CN101893608A - Method for detecting chemical compositions in dendranthema lavandulifolium essential oil - Google Patents
Method for detecting chemical compositions in dendranthema lavandulifolium essential oil Download PDFInfo
- Publication number
- CN101893608A CN101893608A CN2009100621985A CN200910062198A CN101893608A CN 101893608 A CN101893608 A CN 101893608A CN 2009100621985 A CN2009100621985 A CN 2009100621985A CN 200910062198 A CN200910062198 A CN 200910062198A CN 101893608 A CN101893608 A CN 101893608A
- Authority
- CN
- China
- Prior art keywords
- solution
- volatile oil
- ether
- dendranthema indicum
- dendranthema
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000341 volatile oil Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000126 substance Substances 0.000 title claims abstract description 34
- 239000000203 mixture Substances 0.000 title claims abstract description 10
- 235000018951 Chrysanthemum lavandulifolium Nutrition 0.000 title abstract 3
- 241001312631 Chrysanthemum lavandulifolium Species 0.000 title abstract 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 80
- 238000012360 testing method Methods 0.000 claims abstract description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 23
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 20
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 10
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 10
- 240000005250 Chrysanthemum indicum Species 0.000 claims description 45
- 235000018959 Chrysanthemum indicum Nutrition 0.000 claims description 44
- 239000000284 extract Substances 0.000 claims description 25
- 238000000605 extraction Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- 238000001819 mass spectrum Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 235000012054 meals Nutrition 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 52
- 239000007789 gas Substances 0.000 description 13
- 238000001514 detection method Methods 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 235000008495 Chrysanthemum leucanthemum Nutrition 0.000 description 4
- 244000192528 Chrysanthemum parthenium Species 0.000 description 4
- 235000000604 Chrysanthemum parthenium Nutrition 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 235000008384 feverfew Nutrition 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000723353 Chrysanthemum Species 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000000622 liquid--liquid extraction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 208000004429 Bacillary Dysentery Diseases 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000004232 Enteritis Diseases 0.000 description 1
- 241000201295 Euphrasia Species 0.000 description 1
- 206010017915 Gastroenteritis shigella Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 230000001741 anti-phlogistic effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 201000005113 shigellosis Diseases 0.000 description 1
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a method for detecting chemical compositions in dendranthema lavandulifolium essential oil, belonging to the analytical chemistry field. In the method, the dendranthema lavandulifolium essential oil to be detected is processed as follows: (1) adding ethyl ether to performance dissolution, completely extracting by hydrochloric acid with the concentration of 1%, and then completely extracting by ethyl ether to obtain the solution of a test article I; (2) completely extracting the residual solution extracted by the hydrochloric acid with the concentration of 1% by sodium bicarbonate solution with the concentration of 5%, and then completely extracting by ethyl ether to obtain the solution of a test article II; (3) completely extracting the residual solution extracted by the sodium bicarbonate solution with the concentration of 5%, then completely extracting by sodium hydroxide with the concentration of 1%, and finally completely extracting by ethyl ether to obtain the solution of a test article III; and (4) concentrating the residual solution extracted by the sodium hydroxide with the concentration of 1%, adding ethyl ether for constant volume, taking the solution after constant volume as the solution of a test article IV; respectively carrying out GC-MS analysis on the solutions of the test articles I, II, III and IV to determine chemical components contained therein. The method is accurate and reliable, and has good repeatability, wherein RSD is less than 10%.
Description
Technical field
The invention belongs to the analytical chemistry field, relate to a kind of method that detects chemical constitution in the Dendranthema indicum volatile oil.After being specifically related to a kind of liquid-liquid technique separation Dendranthema indicum volatile oil, utilize the method for chemical constitution in the qualitative evaluation Dendranthema indicum of the GC-MS(gas chromatography-mass spectrography) volatile oil.
