CN102475727B - Detection method of external Pianzaihuang preparation - Google Patents
Detection method of external Pianzaihuang preparation Download PDFInfo
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- CN102475727B CN102475727B CN2009100923928A CN200910092392A CN102475727B CN 102475727 B CN102475727 B CN 102475727B CN 2009100923928 A CN2009100923928 A CN 2009100923928A CN 200910092392 A CN200910092392 A CN 200910092392A CN 102475727 B CN102475727 B CN 102475727B
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- ginsenoside
- pien tze
- tze huang
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- 238000002360 preparation method Methods 0.000 title claims abstract description 64
- 238000001514 detection method Methods 0.000 title claims abstract description 19
- 239000013558 reference substance Substances 0.000 claims abstract description 67
- 238000012360 testing method Methods 0.000 claims abstract description 45
- YURJSTAIMNSZAE-HHNZYBFYSA-N ginsenoside Rg1 Chemical compound O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O YURJSTAIMNSZAE-HHNZYBFYSA-N 0.000 claims abstract description 38
- YURJSTAIMNSZAE-UHFFFAOYSA-N UNPD89172 Natural products C1CC(C2(CC(C3C(C)(C)C(O)CCC3(C)C2CC2O)OC3C(C(O)C(O)C(CO)O3)O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O YURJSTAIMNSZAE-UHFFFAOYSA-N 0.000 claims abstract description 36
- CBEHEBUBNAGGKC-UHFFFAOYSA-N ginsenoside Rg1 Natural products CC(=CCCC(C)(OC1OC(CO)C(O)C(O)C1O)C2CCC3(C)C2C(O)CC4C5(C)CCC(O)C(C)(C)C5CC(OC6OC(CO)C(O)C(O)C6O)C34C)C CBEHEBUBNAGGKC-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 34
- UFNDONGOJKNAES-UHFFFAOYSA-N Ginsenoside Rb1 Natural products CC(=CCCC(C)(OC1OC(COC2OC(CO)C(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CC(O)C45C)C UFNDONGOJKNAES-UHFFFAOYSA-N 0.000 claims abstract description 28
- GZYPWOGIYAIIPV-JBDTYSNRSA-N ginsenoside Rb1 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GZYPWOGIYAIIPV-JBDTYSNRSA-N 0.000 claims abstract description 28
- TXEWRVNOAJOINC-UHFFFAOYSA-N ginsenoside Rb2 Natural products CC(=CCCC(OC1OC(COC2OCC(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CCC45C)C TXEWRVNOAJOINC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 22
- KXGVEGMKQFWNSR-UHFFFAOYSA-N deoxycholic acid Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)C(O)C2 KXGVEGMKQFWNSR-UHFFFAOYSA-N 0.000 claims abstract description 14
- BHQCQFFYRZLCQQ-UHFFFAOYSA-N (3alpha,5alpha,7alpha,12alpha)-3,7,12-trihydroxy-cholan-24-oic acid Natural products OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)C(O)C2 BHQCQFFYRZLCQQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004380 Cholic acid Substances 0.000 claims abstract description 13
- BHQCQFFYRZLCQQ-OELDTZBJSA-N cholic acid Chemical compound C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(O)=O)C)[C@@]2(C)[C@@H](O)C1 BHQCQFFYRZLCQQ-OELDTZBJSA-N 0.000 claims abstract description 13
- 235000019416 cholic acid Nutrition 0.000 claims abstract description 13
- 229960002471 cholic acid Drugs 0.000 claims abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N methyl alcohol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 105
- 239000000243 solution Substances 0.000 claims description 67
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 26
- 229930182494 ginsenoside Natural products 0.000 claims description 23
- 229940089161 ginsenoside Drugs 0.000 claims description 23
- 239000012467 final product Substances 0.000 claims description 22
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 230000002303 anti-venom Effects 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000003556 assay Methods 0.000 claims description 14
- 239000003814 drug Substances 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 10
- 238000004811 liquid chromatography Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000004587 chromatography analysis Methods 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 7
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 229940079593 drug Drugs 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 208000004078 Snake Bites Diseases 0.000 claims description 4
- 239000000729 antidote Substances 0.000 claims description 4
- 239000004264 Petrolatum Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004945 emulsification Methods 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002674 ointment Substances 0.000 claims description 3
- 229940066842 petrolatum Drugs 0.000 claims description 3
