig. 3 are respectively the present invention and supply thin-layer chromatogram in Fructus Aurantii in the test agent and tangerine the detection at uviol lamp 254nm, and 365nm inspects figure; Be followed successively by from left to right: sample 1 (lot number: E518001), sample 2 (lot number: E518002), sample 3 (lot number: 200603); Naringin reference substance (middle inspection institute); Negative sample, Fructus Aurantii control medicinal material (middle inspection institute), tangerine medical material;
Fig. 4 inspects figure for the present invention supplies in the test agent Radix Puerariae to detect under ultra-violet lamp (365nm); Be followed successively by from left to right: sample 1 (lot number: E518001); Sample 2 (lot number: E518002), sample 3 (lot number: 200603), Radix Puerariae control medicinal material (middle inspection institute); Puerarin reference substance (middle inspection institute), negative sample;
Fig. 5 inspects figure for the present invention supplies in the test agent windproof detection under ultra-violet lamp (254nm); Be followed successively by from left to right: sample 1 (lot number: E518001); Sample 2 (lot number: E518002), sample 3 (lot number: 200603), windproof control medicinal material (middle inspection institute); 5-O-methyl-visamminol reference substance (middle inspection institute), negative sample;
Fig. 6, Fig. 7 supply the thin-layer chromatogram of the different developing solvents that Radix Scrophulariae detects in the test agent for the present invention; Be followed successively by from left to right: sample 1 (lot number: E518001), sample 2 (lot number: E518002), sample 3 (lot number: 200603); Radix Scrophulariae control medicinal material (middle inspection institute), negative sample;
Fig. 8 is a naringin reference substance chromatogram of the present invention;
Fig. 9 is test sample chromatogram in the naringin detection of the present invention;
Figure 10 is negative sample chromatogram in the naringin detection of the present invention.
The specific embodiment
Below in conjunction with embodiment, the present invention is further specified, 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 XIAOER JINDAN, the step of its method is:
(1) microscopical identification:
These article of getting, put microscopically and observe: the dark brownish red of irregular fine particle, glossy, the edge furvous; Stone cell yellowish-brown or colourless, rectangle like, similar round or out-of-shape, the about 94 μ m of diameter; The needle-like calcium oxalate crystal bunchy, long 100～144 μ m are present in the mucilage cell or are dispersed in; Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance; Oil pipe contains pale brown color secretions, the about 100 μ m of diameter.Calcium oxalate sand crystal is present in the parenchyma cell, and crystal cell connection is sometimes embarked on journey; The fiber bunchy, peripheral cell contains prism of calcium oxalate, forms crystalline cellulose, and the wall lignify of crystal cell thickens; Parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose; Oil pipe contains golden yellow secretions, the about 30 μ m of diameter; Irregular fragment canescence or lark are had gloss slightly, and there is the taupe brown pigment granule on the surface, and irregular lengthwise crack is arranged.
(2) adopt thin layer chromatography, the control medicinal material of acting like a bully is in the past differentiated the Radix Peucedani in the prescription.
1. the preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add kieselguhr 3g, porphyrize adds chloroform 40ml, and supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds chloroform 2ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Radix Peucedani control medicinal material 1g, add chloroform 15ml, process control medicinal material solution with above-mentioned need testing solution method for preparing.
3. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Radix Peucedani, process pill, make negative sample solution by above-mentioned need testing solution method for preparing again by former medicine preparation technology.
4. thin layer condition and result:, draw need testing solution 10 μ l, control medicinal material solution 4 μ l according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test; Negative sample solution 10 μ l put respectively on same silica gel g thin-layer plate, and with petroleum ether (60～90 ℃): ethyl acetate=3: 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, negative sample is noiseless, and the result sees Fig. 1.
(3) adopting thin layer chromatography, is control medicinal material with the Fructus Aurantii, is reference substance with the naringin, differentiates Fructus Aurantii and dried tangerine peel in the prescription.