Background technology
Dendranthema indicum Dendranthema indicum (L.) Des Monl.var aromaticum Q.H.Liuet S.F.Zhang. is the new variant of composite family Chrysanthemum (Dendranthema), be the Shennongjia endemic plant, originate in Hubei Province's Shennongjiawooded Area, be distributed in the field on the open hillside that faces south of height above sea level more than 1200 meters, roadside, rock seam, shrubbery limit, complete stool has special strong fragrance, among the people with its flower, leaf dries in the shade and makes sachet.The west place in Hubei mountain area with Dendranthema indicum be used for anti-curing cold, diseases such as headache, bacillary dysentery, enteritis, constipation, coronary heart disease and hypertension, Dendranthema indicum also has bactericidal antiphlogistic, flat liver make eye bright, the loose effect of wind step-down.It can be used to extract essential oil or medicinal extract, is used for aspects such as medicine, beverage, cigarette and cosmetics.But at present less about the chemical substance fundamental research of Dendranthema indicum, and the chemical constitution that the Dendranthema indicum volatile oil of conventional steam distillation extraction utilizes GC-MS(gas chromatography-mass spectrography) mensuration to identify not is a lot.He Jun etc. identify 50 compounds with capillary gas chromatograph and chromatogram/mass spectrum/computing machine coupling analyser from Dendranthema indicum dried flower essential oil.Xu Pengxiang etc. adopt GC/MS to analyze the chemical composition of Hubei Dendranthema indicum essential oil, detect 54 kinds of components from essential oil altogether.Lu Jin waits clearly and adopts steam distillation to extract volatile oil from Dendranthema indicum, adopts gas chromatography-mass spectrography that chemical composition of volatile oil is carried out Analysis and Identification and identifies 44 chemical constitutions altogether.So, need set up a kind of sample pretreating method preferably in order to go out chemical constitution in the Dendranthema indicum volatile oil than complete detection.
Summary of the invention
At the above-mentioned deficiency of prior art, method of the present invention has been set up a kind of sample pretreating method preferably, has detected 87 kinds of chemical substances from Dendranthema indicum volatile oil, and this method is accurate, reliable, favorable reproducibility.
Technical scheme of the present invention is to detect the method for chemical constitution in the Dendranthema indicum volatile oil, makes meal after the Dendranthema indicum fresh flower is dried in the shade, and presses Chinese Pharmacopoeia (2005 editions) appendix XD determination of volatile oil method and extracts volatile oil; Dendranthema indicum volatile oil to be measured is carried out following processing successively:
(1) ether is added in the Dendranthema indicum volatile oil its dissolving, in the dislocation separating funnel, with the repeatedly shaking out of 1% hydrochloric acid solution, until fully, merging acid extraction liquid and regulating pH value is 7-8, again with repeatedly shaking out of ether, until fully, merge ether extraction liquid and be concentrated to 1-15ml, as test sample I solution;
(2) with above-mentioned 1% hydrochloric acid solution extracted residual Dendranthema indicum volatile oil solution, with the repeatedly shaking out of 5% sodium bicarbonate solution, until fully, merge the alkali extract and regulate the pH value and be 6-7, again with repeatedly shaking out of ether, until fully, merge ether extraction liquid and be concentrated to 1-15ml, as test sample II solution;
(3) with above-mentioned 5% sodium bicarbonate solution extracted residual Dendranthema indicum volatile oil solution, with the repeatedly shaking out of 1% sodium hydroxide solution, until fully, merging the alkali extract and regulating pH is 6-7, again with repeatedly shaking out of ether, until fully, merge ether extraction liquid and be concentrated to 1-15ml, as test sample III solution;
(4) with the remaining Dendranthema indicum volatile oil solution after the above-mentioned 1% sodium hydroxide solution extraction, concentrate, the constant volume that adds diethyl ether is to 1-15ml, as test sample IV solution;
Above-mentioned test sample I, II, III, IV solution are carried out GC-MS respectively analyze,, resolve definite chemical composition that wherein contains in conjunction with relevant mass spectrogram document simultaneously by HP MSD chem workstation retrieval NIST standard mass spectrum picture library.
Method of the present invention is accurate, reliable, favorable reproducibility, and RSD is less than 10%.The method that the liquid-liquid extraction isolation technics is applied to detection feverfew chemical constitution in the GC-MS(gas chromatography-mass spectrography) still belongs to initiative.This method helps more fully to study chemical constitution in the Dendranthema indicum volatile oil.
Description of drawings
Fig. 1 is the GC-MS chromatogram that test sample I soln using liquid-liquid technique separation-GC-MS(gas chromatography-mass spectrography) is measured.
Fig. 2 is the GC-MS chromatogram that test sample II soln using liquid-liquid technique separation-GC-MS(gas chromatography-mass spectrography) is measured.
Fig. 3 is the GC-MS chromatogram that test sample III soln using liquid-liquid technique separation-GC-MS(gas chromatography-mass spectrography) is measured.