- 235000019271 petrolatum Nutrition 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 claims 2
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 claims 2
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 claims 2
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000001228 spectrum Methods 0.000 abstract 2
- LLPWNQMSUYAGQI-QBQUQATFSA-N Ginsenoside R1 Natural products O([C@](CC/C=C(\C)/C)(C)[C@@H]1[C@H]2[C@@H](O)C[C@H]3[C@](C)([C@]2(C)CC1)C[C@H](O[C@@H]1[C@H](O[C@@H]2[C@@H](O)[C@@H](O)[C@@H](O)CO2)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@H]1C(C)(C)[C@@H](O)CC[C@]31C)[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O1 LLPWNQMSUYAGQI-QBQUQATFSA-N 0.000 abstract 1
- KXGVEGMKQFWNSR-LLQZFEROSA-N deoxycholic acid Chemical compound C([C@H]1CC2)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(O)=O)C)[C@@]2(C)[C@@H](O)C1 KXGVEGMKQFWNSR-LLQZFEROSA-N 0.000 abstract 1
- 229960003964 deoxycholic acid Drugs 0.000 abstract 1
- LLPWNQMSUYAGQI-OOSPGMBYSA-N notoginsenoside R1 Chemical compound O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)CO2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O LLPWNQMSUYAGQI-OOSPGMBYSA-N 0.000 abstract 1
- JURZHOVRCOWZFN-UHFFFAOYSA-N notoginsenoside R1 Natural products CC(=CCCC(C)(OC1OC(CO)C(O)C(O)C1O)C2CCC3(C)C2C(O)CC4C5(C)CCC(O)C(C)(C)C5C(CC34C)OC6OC(COC7OCC(O)C(O)C7O)C(O)C(O)C6O)C JURZHOVRCOWZFN-UHFFFAOYSA-N 0.000 abstract 1
- 238000004809 thin layer chromatography Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- -1 dry Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 235000003143 Panax notoginseng Nutrition 0.000 description 2
- 241000180649 Panax notoginseng Species 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229940040145 liniment Drugs 0.000 description 2
- 239000000865 liniment Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229930182490 saponin Natural products 0.000 description 2
- 150000007949 saponins Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 235000003181 Panax pseudoginseng Nutrition 0.000 description 1
- 244000131316 Panax pseudoginseng Species 0.000 description 1
- ZMZINYUKVRMNTG-UHFFFAOYSA-N acetic acid;formic acid Chemical compound OC=O.CC(O)=O ZMZINYUKVRMNTG-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- VNFPBHJOKIVQEB-UHFFFAOYSA-N clotrimazole Chemical compound ClC1=CC=CC=C1C(N1C=NC=C1)(C=1C=CC=CC=1)C1=CC=CC=C1 VNFPBHJOKIVQEB-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 229940098465 tincture Drugs 0.000 description 1
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Abstract
The invention discloses a quality detection method of Pianzaihuang. The quality detection method of the Pianzaihuang is characterized by comprising identification and content determination, wherein the identification comprises the following steps of: preparing a test product solution from Pianzaihuang fine powder; further taking ginsenoside Rb1, ginsenoside Rg1, notoginsenoside R1 or cholic acid and deoxycholic acid to prepare a reference substance solution; and testing according to a thin-layer chromatography method (Appendix VI B of Part 1 of Chinese Pharmacopoeia 2005) and respectively showing spots in the same color in corresponding positions of color spectrums of reference medicinal materials and reference substances in the color spectrum of a test product; and the content determination comprises the following step of: determining according to a high performance liquid chromatography method, wherein the total amount of the ginsenoside Rg1 (C42H72O14) and the ginsenoside Rb1 (C21H28N2O2.2HCl) in each gram of an external Pianzaihuang preparation is not less than 0.70mg.
Description
Technical field
The present invention relates to a kind of detection method of pharmaceutical composition, particularly the detection method of Chinese medicine Pien Tze Huang external preparation.
Background technology
The Pien Tze Huang external preparation is that produce without competition in the whole nation and middle subject matter insured kind recorded that (standard number: WS3-B-3441-98), the quality determining method that will possess better stability, reappearance and specificity of still needing is at present effectively controlled the quality of this kind in " the 18 of the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation " in 1998.
Summary of the invention
The object of the invention is to provide the detection method of Chinese medicine Pien Tze Huang external preparation.