Seeing that Fructus Aurantii and dried tangerine peel all belong to rutaceae, contain the identical composition of part.Nat'l Pharmaceutical & Biological Products Control Institute does not provide tangerine control medicinal material as yet at present, so with reference to " related content of Chinese pharmacopoeia version in 2005 adopts thin layer chromatography, is control medicinal material with the Fructus Aurantii, is reference substance with the naringin, and the Fructus Aurantii in the discriminating prescription is with tangerine.
1. the preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add methanol 30ml, supersound process 30 minutes; Filter, the filtrating evaporate to dryness, residue adds water 20ml makes dissolving; Extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Fructus Aurantii control medicinal material 1g, add methanol 15ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds methanol 1ml makes dissolving, as control medicinal material solution.
3. the preparation of reference substance solution: get the naringin reference substance, add methanol and process the solution that every 1ml contains 1mg, as reference substance solution.
4. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Fructus Aurantii and dried tangerine peel, process pill, make negative sample solution by above-mentioned need testing solution method for preparing again by former medicine preparation technology.
5. thin layer condition and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw above-mentioned need testing solution and control medicinal material solution 10 μ l, reference substance solution 4 μ l, put in same silica gel G F respectively
254On the lamellae, with ethyl acetate: butanone: ethanol=12: 5: 1 is developing solvent, launches, and takes out, and dries, and spray is with 5% aluminum chloride alcoholic solution, and heating is put and reached ultra-violet lamp (365nm) ultra-violet lamp (254nm) under and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle and the fluorescence speckle of same color, negative sample is noiseless.The result sees Fig. 2, Fig. 3.
(4) adopting thin layer chromatography, is control medicinal material with the Radix Puerariae, is reference substance with the puerarin, differentiates the Radix Puerariae in the prescription.
1. the preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add methanol 30ml, supersound process 30 minutes; Filter, the filtrating evaporate to dryness, residue adds water 20ml makes dissolving; Extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Radix Puerariae control medicinal material 1g, add methanol 15ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds methanol 1ml makes dissolving, as control medicinal material solution.
3. reference substance solution preparation: get the puerarin reference substance, add methanol and process the solution that every ml contains 1mg, as reference substance solution.
4. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Radix Puerariae, process pill, make negative sample solution by above-mentioned need testing solution method for preparing again by former medicine preparation technology.
5. thin layer condition and result:, draw each 10 μ l of above-mentioned need testing solution, negative sample solution and control medicinal material solution, reference substance solution 4 μ l 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: methanol: water=7: 2.5: 0.25 is developing solvent, launches, and takes out; Dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.Negative sample is noiseless, and the result sees Fig. 4.
(5) adopting thin layer chromatography, is control medicinal material with windproof, and 5-O-methyl-visamminol is a reference substance, differentiates windproof in the prescription.
1. the preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add kieselguhr 3g, porphyrize adds acetone 40ml, and supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get windproof control medicinal material 1g, add acetone 10ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as control medicinal material solution.
3. the preparation of reference substance solution: get the 5-O-methyl-visamminol reference substance, add methanol and process the solution that every 1ml contains 1mg, as reference substance solution.
4. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that windproof, process pill, make negative sample solution by above-mentioned need testing solution method for preparing again by former medicine preparation technology.
5. thin layer condition and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 10 μ l of above-mentioned four kinds of solution, put in same silica gel G F respectively
254On the lamellae, be developing solvent, launch, take out, dry, put under the ultra-violet lamp 254nm and inspect with chloroform-methanol (4: 1).In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.Negative sample is noiseless, and the result sees Fig. 4.
(6) adopting thin layer chromatography, is control medicinal material with the Radix Scrophulariae, differentiates the Radix Scrophulariae in the prescription.
1. the preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add water 40ml, heating makes dissolving; Put coldly, filter, filtrating is extracted 2 times with the ether jolting, at every turn 20ml; Discard ether solution, water liquid extracts with water saturated n-butyl alcohol 40ml jolting, obtains n-butyl alcohol liquid; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Radix Scrophulariae control medicinal material 2.5g, add ethanol 50ml, reflux 1 hour filters, the filtrating evaporate to dryness, and residue adds water 30ml makes dissolving, shines medical material solution in pairs with legal system.
3. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Radix Scrophulariae, process pill, make negative sample solution by above-mentioned need testing solution method for preparing again by former medicine preparation technology.