Fig. 4 is the GC-MS chromatogram that test sample IV soln using liquid-liquid technique separation-GC-MS(gas chromatography-mass spectrography) is measured.
Embodiment
Below relevant technologies problem of the present invention is described in further detail.In order to go out chemical constitution in the Dendranthema indicum volatile oil than complete detection, need set up a kind of sample pretreating method preferably.Method of the present invention is utilized chemical constitution in the qualitative evaluation Dendranthema indicum of the GC-MS(gas chromatography-mass spectrography) volatile oil after separating Dendranthema indicum volatile oil with liquid-liquid technique, and chemical constitution in the qualitative evaluation Dendranthema indicum volatile oil detects 87 kinds of chemical constitutions altogether.Maximum than the detected chemical composition of other detection methods, and at present not about adopting liquid-liquid technique pre-separation feverfew sample especially to separate the bibliographical information that Dendranthema indicum volatile oil adopts its this method of chemical constitution of the qualitative evaluation of GC-MS(gas chromatography-mass spectrography) afterwards again.The method that the liquid-liquid extraction isolation technics is applied to detection feverfew chemical constitution in the GC-MS(gas chromatography-mass spectrography) still belongs to initiative.This method helps more fully to study chemical constitution in the Dendranthema indicum volatile oil, and method is accurate, reliable, favorable reproducibility, and RSD is less than 10%.This method can be used for the qualitative determination of chemical constitution in the Dendranthema indicum volatile oil, also can be used for the qualitative determination of other material volatile oil chemical constitution.
The method of chemical constitution has been determined wherein 87 chemical compositions (seeing Table 1) altogether in the qualitative evaluation Dendranthema indicum of the present invention volatile oil, maximum than the detected chemical composition of other detection methods, and do not utilize afterwards this bibliographical information of its chemical constitution of the qualitative evaluation of GC-MS(gas chromatography-mass spectrography) more at present with method about adopting liquid-liquid technique pre-separation feverfew sample especially to separate Dendranthema indicum volatile oil.
Table 1 Dendranthema indicum chemical composition of volatile oil
The extraction of Dendranthema indicum volatile oil takes by weighing meal 200g after the Dendranthema indicum fresh flower is dried in the shade, and adds the water of 12 times of amounts, presses Chinese Pharmacopoeia (2005 editions) appendix XD determination of volatile oil method and extracts volatile oil, extracts 12h continuously, collects volatile oil.
Dendranthema indicum volatile oil 1.10g is got in the preparation of need testing solution, the 10mL that adds diethyl ether dissolving is in the dislocation separating funnel, with 1% hydrochloric acid solution gradation shaking out, each 10mL, extract 3 times, merge acid liquid and add strong ammonia solution and regulate pH value to 8, with ether gradation shaking out, each 10mL, extract 3 times, merge ether solution and be concentrated into 10mL, as test sample I solution.Above-mentioned 1% hydrochloric acid solution extraction back surplus solution, with 5% sodium bicarbonate solution gradation shaking out, each 10mL, extract 3 times, merge alkaline solution and add 1% hydrochloric acid solution and regulate pH value to 6, with ether gradation shaking out, each 10mL, extract 3 times, merge ether solution and be concentrated into 10mL, as test sample II solution.Above-mentioned 5% sodium bicarbonate solution extraction back surplus solution, extract with 1% sodium hydroxide solution gradation, each 10mL, extract 3 times, merge alkaline solution and add 1% hydrochloric acid solution test solution and regulate pH value to 6, with ether gradation shaking out, each 10mL, extract 3 times, combined ether layer also is concentrated into 10mL, as test sample III solution.Surplus solution after the above-mentioned 1% sodium hydroxide solution extraction concentrates, and adding diethyl ether is settled to 10mL, as test sample IV solution.
GC-MS analyzes and gets need testing solution 3 μ L respectively, carries out GC-MS and analyzes, and analysis condition is: chromatographic column: DB-WAX (30m * 0.32mm * 0.25 μ m) quartz capillary column; Temperature programme: 60 ℃, kept 3 minutes, be warming up to 120 ℃ with 3 ℃/minute earlier, be warming up to 140 ℃ with 1 ℃/minute again, keep 3min, be warming up to 240 ℃ with 8 ℃/minute at last, kept 5 minutes; 250 ℃ of injector temperatures; Carrier gas: 99.999% helium; Flow rate of carrier gas: 1.2mL/min; Split ratio 30: 1; Solvent time-delay 3min.Mass spectrum condition: ion gun: EI source; Ion source temperature: 230 ℃; Level Four bar temperature: 150 ℃; Electron energy: 70eV; Multiplier tube voltage: 1.2KV; Interface temperature: 250 ℃; Mass scanning scope 30-450amu by HP MSD chem workstation retrieval NIST standard mass spectrum picture library, resolves in conjunction with relevant mass spectrogram document simultaneously.