The present invention seeks to be achieved through the following technical solutions:
Pien Tze Huang external preparation detection method comprises one or more in following discriminating and the assay:
Differentiate: get Pien Tze Huang external preparation 3-8g, put in the tool plug conical flask, add absolute ethyl alcohol 5-15ml, jolting makes and leaches, ultrasonic processing was put in the ice bath and is cooled off after 25-35 minute, took out, and filtered rapidly, get filtrate 3-6ml, water-bath is concentrated into 1-2ml, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take normal hexane-ethyl acetate-acetic acid-methyl alcohol (18-22: 22-27: 1-3: 2-4) as developping agent, launch, take out, dry, spray is with 10% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
Assay: ginsenoside Rg1, ginsenoside Rb1 measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, carry out gradient elution (seeing the following form), from 0 to 75 minute acetonitrile-0.2% phosphoric acid (15: 85) → (35: 65), from 75 to 95 minutes acetonitrile-0.2% phosphoric acid (35: 65) → (70: 30); 20 ℃ of column temperatures; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000.
The ginsenoside Rg is got in the preparation of reference substance solution
1Reference substance and ginsenoside Rb
1Reference substance is an amount of, and is accurately weighed, makes the mixed solution that every 1ml contains ginsenoside Rg1 0.1mg, ginsenoside Rb1 0.1mg with methyl alcohol, and get final product; Pien Tze Huang external preparation 4-8g is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 20-40ml, ultrasonic processing 20-40 minute, jolting makes and is uniformly dispersed, and adds hot reflux 0.5-1 hour, takes out, put in the ice bath and cool off, filter rapidly in the 50ml measuring bottle, with methanol wash for several times, be placed to room temperature,, shake up to scale with methyl alcohol, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains ginsenoside Rg1 (C42H72O14) and ginsenoside Rb1's (C21H28N2O22HCl) total amount meter, must not be less than 0.70mg.
Quality determining method of the present invention is preferably as follows one or more of discriminating and/or assay:
Differentiate: get Pien Tze Huang external preparation 5g, put in the tool plug conical flask, add absolute ethyl alcohol 10ml, jolting makes and leaches, and ultrasonic processing was put in the ice bath and cooled off 30 minutes after 30 minutes, took out, and filtered rapidly, got filtrate 4ml, and water-bath is concentrated into 2ml, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (20: 25: 2: 3) as developping agent, expansion was taken out take normal hexane-ethyl acetate-acetic acid-methyl alcohol, dry, spray is with 10% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color respectively.
Assay: ginsenoside Rg1, ginsenoside Rb1 measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, carry out gradient elution, from 0 to 75 minute acetonitrile-0.2% phosphoric acid (15: 85) → (35: 65), from 75 to 95 minutes acetonitrile-0.2% phosphoric acid (35: 65) → (70: 30); 20 ℃ of column temperatures; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000.
Ginsenoside Rg1's reference substance is got in the preparation of reference substance solution and ginsenoside Rb1's reference substance is an amount of, and is accurately weighed, makes the mixed solution that every 1ml contains ginsenoside Rg1 0.1mg, ginsenoside Rb1 0.1mg with methyl alcohol, and get final product; The about 6g of Pien Tze Huang external preparation is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 30ml, ultrasonic processing (power 250W, frequency 33kHz) 30 minutes, jolting made and is uniformly dispersed, and added hot reflux 1 hour, take out, put in the ice bath and cooled off 20 minutes, filter rapidly in the 50ml measuring bottle, with methanol wash for several times, be placed to room temperature, with methyl alcohol to scale, shake up, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains ginsenoside Rg1 (C42H72O14) and ginsenoside Rb1's (C21H28N2O22HCl) total amount meter, must not be less than 0.70mg.
Pien Tze Huang external preparation of the present invention is comprised of the bulk drug of following weight portion:
Pien Tze Huang powder 220～450 weight portions, antivenom tablet 200～500 weight portions.
Traditional Chinese medicinal composition raw materials of the present invention is preferably as follows weight portion:
Pien Tze Huang powder 250 weight portions, antivenom tablet 450 weight portions; Or
Pien Tze Huang powder 330 weight portions, antivenom tablet 350 weight portions; Or
Pien Tze Huang powder 400 weight portions, antivenom tablet 250 weight portions.
Described Pien Tze Huang powder and antivenom tablet all can be buied from market.Described antivenom tablet refers to jidesheng sheyao tablets, records in the 15 107 pages of Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparations, standard number: WS3-B-2914-98.
Get the invention described above traditional Chinese medicinal composition raw materials, technique routinely adds or does not add conventional auxiliary material and is prepared into clinical acceptable any exterior-applied formulation, such as paste, liniment, film or tincture etc.
The preparation method of Pien Tze Huang external preparation ointment of the present invention is:
Take by weighing by weight proportion the Pien Tze Huang powder, antivenom tablet; The Pien Tze Huang powder, dissolving, for subsequent use; Antivenom tablet extracted 1-3 hour, and it is for subsequent use to get supernatant; Take by weighing glycerine 750～1100 weight portions, triethanolamine 60～100 weight portions, drop into the water material-compound tank, add the supernatant that antidote for snakebite extracts, be heated to boiling, add while stirring above-mentioned Pien Tze Huang powder liquid, again be heated to boiling, be mixed into water, for subsequent use; Take by weighing albolene 850～1200 weight portions, stearic acid 200～420 weight portions, light liquid petrolatum 500～750 weight portions, drop into the oil phase material-compound tank, be heated to whole fusings, stir evenly, for subsequent use; Cooling after oil phase and the water emulsification evenly, discharging; Can namely gets paste.
Description of drawings:
Fig. 1: the thin-layer chromatogram of cholic acid, deoxycholic aicd in the compound Pien Tze Huang external preparation;
Fig. 2: Panax Notoginseng saponin R
1Reference substance, compound Pien Tze Huang external preparation sample chromatogram figure;
Fig. 3: ginsenoside Rg
1And Rb
1Reference substance, compound Pien Tze Huang external preparation sample chromatogram figure
Fig. 4: ginsenoside canonical plotting
Following experiment and embodiment are used for further specifying but are not limited to the present invention.
Experimental example 1 is differentiated
The effects is that 10g/ props up with the specification of sample;
(10 * 20cm): the laboratory is from making sheet, 500 μ m, 105 ℃ of activation 30min for thin layer plate.
In the test sample chromatogram, with cholic acid, the corresponding position of deoxycholic aicd reference substance chromatogram on, the spot of aobvious same color, negative noiseless, method is feasible.The results are shown in Figure 1.
1, sample (lot number: 081009)
2, sample (lot number: 081110)
3, sample (lot number: 081111)
4, lack cholic acid, deoxycholic aicd and antivenom tablet negative sample (source: producer provides)
5, cholic acid reference substance (lot number: 100078-200414 source: Nat'l Pharmaceutical ﹠ Biological Products Control Institute)
6, deoxycholic aicd reference substance (lot number: 110724-200207 source: Nat'l Pharmaceutical ﹠ Biological Products Control Institute)
7, cholic acid, deoxycholic aicd mixing reference substance
Experimental example 2 assays
1 instrument and reagent
Waters high performance liquid chromatograph e2695-2998.Ultrasonic cleaner (model: KQ-300 type, city of Kunshan Instr Ltd.).Chromatographic column: Waters SunFire
TMC18 5 μ m 4.6 * 250mm.The ginsenoside Rg
1Reference substance and ginsenoside Rb
1Reference substance is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.The methodology checking adopts compound Pien Tze Huang external preparation sample lot number to be: 081009.
2 assay indexs
Find Panax Notoginseng saponin R in the sample according to the high efficiency liquid phase experimental result
1Content lower, its peak area and ginsenoside Rg under the same sample concentration
1And Rb
1Peak area differ large (retention time: R
1=31.466minRg
1=35.083min Rb
1=65.430min; Peak area: R
1=38495 Rg
1=221890 Rb
1=162336, see Fig. 2), and degree of separation neither be fine, not yet reaches baseline separation, thinks that the pseudo-ginseng content of sample is with the ginsenoside Rg
1With ginsenoside Rb
1The total amount meter be rational.
The preparation of 3 reference substance solution
Because the peak area of reference substance is that the twice of sample peak area is many, so will " adding methyl alcohol makes every 1ml and contain 0.15mgRg
1And 0.15mgRb
1Mixed solution ... " change that " adding methyl alcohol makes every 1ml and contain 0.1mgRg into
1And 0.1mgRb
1Mixed solution ... "
4. the methodological study checkings such as repeatability, stability and the recovery.
4.1 specificity experiment:
In the test sample chromatogram, with the ginsenoside Rg
1And Rb
1Reference substance chromatographic retention corresponding position is identical chromatographic peak, the results are shown in Figure 3.The method is feasible.
4.2 linear
Precision takes by weighing the ginsenoside Rg respectively
1Reference substance and ginsenoside Rb
1Reference substance is an amount of, adds the methyl alcohol dissolving, makes every 1ml and contains the ginsenoside Rg
10.2152mg and ginsenoside Rb
10.1944mg mix reference substance solution (I).Accurate reference substance solution (I) 1ml that draws puts in the 10ml measuring bottle, adds methyl alcohol and is diluted to scale mark, shakes up namely to get to mix reference substance solution (II).Accurate reference substance solution (II) 1ml that draws puts in the 10ml measuring bottle, adds methyl alcohol and is diluted to scale mark, shakes up namely to get to mix reference substance solution (III).Precision is drawn reference substance solution (I) 50 μ l, 10 μ l, 5 μ l respectively, and reference substance solution (II) 10 μ l and reference substance solution (III) 20 μ l measure with the inventive method chromatographic condition, the results are shown in Table 1.Take reference substance sample size X (μ g) as horizontal ordinate, peak area integrated value (mAU) is ordinate, and the drawing standard curve the results are shown in Figure 4, the ginsenoside Rg
1Regression equation Y=293364X+1806.2, correlation coefficient r=0.9999 shows the ginsenoside Rg
1In 0.04304 μ g～4.304 μ g scopes, be good linear relationship.Ginsenoside Rb
1Regression equation Y=240654X+1798.8, correlation coefficient r=1 shows the ginsenoside Rg
1In 0.03888 μ g～3.888 μ g scopes, be good linear relationship.
Table 1 ginsenoside Rg
1, Rb
1The linear relationship investigation table
4.3 replica test
Get with 6 parts of a collection of product (lot number 081009), measure by the inventive method content assaying method.The results are shown in Table 2, the ginsenoside Rg
1And Rb
1The RSD of total amount is 1.842%, shows that the repeatability of the method is good.
Table 2 reproducible test results
4.4 stability test
Get the need testing solution of lot number 081009, at rear 0 hour, 4 hours, 10 hours, 19 hours, 28 hours sample introductions of preparation, analyze by above-mentioned chromatographic condition, as a result table 3 respectively.The result is with the ginsenoside Rg
1Peak area meter RSD is 0.856%, with ginsenoside Rb
1Peak area meter RSD is 1.880%, shows that sample places in 28 hours stable.
Table 3 ginsenoside Rg
1, Rb
1The stability test result
4.5 recovery test
Same sample is got 5 parts (sample volume reduces by half), adds reference substance in 1: 1 ratio.The results are shown in Table 4.The result presentation method accuracy is good.
Table 4 Ginsenosides Rg1 and Rb1 recovery test measurement result
Table 5 compound Pien Tze Huang external preparation assay result
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment
Embodiment 1: the detection of Pien Tze Huang external preparation
Pien Tze Huang powder 250Kg, antivenom tablet 450Kg; Get the bulk drug of above-mentioned weight, technique adds conventional auxiliary material and is prepared into paste routinely.
Differentiate: get Pien Tze Huang external preparation 5g, put in the tool plug conical flask, add absolute ethyl alcohol 10ml, jolting makes and leaches, and ultrasonic processing was put in the ice bath and cooled off 30 minutes after 30 minutes, took out, and filtered rapidly, got filtrate 4ml, and water-bath is concentrated into 2ml, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (20: 25: 2: 3) as developping agent, expansion was taken out take normal hexane-ethyl acetate-acetic acid-methyl alcohol, dry, spray is with 10% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
Assay: ginsenoside Rg1, ginsenoside Rb1 measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, the regulation in the according to the form below is carried out gradient elution; 20 ℃ of column temperatures; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000.
Ginsenoside Rg1's reference substance is got in the preparation of reference substance solution and ginsenoside Rb1's reference substance is an amount of, and is accurately weighed, makes the mixed solution that every 1ml contains ginsenoside Rg1 0.1mg, ginsenoside Rb1 0.1mg with methyl alcohol, and get final product; The about 6g of Pien Tze Huang external preparation is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 30ml, ultrasonic processing (power 250W, frequency 33kHz) 30 minutes, jolting made and is uniformly dispersed, and added hot reflux 1 hour, take out, put in the ice bath and cooled off 20 minutes, filter rapidly in the 50ml measuring bottle, with methanol wash for several times, be placed to room temperature, with methyl alcohol to scale, shake up, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains ginsenoside Rg1 (C42H72O14) and ginsenoside Rb1's (C21H28N2O22HCl) total amount meter, must not be less than 0.70mg.
Embodiment 2: the detection of Pien Tze Huang external preparation
Pien Tze Huang powder 330Kg, antivenom tablet 350Kg; Get the bulk drug of above-mentioned weight, technique adds conventional auxiliary material and is prepared into liniment routinely.
Assay: ginsenoside Rg1, ginsenoside Rb1 measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, the regulation in the according to the form below is carried out gradient elution; 20 ℃ of column temperatures; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000.
Ginsenoside Rg1's reference substance is got in the preparation of reference substance solution and ginsenoside Rb1's reference substance is an amount of, and is accurately weighed, makes the mixed solution that every 1ml contains ginsenoside Rg1 0.1mg, ginsenoside Rb1 0.1mg with methyl alcohol, and get final product; The about 6g of Pien Tze Huang external preparation is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 30ml, ultrasonic processing (power 250W, frequency 33kHz) 30 minutes, jolting made and is uniformly dispersed, and added hot reflux 1 hour, take out, put in the ice bath and cooled off 20 minutes, filter rapidly in the 50ml measuring bottle, with methanol wash for several times, be placed to room temperature, with methyl alcohol to scale, shake up, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains ginsenoside Rg1 (C42H72O14) and ginsenoside Rb1's (C21H28N2O22HCl) total amount meter, must not be less than 0.70mg.
Embodiment 3: the detection of Pien Tze Huang external preparation
Pien Tze Huang powder 400Kg, antivenom tablet 250Kg; Get the bulk drug of above-mentioned weight, technique adds conventional auxiliary material and is prepared into film routinely.
Differentiate: get Pien Tze Huang external preparation 5g, put in the tool plug conical flask, add absolute ethyl alcohol 10ml, jolting makes and leaches, and ultrasonic processing was put in the ice bath and cooled off 30 minutes after 30 minutes, took out, and filtered rapidly, got filtrate 4ml, and water-bath is concentrated into 2ml, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (8: 4: 2: 1) as developping agent, expansion was taken out take isooctane-butyl acetate-glacial acetic acid-formic acid, dry, spray is with 30% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color respectively.
Embodiment 4: the detection of Pien Tze Huang external preparation
Pien Tze Huang powder 330Kg antivenom tablet 350Kg
Get antidote for snakebite by inventory, extracted 2 hours, it is for subsequent use to get supernatant.Take by weighing the Pien Tze Huang powder by inventory, dissolving, for subsequent use.Take by weighing glycerine 900Kg, triethanolamine 80Kg by inventory, drop into the water material-compound tank, add the supernatant of the filtrate of antidote for snakebite extraction, be heated to boiling, add while stirring above-mentioned Pien Tze Huang powder liquid, again be heated to boiling, be mixed into water, for subsequent use.Take by weighing albolene 1000Kg, stearic acid 300Kg, light liquid petrolatum 600Kg by inventory, drop into the oil phase material-compound tank, be heated to whole fusings, stir evenly, for subsequent use.Cooling after oil phase and the water emulsification evenly, discharging.Lotion is poured can in the bottle placer into, every 10g, and get final product.External application is applied to the affected part, 2-3 time on the one.
Differentiate: get Pien Tze Huang external preparation 5g, put in the tool plug conical flask, add absolute ethyl alcohol 10ml, jolting makes and leaches, and ultrasonic processing was put in the ice bath and cooled off 30 minutes after 30 minutes, took out, and filtered rapidly, got filtrate 4ml, and water-bath is concentrated into 2ml, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (20: 25: 2: 3) as developping agent, expansion was taken out take normal hexane-ethyl acetate-acetic acid-methyl alcohol, dry, spray is with 10% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
Assay: ginsenoside Rg1, ginsenoside Rb1 measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, the regulation in the according to the form below is carried out gradient elution; 20 ℃ of column temperatures; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000.
Ginsenoside Rg1's reference substance is got in the preparation of reference substance solution and ginsenoside Rb1's reference substance is an amount of, and is accurately weighed, makes the mixed solution that every 1ml contains ginsenoside Rg1 0.1mg, ginsenoside Rb1 0.1mg with methyl alcohol, and get final product; The about 6g of Pien Tze Huang external preparation is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 30ml, ultrasonic processing (power 250W, frequency 33kHz) 30 minutes, jolting made and is uniformly dispersed, and added hot reflux 1 hour, take out, put in the ice bath and cooled off 20 minutes, filter rapidly in the 50ml measuring bottle, with methanol wash for several times, be placed to room temperature, with methyl alcohol to scale, shake up, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains ginsenoside Rg1 (C42H72O14) and ginsenoside Rb1's (C21H28N2O22HCl) total amount meter, must not be less than 0.70mg.
Claims (1)
1. the quality determining method of a Pien Tze Huang external preparation is characterized in that the method comprises one or more in following discriminating and the assay:
Differentiate: get Pien Tze Huang external preparation 3-8g, put in the tool plug conical flask, add absolute ethyl alcohol 5-15m1, jolting makes and leaches, ultrasonic processing was put in the ice bath and is cooled off after 25-35 minute, took out, and filtered rapidly, get filtrate 3-6m1, water-bath is concentrated into 1-2m1, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every lml contains lmg, in contrast product solution; Test according to thin-layered chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take normal hexane-ethyl acetate of 18-22:22-27:1-3:2-4-acetic acid-methyl alcohol as developping agent, launch, take out, dry, spray is with 10% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, and 365nm puts under the ultraviolet lamp and inspects; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
Assay: ginsenoside Rg1, ginsenoside Rb1 are according to high effective liquid chromatography for measuring; Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, carry out gradient elution, from 0 to 75 minute acetonitrile-0.2% phosphatase 11 5:85 → 35:65, from 75 to 95 minutes acetonitrile-0.2% phosphoric acid 35:65 → 70:30; 20 ℃ of column temperatures; The detection wavelength is 203nm; Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000;
Ginsenoside Rg1's reference substance is got in the preparation of reference substance solution and ginsenoside Rb1's reference substance is an amount of, and is accurately weighed, makes the mixed solution that every lml contains ginsenoside Rg l 0.lmg, ginsenoside Rb1 0. 1mg with methyl alcohol, and get final product; Pien Tze Huang external preparation 4-8g is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 20-40ml, ultrasonic processing 20-40 minute, jolting makes and is uniformly dispersed, and adds hot reflux 0.5-1 hour, takes out, put in the ice bath and cool off, filter rapidly in the 50ml measuring bottle, with methanol wash for several times, be placed to room temperature,, shake up to scale with methyl alcohol, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains the total amount meter of ginsenoside Rg1 (C42H72O14) and ginsenoside Rbl (C21H28N2O22HCl), must not be less than 0.70mg;
The ointment that the Pien Tze Huang external preparation is comprised of the bulk drug of following weight portion:
Pien Tze Huang powder 220-450 weight portion, antivenom tablet 200-500 weight portion;
Described Pien Tze Huang ointment is made by the following method:
Take by weighing by weight proportion the Pien Tze Huang powder, antivenom tablet; The Pien Tze Huang powder, dissolving, for subsequent use; Antivenom tablet extracted 1-3 hour, and it is for subsequent use to get supernatant; Take by weighing glycerine 750-1100 weight portion, triethanolamine 60-100 weight portion, drop into the water material-compound tank, add the supernatant that antidote for snakebite extracts, be heated to boiling, add while stirring above-mentioned Pien Tze Huang powder liquid, again be heated to boiling, mixing
Become water, for subsequent use; Take by weighing albolene 850-1200 weight portion, stearic acid 200-420 weight portion, light liquid petrolatum 500-750 weight portion, drop into the oil phase material-compound tank, be heated to whole fusings, stir evenly, for subsequent use; Cooling after oil phase and the water emulsification evenly, discharging; Can namely gets paste.
2.The quality determining method of Pien Tze Huang external preparation as claimed in claim 1 is characterized in that the method comprises one or more in following discriminating and the assay:
Differentiate: get Pien Tze Huang external preparation 5g, put in the tool plug conical flask, add absolute ethyl alcohol l0ml, jolting makes and leaches, and ultrasonic processing was put in the ice bath and cooled off 30 minutes after 30 minutes, took out, and filtered rapidly, got filtrate 4ml, and water-bath is concentrated into 2ml, as need testing solution; Other gets cholic acid, deoxycholic aicd reference substance, adds absolute ethyl alcohol and makes the mixed solution that every lml contains lmg, in contrast product solution; Test according to thin-layered chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take normal hexane-ethyl acetate of 20:25:2:3-acetic acid-methyl alcohol as developping agent, launch, take out, dry, spray is with 10% sulfuric acid ethanol, and it is clear to be heated to the spot colour developing at 105 ℃, and 365nm puts under the ultraviolet lamp and inspects; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
Assay: ginsenoside Rg1, ginsenoside Rb1 are according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Take acetonitrile as mobile phase A, take 0.2% phosphoric acid solution as Mobile phase B, carry out gradient elution, from 0 to 75 minute acetonitrile-0.2% phosphatase 11 5:85 → 35:65, from 75 to 95 minutes acetonitrile-0.2% phosphoric acid 35:65 → 70:30; 20 ℃ of column temperatures; The detection wavelength is 203nm; Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 6000;
Ginsenoside Rg1's reference substance is got in the preparation of reference substance solution and ginsenoside Rb1's reference substance is an amount of, and is accurately weighed, makes the mixed solution that every lml contains ginsenoside Rg1 0.lmg, ginsenoside Rb1 0. lmg with methyl alcohol, and get final product; The about 6g of Pien Tze Huang external preparation is got in the preparation of need testing solution, and is accurately weighed, put in the tool plug conical flask, add methyl alcohol 30ml, at power 250W, ultrasonic processing is 30 minutes under the frequency 33kHz condition, and jolting makes and is uniformly dispersed, and adds hot reflux 1 hour, take out, put in the ice bath and cooled off 20 minutes, filter rapidly in the 50m1 measuring bottle, with methanol wash for several times, be placed to room temperature, with methyl alcohol to scale, shake up, and get final product; Determination method, precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product; The every gram of Pien Tze Huang external preparation contains ginsenoside Rg1 (C42H72O14) and ginsenoside Rb1's (C21H28N2O22HCl) total amount meter, must not be less than 0.70mg.
3.The quality determining method of Pien Tze Huang external preparation as claimed in claim 1 or 2 is characterized in that the method Raw medicine consists of:
Pien Tze Huang powder 250 weight portions, antivenom tablet 450 weight portions.
4.The quality determining method of Pien Tze Huang external preparation as claimed in claim 1 or 2 is characterized in that the method Raw medicine consists of:
Pien Tze Huang powder 330 weight portions, antivenom tablet 350 weight portions.
5.The quality determining method of Pien Tze Huang external preparation as claimed in claim 1 or 2 is characterized in that the method Raw medicine consists of:
Pien Tze Huang powder 400 weight portions, antivenom tablet 250 weight portions.
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Address after: 18/F, Pianzihuang Building, No. 1 Amber Road, Xiangcheng District, Zhangzhou City, Fujian Province, 363000 Patentee after: Fujian pianzehuang Health Technology Co.,Ltd. Patentee after: ZHANGZHOU PIEN TZE HUANG PHARMACEUTICAL Co.,Ltd. Address before: 18/F, Pianzihuang Building, No. 1 Amber Road, Xiangcheng District, Zhangzhou City, Fujian Province, 363000 Patentee before: Fujian Pianzihuang Health Industry Co.,Ltd. Patentee before: ZHANGZHOU PIEN TZE HUANG PHARMACEUTICAL Co.,Ltd. |
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Effective date of registration: 20230412 Address after: 18/F, Pianzihuang Building, No. 1 Amber Road, Xiangcheng District, Zhangzhou City, Fujian Province, 363000 Patentee after: Fujian Pianzihuang Health Industry Co.,Ltd. Patentee after: ZHANGZHOU PIEN TZE HUANG PHARMACEUTICAL Co.,Ltd. Address before: 363000 Jingcheng New District, Nanjing County, Zhangzhou City, Fujian Province Patentee before: Fujian pianzehuang Health Technology Co.,Ltd. Patentee before: ZHANGZHOU PIEN TZE HUANG PHARMACEUTICAL Co.,Ltd. |
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