4. thin layer condition and result:
A, according to 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 chloroform: methanol=5: 1 is developing solvent; Launch, take out, dry, spray is with 5% vanillin sulfuric acid solution; It is clear to be heated to speckle colour developing, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on; Do not show identical speckle, negative sample is noiseless, and the result sees Fig. 6.
B, according to 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; Chloroform: methanol: water=13: 7: 2 is developing solvent at 10 ℃ with the stratified lower floor of held solution, launches, and takes out; Dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, do not show identical speckle; Negative sample is noiseless, and the result sees Fig. 7.
(7) with the naringin be reference substance, liquid chromatography detects the content of naringin in the prescription
1. chromatographic condition: with reference to " relevant content assaying method of Chinese pharmacopoeia version in 2005 is formulated.Use octadecylsilane chemically bonded silica to be filler; Mobile phase: methanol: water: phosphoric acid=35: 65: 0.05; Column temperature: 35 ℃; Flow velocity: 1ml/min; Detect wavelength: 283nm, number of theoretical plate calculates by the naringin peak and is not less than 3000.
2. the preparation of reference substance solution: it is an amount of to get the naringin reference substance, and accurate the title decides, and adds methanol and processes the solution that every 1ml contains naringin reference substance 0.1mg, shakes up, and promptly gets, and the accurate 10 μ l that draw inject chromatograph of liquid, and the result sees Fig. 8.
3. the preparation of need testing solution: it is an amount of to get the XIAOER JINDAN sample, shreds, and gets 2.5g, and accurate the title decides, and puts in the tool plug conical flask; The accurate methanol 50ml that adds claims to decide weight, and supersound process (power 50W, frequency 50kHz) 30 minutes is put cold; Claim again to decide weight, supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate with methanol; Promptly get, the accurate 10 μ l that draw inject chromatograph of liquid, and the result sees Fig. 9.
4. the preparation of negative sample solution: get the medical material of respectively distinguishing the flavor of that removes tangerine and Fructus Aurantii by prescription, make sample, by " 3. " need testing solution method for preparing in this step, make negative sample solution again by former medicine preparation technology.The accurate 10 μ l that draw inject chromatograph of liquid.With the corresponding retention time of naringin reference substance chromatographic peak place, no chromatographic peak occurs, and negative sample is noiseless.The result sees Figure 10.
5. the formulation of content limit
In the prescription, Fructus Aurantii accounts for 4.17% of prescription total amount, concocts; In view of these article are starch, dried tangerine peel also contains a small amount of naringin in the side elsewhere, takes all factors into consideration; The naringin rate of transform is by 100% calculating (" content limit calculates under Fructus Aurantii item of Chinese pharmacopoeia version in 2005) in the Fructus Aurantii; Every 1g contains naringin must not be less than 0.72mg, if calculate according to every ball, contains naringin and must not be less than 1.1mg.
(8) adopt potentiometric titration, measure the content of cinnabar in the XIAOER JINDAN prescription Cinnabaris.
1. constant-current titration
Principle: this method is to utilize the hop of current potential to confirm titration end-point, and the result judges accurately.
2. cinnabar assay in the Cinnabaris
Get the about 0.1g of Cinnabar, totally 6 parts, the accurate title, decide; Put in the 100ml conical flask, add sulphuric acid 10ml and potassium nitrate 1.5g, heating makes dissolving; Put coldly, add water 50ml, add 1% potassium permanganate solution to showing pink; Drip 2% copperas solution again to red color disappeared, with ammonium thiocyanate volumetric solution (0.1047mol/L) titration.Every 1ml ammonium thiocyanate volumetric solution (0.1mol/L) is equivalent to the cinnabar (HgS) of 11.63mg, and the meansigma methods of content is 97.48%, and RSD is 0.92%, and the result sees table 1.
3. the test sample processing method is definite: it is an amount of to get the XIAOER JINDAN sample, shreds, and gets 2g, and accurate the title decides; Put in the 100ml conical flask, add sulphuric acid 20ml, potassium nitrate 2g; Heating makes into milky, puts coldly, adds water 40ml; Drip 1% potassium permanganate solution to showing pink, drip 2% copperas solution again to red color disappeared, with ammonium thiocyanate volumetric solution (0.1mol/L) titration with the degree of being that do not disappear in 2 minutes.Every 1ml ammonium thiocyanate volumetric solution (0.1mol/L) is equivalent to the cinnabar (HgS) of 11.63mg.
4. blank assay: by " 2. " method, do not add sample and measure, two parts of consume sulfur ammonium cyanates of result volumetric solution is 0.02ml according to 0.1mol/L ammonium thiocyanate meter.
5. negative sample test: by the proportioning of prescription; Get each flavour of a drug that removes Cinnabaris; Make sample by former medicine preparation technology; Measure by the processing method of " 3. " test sample in this step, it is 0.02ml that the result consumes 0.1mol/L ammonium thiocyanate volumetric solution, shows that negative sample does not have obvious influence to the quantitative assay of Cinnabaris again.
6. content limit confirms
In the prescription; Cinnabaris accounts for 4.83% of prescription total amount (honey is than 100/130), must not be less than 96.0% regulation according to pharmacopeia to Cinnabaris Containing Sulfur hydrargyrum, and XIAOER JINDAN sample Containing Sulfur hydrargyrum theoretical amount should be 46.38mg/g; In view of these article are big honeyed pills; Fluctuate according to ± 15%, per 1 ball of XIAOER JINDAN sample contains Cinnabaris in cinnabar (HgS), should be 60～80mg.
Cinnabar assay result in table 1 Cinnabaris
Claims (1)
1. the detection method of a Chinese medicine preparation XIAOER JINDAN, it is characterized in that: the step of its method is:
(1) microscopical identification;
(2) the former control medicinal material of acting like a bully, thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain the Radix Peucedani composition;
(3) being control medicinal material with the Fructus Aurantii, is reference substance with the naringin, and thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain the Fructus Aurantii composition;
(4) being control medicinal material with the Radix Puerariae, is reference substance with the puerarin, and thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain the Radix Puerariae composition;
(5) with windproof be control medicinal material, 5-0-methyl visamminol glycosides is a reference substance, and thin layer chromatography differentiates in the XIAOER JINDAN prescription whether contain windproof composition;
(6) with the naringin be reference substance, liquid chromatography detects the content of naringin in the XIAOER JINDAN prescription;
(7) adopt potentiometric titration, measure the content of cinnabar in the XIAOER JINDAN prescription Cinnabaris;
Said microscopical identification is observed for XIAOER JINDAN being put microscopically: the dark brownish red of irregular fine particle, and glossy, the edge furvous; Stone cell yellowish-brown or colourless, rectangle like, similar round or out-of-shape, the about 94 μ m of diameter; The needle-like calcium oxalate crystal bunchy, long 100～144 μ m are present in the mucilage cell or are dispersed in; Connect latex dust diameter 14～25 μ m, contain faint yellow granular substance; Oil pipe contains pale brown color secretions, the about 100 μ m of diameter; Calcium oxalate sand crystal is present in the parenchyma cell, and crystal cell connection is sometimes embarked on journey; The fiber bunchy, peripheral cell contains prism of calcium oxalate, forms crystalline cellulose, and the wall lignify of crystal cell thickens; Parenchyma cell contains prism of calcium oxalate around the fibre bundle, forms crystalline cellulose; Oil pipe contains golden yellow secretions, the about 30 μ m of diameter; Irregular fragment canescence or lark are had gloss slightly, and there is the taupe brown pigment granule on the surface, and irregular lengthwise crack is arranged;
Said thin layer chromatography differentiates that the method for the Radix Peucedani composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add kieselguhr 3g, porphyrize adds chloroform 40ml, and supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds chloroform 2ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Radix Peucedani control medicinal material 1g, add chloroform 15ml, process control medicinal material solution with above-mentioned need testing solution method for preparing;
(3) thin layer condition and result: the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 4 μ l; Put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate=3: 1 is developing solvent, launches; Take out, dry, put under the ultra-violet lamp 365nm and inspect; Inspect in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on whether show the fluorescence speckle of same color, and then confirm to supply whether to contain the Radix Peucedani composition in the test agent;
Said thin layer chromatography differentiates that the method for the Fructus Aurantii composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add methanol 30ml, supersound process 30 minutes; Filter, the filtrating evaporate to dryness, residue adds water 20ml makes dissolving; Extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Fructus Aurantii control medicinal material 1g, add methanol 15ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds methanol 1ml makes dissolving, as control medicinal material solution;
(3) preparation of reference substance solution: get the naringin reference substance, add methanol and process the solution that every 1ml contains 1mg, as reference substance solution;
(4) thin layer condition and result: the thin layer chromatography test, draw above-mentioned need testing solution and control medicinal material solution 10 μ l, reference substance solution 4 μ l, put in same silica gel G F respectively
254On the lamellae, with ethyl acetate: butanone: ethanol=12: 5: 1 is developing solvent, launches; Take out, dry, spray is with 5% aluminum chloride alcoholic solution; Heating; Put ultra-violet lamp 254nm down and ultra-violet lamp 365nm inspect, inspect in the test sample chromatograph with control medicinal material and the corresponding position of reference substance chromatograph on whether show the speckle and the fluorescence speckle of same color, and then whether contain Fructus Aurantii and tangerine composition in definite sample;
Said thin layer chromatography differentiates that the method for the Radix Puerariae composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add methanol 30ml, supersound process 30 minutes; Filter, the filtrating evaporate to dryness, residue adds water 20ml makes dissolving; Extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get Radix Puerariae control medicinal material 1g, add methanol 15ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds methanol 1ml makes dissolving, as control medicinal material solution;
(3) reference substance solution preparation: get the puerarin reference substance, add methanol and process the solution that every ml contains 1mg, as reference substance solution;
(4) thin layer condition and result: the thin layer chromatography test, draw above-mentioned need testing solution, each 10 μ l of control medicinal material solution, reference substance solution 4 μ l; Put respectively on same silica gel g thin-layer plate, with chloroform: methanol: water=7: 2.5: 0.25 is developing solvent, launches; Take out; Dry, put under the ultra-violet lamp 365nm and inspect, inspect in the test sample chromatograph with control medicinal material and the corresponding position of reference substance chromatograph on whether show the fluorescence speckle of same color;
Said thin layer chromatography differentiates that the step of the windproof composition in the prescription is:
(1) preparation of need testing solution: get XIAOER JINDAN sample 10g, shred, add kieselguhr 3g, porphyrize adds acetone 40ml, and supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as need testing solution;
(2) preparation of control medicinal material solution: get windproof control medicinal material 1g, add acetone 10ml, supersound process 30 minutes filters, the filtrating evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as control medicinal material solution;
(3) preparation of reference substance solution: get the 5-O-methyl-visamminol reference substance, add methanol and process the solution that every 1ml contains 1mg, as reference substance solution;
(4) thin layer condition and result: the thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put in same silica gel G F respectively
254On the lamellae; With chloroform: methanol=4: 1 is developing solvent, launches, and takes out; Dry; Put under the ultra-violet lamp 254nm and inspect, inspect in the test sample chromatograph with control medicinal material and the corresponding position of reference substance chromatograph on whether show the speckle of same color, and then confirm to supply whether to contain windproof composition in the test agent;
Said is reference substance with the naringin, and the method that liquid chromatography detects the content of naringin in the prescription is:
(1) chromatographic condition: use octadecylsilane chemically bonded silica to be filler; Mobile phase: methanol: water: phosphoric acid=35: 65: 0.05; Column temperature: 35 ℃; Flow velocity: 1ml/min; Detect wavelength: 283nm, number of theoretical plate calculates by the naringin peak and is not less than 3000;
(2) preparation of reference substance solution: it is an amount of to get the naringin reference substance, and accurate the title decides, and adds methanol and processes the solution that every 1ml contains naringin reference substance 0.1mg, shakes up, and promptly gets, and the accurate 10 μ l that draw inject chromatograph of liquid and detect;
(3) preparation of need testing solution: it is an amount of to get the XIAOER JINDAN sample, shreds, and gets 2.5g, and accurate the title decides, and puts in the tool plug conical flask; The accurate methanol 50ml that adds claims to decide weight, and supersound process 30 minutes is put cold; Claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol; Get subsequent filtrate, promptly get, the accurate 10 μ l that draw inject chromatograph of liquid and detect;
(4) formulation of content limit
In the XIAOER JINDAN sample, Fructus Aurantii accounts for 4.17% of prescription total amount, concocts; These article are starch, and dried tangerine peel also contains a small amount of naringin in the side elsewhere, takes all factors into consideration; The naringin rate of transform is calculated by 100% in the Fructus Aurantii; Every 1g contains naringin must not be less than 0.72mg, if calculate according to every ball, contains naringin and must not be less than 1.1mg;
Said employing potentiometric titration, the method for measuring the content of cinnabar in the XIAOER JINDAN prescription Cinnabaris is:
(1) cinnabar assay in the Cinnabaris
Get the about 0.1g of Cinnabar, totally 6 parts, the accurate title, decide, and puts in the 100ml conical flask; Add sulphuric acid 10ml and potassium nitrate 1.5g, heating makes dissolving, puts coldly, adds water 50ml; Add 1% potassium permanganate solution to showing pink, drip 2% copperas solution again to red color disappeared, with ammonium thiocyanate volumetric solution 0.1047mol/L titration; Every 1ml ammonium thiocyanate volumetric solution 0.1mol/L is equivalent to the cinnabar HgS of 11.63mg, and the meansigma methods of content is 97.48%, and RSD is 0.92%;
(2) confirming of test sample processing method: it is an amount of to get the XIAOER JINDAN sample, shreds, and gets 2g, and accurate the title decides; Put in the 100ml conical flask, add sulphuric acid 20ml, potassium nitrate 2g, heating makes into milky; Put coldly, add water 40ml, drip 1% potassium permanganate solution to showing pink with the degree of being that do not disappear in 2 minutes; Drip 2% copperas solution again to red color disappeared, with ammonium thiocyanate volumetric solution 0.1mol/L titration, every 1ml ammonium thiocyanate volumetric solution 0.1mol/L is equivalent to the cinnabar of 11.63mg;
(3) content limit confirms
In the prescription; Cinnabaris accounts for 4.83% of prescription total amount, must not be less than 96.0% regulation according to pharmacopeia to Cinnabaris Containing Sulfur hydrargyrum, and XIAOER JINDAN sample Containing Sulfur hydrargyrum theoretical amount should be 46.38mg/g; In view of these article are big honeyed pills; Fluctuate according to ± 15%, per 1 ball of XIAOER JINDAN sample contains Cinnabaris in cinnabar HgS, should be 60～80mg;
Said XIAOER JINDAN is made up of Cinnabaris, dried tangerine peel, Bulbus Fritillariae Ussuriensis, Arisaema Cum Bile, Radix Peucedani, Radix Scrophulariae, the Rhizoma Pinelliae, Folium Isatidis, Caulis Akebiae, Radix Platycodonis, Herba Schizonepetae, Rhizoma Et Radix Notopterygii, Cacumen Tamaricis, Radix Rehmanniae, Fructus Aurantii, Radix Paeoniae Rubra, Ramulus Uncariae Cum Uncis, Radix Puerariae, Fructus Arctii, Rhizoma Gastrodiae, Radix Glycyrrhizae, windproof, Borneolum Syntheticum, Pulvis Cornus Bubali Concentratus, Cornu Saigae Tataricae, Herba Menthae; Method for preparing: above 20 Six-elements; The Cornu Saigae Tataricae file is ground into fine powder; Pulvis Cornus Bubali Concentratus, Borneolum Syntheticum are ground into fine powder, and Cinnabaris water flies into impalpable powder; 22 flavors such as all the other Bulbus Fritillariae Ussuriensiss are ground into fine powder, sieve; With powder facing-ups such as Cornu Saigae Tataricae powder, Pulvis Cornus Bubali Concentratus, Borneolum Syntheticum, Cinnabaris fine powder and Bulbus Fritillariae Cirrhosaes, sieve, mixing, every 100g powder add refined honey 120～140g and process big honeyed pills, promptly get.
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