Embodiment 2
The extraction of Dendranthema indicum volatile oil takes by weighing meal 200g after the Dendranthema indicum fresh flower is dried in the shade, and adds the water of 12 times of amounts, presses Chinese Pharmacopoeia (2005 editions) appendix XD determination of volatile oil method and extracts volatile oil, extracts 12h continuously, collects volatile oil.
Dendranthema indicum volatile oil 1.60g is got in the preparation of need testing solution, the 15mL that adds diethyl ether dissolving is in the dislocation separating funnel, with 1% hydrochloric acid solution gradation shaking out, each 15mL, extract 4 times, merge acid liquid and add strong ammonia solution and regulate pH value to 8, with ether gradation shaking out, each 15mL, extract 4 times, merge ether solution and be concentrated into 15mL, as test sample I solution.Above-mentioned 1% hydrochloric acid solution extraction back surplus solution, with 5% sodium bicarbonate solution gradation shaking out, each 15mL, extract 4 times, merge alkaline solution and add 1% hydrochloric acid solution and regulate pH value to 6, with ether gradation shaking out, each 15mL, extract 4 times, merge ether solution and be concentrated into 15mL, as test sample II solution.Above-mentioned 5% sodium bicarbonate solution extraction back surplus solution, extract with 1% sodium hydroxide solution gradation, each 15mL, extract 4 times, merge alkaline solution and add 1% hydrochloric acid solution test solution and regulate pH value to 6, with ether gradation shaking out, each 15mL, extract 3 times, combined ether layer also is concentrated into 15mL, as test sample III solution.Surplus solution after the above-mentioned 1% sodium hydroxide solution extraction concentrates, and adding diethyl ether is settled to 15mL, as test sample IV solution.
GC-MS analyzes and gets need testing solution 3 μ L respectively, carries out GC-MS and analyzes, and analysis condition is: chromatographic column: DB-WAX (30m * 0.32mm * 0.25 μ m) quartz capillary column; Temperature programme: 60 ℃, kept 3 minutes, be warming up to 120 ℃ with 3 ℃/minute earlier, be warming up to 140 ℃ with 1 ℃/minute again, keep 3min, be warming up to 240 ℃ with 8 ℃/minute at last, kept 5 minutes; 250 ℃ of injector temperatures; Carrier gas: 99.999% helium; Flow rate of carrier gas: 1.2mL/min; Split ratio 30: 1; Solvent time-delay 3min.Mass spectrum condition: ion gun: EI source; Ion source temperature: 230 ℃; Level Four bar temperature: 150 ℃; Electron energy: 70eV; Multiplier tube voltage: 1.2KV; Interface temperature: 250 ℃; Mass scanning scope 30-450amu by HP MSD chem workstation retrieval NIST standard mass spectrum picture library, resolves in conjunction with relevant mass spectrogram document simultaneously.
Claims (1)
1. a method that detects chemical constitution in the Dendranthema indicum volatile oil is characterized in that: make meal after the Dendranthema indicum fresh flower is dried in the shade, press Chinese Pharmacopoeia (2005 editions) appendix XD determination of volatile oil method and extract volatile oil; Dendranthema indicum volatile oil to be measured is carried out following processing successively:
(1) ether is added in the Dendranthema indicum volatile oil its dissolving, in the dislocation separating funnel, with the repeatedly shaking out of 1% hydrochloric acid solution, until fully, merging acid extraction liquid and regulating pH value is 7-8, again with repeatedly shaking out of ether, until fully, merge ether extraction liquid and be concentrated to 1-15ml, as test sample I solution;
(2) with above-mentioned 1% hydrochloric acid solution extracted residual Dendranthema indicum volatile oil solution, with the repeatedly shaking out of 5% sodium bicarbonate solution, until fully, merge the alkali extract and regulate the pH value and be 6-7, again with repeatedly shaking out of ether, until fully, merge ether extraction liquid and be concentrated to 1-15ml, as test sample II solution;
(3) with above-mentioned 5% sodium bicarbonate solution extracted residual Dendranthema indicum volatile oil solution, with the repeatedly shaking out of 1% sodium hydroxide solution, until fully, merging the alkali extract and regulating pH is 6-7, again with repeatedly shaking out of ether, until fully, merge ether extraction liquid and be concentrated to 1-15ml, as test sample III solution;
(4) with the remaining Dendranthema indicum volatile oil solution after the above-mentioned 1% sodium hydroxide solution extraction, concentrate, the constant volume that adds diethyl ether is to 1-15ml, as test sample IV solution;
Above-mentioned test sample I, II, III, IV solution are carried out GC-MS respectively analyze,, resolve definite chemical composition that wherein contains in conjunction with relevant mass spectrogram document simultaneously by HP MSD chem workstation retrieval NIST standard mass spectrum picture library.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910062198A CN101893608B (en) | 2009-05-22 | 2009-05-22 | Method for detecting chemical compositions in dendranthema lavandulifolium essential oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910062198A CN101893608B (en) | 2009-05-22 | 2009-05-22 | Method for detecting chemical compositions in dendranthema lavandulifolium essential oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101893608A true CN101893608A (en) | 2010-11-24 |
| CN101893608B CN101893608B (en) | 2012-10-24 |
Family
ID=43102867
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910062198A Expired - Fee Related CN101893608B (en) | 2009-05-22 | 2009-05-22 | Method for detecting chemical compositions in dendranthema lavandulifolium essential oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101893608B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103892637A (en) * | 2012-12-25 | 2014-07-02 | 神农架林晖绿色开发有限责任公司 | Healthcare drug pillow |
-
2009
- 2009-05-22 CN CN200910062198A patent/CN101893608B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103892637A (en) * | 2012-12-25 | 2014-07-02 | 神农架林晖绿色开发有限责任公司 | Healthcare drug pillow |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101893608B (en) | 2012-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104502518B (en) | A kind of detection method for the treatment of the Chinese medicine preparation of baby anorexia | |
| Kaya et al. | HPLC-DAD analysis of lycorine in Amaryllidaceae species | |
| CN108693262B (en) | Method for determining various preservatives in cosmetics | |
| CN101028388B (en) | Quality inspection of Chinese-medicinal preparation for treating shortsighness and asthenopia | |
| CN104922196A (en) | General ohwia flavone extract preparation method and general ohwia flavone extract quality detecting method | |
| CN106353417A (en) | UPLC (ultra-performance liquid chromatography) detection method of multiple steroid saponins in Yunnan rhizoma paridis or its polygerm strain | |
| CN104345110A (en) | Content determination method for seven compositions in traditional Chinese medicine composition preparation | |
| CN110346462A (en) | Leaf of Moringa UPLC fingerprint and its UPLC finger-print | |
| CN105445407A (en) | Detection method for fatty acid and vitamin E in idesia | |
| CN101718764B (en) | Detection method of residual polychlorinated biphenyl in cosmetics with gas chromatography-mass spectrum method | |
| CN103713058B (en) | The detection method of diester-type alkaloids in a kind of Huafeng pill medicine mother | |
| CN102552476B (en) | Quality control method for Rosa laevigata root | |
| CN101703610A (en) | Quality detection method of Qingnao antihypertensive tablet | |
| CN101893608A (en) | Method for detecting chemical compositions in dendranthema lavandulifolium essential oil | |
| CN101816753B (en) | Method for detecting quality of compound preparation for treating cold | |
| CN102048906B (en) | Content measurement method of abrus herb capsules | |
| CN101317935B (en) | Rujietai formulation and quality detection method | |
| CN107748211B (en) | Method for extracting and measuring 5 macamides in maca by using deep eutectic solvent | |
| CN103424499B (en) | Method for detecting picrasma quassioides alkali content in picrasma quassioides | |
| CN107037155B (en) | Simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of algae toxins method | |
| CN101871924B (en) | Method for synchronous detection of xanthohumol, isoxanthohumol and 8-isopentenylnaringenin in lupulus | |
| CN102028760A (en) | Quality detecting method for polygonum perfoliatum | |
| CN101953978B (en) | Heart-soothing and lipid-lowering tablet medicine quality detecting method | |
| Al-Tahami | Determination of sildenafil, vardenafil and tadalafil in dietary supplements sold in the Yemeni market | |
| CN100571755C (en) | A kind of detection method of common cold-fever-clearing preparation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121024 Termination date: 20160522 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |