CN1963496A - Method for setting up finger-print of pain-eliminate paste and standard finger-print thereof - Google Patents
Method for setting up finger-print of pain-eliminate paste and standard finger-print thereof Download PDFInfo
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- 208000002193 Pain Diseases 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000036407 pain Effects 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 27
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 17
- WEEGYLXZBRQIMU-UHFFFAOYSA-N 1,8-cineole Natural products C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 claims abstract description 16
- WEEGYLXZBRQIMU-WAAGHKOSSA-N Eucalyptol Chemical compound C1C[C@H]2CC[C@]1(C)OC2(C)C WEEGYLXZBRQIMU-WAAGHKOSSA-N 0.000 claims abstract description 16
- 229960005233 cineole Drugs 0.000 claims abstract description 16
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000014759 maintenance of location Effects 0.000 claims description 93
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 238000012360 testing method Methods 0.000 claims description 31
- 239000000284 extract Substances 0.000 claims description 24
- 239000006071 cream Substances 0.000 claims description 16
- 238000003908 quality control method Methods 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 14
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 238000003822 preparative gas chromatography Methods 0.000 claims description 4
- 230000000202 analgesic effect Effects 0.000 claims description 3
- 238000004817 gas chromatography Methods 0.000 claims description 3
- 238000000874 microwave-assisted extraction Methods 0.000 claims description 3
- 239000011505 plaster Substances 0.000 claims description 3
- 238000011003 system suitability test Methods 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 abstract description 6
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 abstract 1
- 230000008030 elimination Effects 0.000 abstract 1
- 238000003379 elimination reaction Methods 0.000 abstract 1
- 239000000839 emulsion Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 150000000193 1,8-cineol derivatives Chemical class 0.000 description 1
- 241001191006 Phlomoides rotata Species 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 239000003962 counterfeit drug Substances 0.000 description 1
- 229940109262 curcumin Drugs 0.000 description 1
- 235000012754 curcumin Nutrition 0.000 description 1
- 239000004148 curcumin Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
This invention discloses one pains elimination powder or emulsion or extraction GC and GC/MS finger spectrum establishing method and its standard finger spectrum, which comprises the following steps: a, preparing the sample solution to take for certain volume and fine weighting into sorbite extractor container and adding ether into flow for filtering as sample liquid; b, using gas phase spectrum method and gas phase spectrum to quantum cross usage to identify the 18 reference peak as characteristic peaks for identification results; c, according to eucalyptol characteristic reference peak to compute relative keep time and area to get the extraction standard finger spectrum.
Description
Technical field
The present invention relates to the method for building up of the finger-print of Chinese medicine, specifically the invention relates to method for building up and standard finger-print thereof that the pain that disappears is pasted the finger-print of powder or cream or extract.
Background technology
The pain that disappears is pasted the tibetan traditional medicine of producing for Tibet Linzhi's Qizheng Tibetan Medicine factory, is the secret kind of country, Chinese medicine protection kind.Adopt the distinctive natural drug of Chinese Tibet plateau, form through special cryogenic vacuum dewatering process is refining, major function is promoting blood circulation and removing blood stasis, swelling and pain relieving, being used for acute and chronic dampens, fall and beat stasis of blood pain, osteoproliferation, rheumatism and rheumatoid pain etc., because its remarkable effect enjoys a good market both at home and abroad, at present, the assay that has only curcumin in its quality control, the thin layer of lamiophlomis rotata is differentiated, check, list is lost comprehensively rather with regard to the quality of these two these products of control indexes, and make illegal retailer bore the sky of its quality control standard easily, make and sell the counterfeit drug of " conformance with standard ", foundation to finger-print of pain-eliminate paste does not now appear in the newspapers, in order to remedy above-mentioned deficiency, make its Quality Control Technology more perfect, science also provides a kind of utilizable quality control pattern to its standardized production from now on, and the product of 50 continuous 6 years different lot numbers has been carried out investigating relatively, sets up the assay method of the standard finger-print of this product volatile ingredient extract.
Summary of the invention
The objective of the invention is by offseting the research that pain is pasted the GC and the GC/MS finger-print of powder or cream or extract, find out a kind of pain that disappears and paste the method for quality control of powder or cream or extract, set up the method for the accurate finger-print of pain decals that disappears, remedy the deficiencies in the prior art, make it more perfect, science, more reasonable more.
The present invention is achieved by following technical proposals:
(1) preparation of need testing solution: cancellation pain emplastrum or powder or extract are an amount of, the accurate title, decide, add ether or chloroform, put in the apparatus,Soxhlet's, refluxing extraction 1～12 hour or ultrasonic Extraction 5～60 minutes or refluxing extraction 0.5～8 hour or microwave abstracting 0.1～4 hour, filter, the filtrate evaporate to dryness adds methanol constant volume as need testing solution.
(2) mensuration of finger-print: chromatographic condition and system suitability test are immobile liquid with SE-54 or OV-1701 or OV-11; Chromatographic column is a quartz capillary column, and column temperature is temperature programme, and initial column temperature is 100～170 ℃, after constant 1～15 minute with 1～30 ℃/minute rise to 170～230 ℃ constant 1～30 minute, carrier gas is high purity nitrogen, detecting device is a hydrogen flame detector; The accurate need testing solution 0.5 μ L～5 μ L that draw adopt and do not shunt or the split sampling mode; Use gas chromatograph for determination, the relative retention time and the relative peak area of No. 10 chromatographic peaks (characteristic peak of eucalyptol) are 1, calculate relative retention time and relative peak area, and the accurate finger-print I of pain decals promptly obtains disappearing.
(3) measuring identical chromatographic condition according to the preparation method of described need testing solution and GC carries out GC/MS and analyzes resulting total ion current figure and constitute the standard finger-print II that the pain that disappears is pasted.
This method is: sample thief is an amount of, the accurate title, decide, add ether or chloroform, put soaked overnight in the apparatus,Soxhlet's, refluxing extraction 1～12 hour or ultrasonic Extraction 5～60 minutes or refluxing extraction 0.5～8 hour or Microwave Extraction 0.1～4 hour are filtered, the filtrate evaporate to dryness, add methanol constant volume, miillpore filter (0.45um) filters, and pastes the need testing solution of powder or cream or extract as the pain that disappears; According to an appendix VIE of Chinese Pharmacopoeia version in 2005 vapor-phase chromatography test, be immobile liquid with SE-54 or OV-1701 or OV-11; Chromatographic column is a quartz capillary column, and column temperature is temperature programme, and initial column temperature is 100～170 ℃, after constant 1～15 minute with 1～30 ℃/minute rise to 170～230 ℃ constant 1～30 minute, carrier gas is high purity nitrogen, and detecting device is a hydrogen flame detector, adopts and does not shunt or the split sampling mode; The relative retention time and the relative peak area of No. 10 chromatographic peaks (characteristic peak of eucalyptol) are 1, calculate relative retention time and relative peak area, promptly obtain analgesic plaster extract standard finger-print.
This method is: cancellation pain emplastrum or powder or extract sample are an amount of, the accurate title, decide, add ether or chloroform, put soaked overnight in the apparatus,Soxhlet's, refluxing extraction 1～12 hour or ultrasonic Extraction 5～60 minutes or refluxing extraction 0.5～8 hour or Microwave Extraction 0.1～4 hour are filtered, the filtrate evaporate to dryness, add methanol constant volume, miillpore filter (0.45 μ m) filters, as the need testing solution of analgesic plaster powder extracts; According to the test of an appendix VIE of Chinese Pharmacopoeia version in 2005 vapor-phase chromatography, be immobile liquid with SE-54; Chromatographic column is a quartz capillary column, column temperature is temperature programme, draw need testing solution 0.5～2 μ L, inject gas chromatograph, the relative retention time and the relative peak area of No. 10 chromatographic peaks (characteristic peak of eucalyptol) are 1, calculate relative retention time and relative peak area, the pain accurate finger-print I of decals (Fig. 1) promptly obtains disappearing.
This method is: the pain that disappears is pasted powder or cream or extract need testing solution, and according to gas chromatography determination, chromatographic column is a quartz capillary column, adopts not shunt or be regardless of to flow to sample loading mode, and theoretical cam curve is calculated with No. 10 peaks, is not less than 40000.
This method is: chromatographic column is an immobile liquid with SE-54 or OV-1701 or OV-11; Chromatographic column is a quartz capillary column, and column parameter is φ 0.22mm * (20m～35m).
This method is: sample thief 1g, and accurate the title, decide, and adds ether, put in the apparatus,Soxhlet's, refluxing extraction 12 hours, the extract evaporate to dryness adds methanol constant volume as need testing solution.
This method is: the addition of need testing solution is 0.5 μ L.
This method is: carry out GC/MS and analyze and obtain No. 10 with reference to the structural information at peak and to identify be the characteristic peak of eucalyptol to measure identical chromatographic condition according to the preparation method of described need testing solution and GC; Obtain GC/MS total ion current figure simultaneously and constitute the pain accurate finger-print II of decals (Fig. 2) that disappears.
In the accurate finger-print of pain decals that disappears that this method obtains, the common characteristic fingerprint peaks has 18, and its peak area summation accounts for more than 90% of total peak area.
Relative retention time and relative peak area with the chromatographic peak (No. 10 peaks) of eucalyptol are 1, and the common characteristic peak is (Fig. 1 or Fig. 2) in the resulting accurate finger-print of pain decals that disappears:
No. 1 peak: relative retention time 2.08～3.86, relative peak area 2.06～685.73
No. 2 peaks: relative retention time 2.00～3.68, relative peak area 5.88～552.83
No. 3 peaks: relative retention time 1.00～2.00, relative peak area 54.04～604.21
No. 4 peaks: relative retention time 1.00～2.00, relative peak area 9.60～560.99;
No. 5 peaks: relative retention time 0.99～1.99, relative peak area 8.30～604.11;
No. 6 peaks: relative retention time 0.89～1.55, relative peak area 10.44～86.90;
No. 7 peaks: relative retention time 0.87～1.54, relative peak area 10.31～640.7;
No. 8 peaks: relative retention time 0.86～1.53, relative peak area 1.05～20.78
No. 9 peaks: relative retention time 0.85～1.51, relative peak area 5.72～218.28;
No. 10 peaks (with reference to the peak): relative retention time 1, relative peak area 1;
No. 11 peaks: relative retention time 0.81～1.50, relative peak area 3.90～384.76
No. 12 peaks: relative retention time 0.80～1.49, relative peak area 2.84～444.0
No. 13 peaks: relative retention time 0.78～1.47, relative peak area 6.98～311.99;
No. 14 peaks: relative retention time 0.76～1.45, relative peak area 5.89～80.98;
No. 15 peaks: relative retention time 0.64～1.43, relative peak area 0.64～20.99;
No. 16 peaks: relative retention time 0.53～1.40, relative peak area 8.98～560.04;
No. 17 peaks: relative retention time 0.52～1.38, relative peak area 14.77～523.15;
No. 18 peaks: relative retention time 0.48～1.20, relative peak area 22.32～600.34;
Preferably, be 1 with the relative retention time and the relative peak area of the chromatographic peak (No. 10 peaks) of eucalyptol, the common characteristic peak is in the resulting accurate finger-print of the pain decals peak that disappears:
No. 1 peak: relative retention time 3.78, relative peak area 3.06～585.73
No. 2 peaks: relative retention time 2.42, relative peak area 7.88～452.88
No. 3 peaks: relative retention time 1.61, relative peak area 14.04～504.20
No. 4 peaks: relative retention time 1.33, relative peak area 8.60～460.90;
No. 5 peaks: relative retention time 1.22, relative peak area 18.30～504.20;
No. 6 peaks: relative retention time 1.21, relative peak area 20.44～146.96;
No. 7 peaks: relative retention time 1.06, relative peak area 30.31～540.7;
No. 8 peaks: relative retention time 1.03, relative peak area 2.17～8.23;
No. 9 peaks: relative retention time 1.02, relative peak area 15.22～163.28;
No. 10 peaks (with reference to the peak): relative retention time 1, relative peak area 1;
No. 11 peaks: relative retention time 0.98, relative peak area 10.99～218.24;
No. 12 peaks: relative retention time 0.95, relative peak area 11.84～349.75;
No. 13 peaks: relative retention time 0.88, relative peak area 12.11;
No. 14 peaks: relative retention time 0.86, relative peak area 12.25～40.78;
No. 15 peaks: relative retention time 0.82, relative peak area 1.61～9.97;
No. 16 peaks: relative retention time 0.78, relative peak area 16.73～460.90;
No. 17 peaks: relative retention time 0.72, relative peak area 24.97～425.14;
No. 18 peaks: relative retention time 0.60, relative peak area 52.71～486.48;
The present invention has that method is easy, stable, precision is high, favorable reproducibility, the characteristics that are easy to grasp.
Description of drawings
Fig. 1 is the standard finger-print I that the present invention disappears and pastes bitterly.
Fig. 2 is the accurate finger-print II of pain decals that disappears that GC/MS total ion current figure of the present invention constitutes.
Below further specify the present invention by specific embodiment, but be not construed as limiting the invention.
Embodiment 1: the method for building up of QIZHENG XIAOTONG TIE powder standard finger-print I
1. instrument and reagent
1.1 instrument
Tianjin, island GC-17A gas chromatograph; Hydrogen flame detector; Tianjin, island Class-GC10 workstation
1.2 reagent
Ether is analyzed pure; Methyl alcohol, chromatographically pure; The syringe-type nuclepore membrane filter, organic system, diameter 13mm, 0.45um; It is that Tibet Linzhi's Qizheng Tibetan Medicine factory produces that the pain that disappears is pasted powder.
2. method and result
2.1 chromatographic condition
Chromatographic column: SE-54,0.22mm * 25m quartz capillary column; Carrier gas is high purity nitrogen; Detecting device is a hydrogen flame detector, and theoretical cam curve is calculated with the characteristic peak of No. 10 eucalyptols, must not be lower than 40000.Injector temperature is 250 ℃, and detector temperature is 280 ℃, temperature programme:
Adopt not split sampling; Sample size 0.5 μ L.
2.2 the mensuration of finger-print
Pain is pasted the preparation of powder finger-print 2.2.1 disappear
The preparation of need testing solution: the cancellation pain is pasted powder sample 1.0g, and the adding ether is an amount of, puts in the apparatus,Soxhlet's, and refluxing extraction 12 hours is settled to 5.00ml, gets 2.00ml, volatilizes, and adds methyl alcohol 0.50ml, filters, and filtrate is as need testing solution.
The accurate need testing solution 0.5ul that draws in the inject gas chromatograph, according to gas chromatography determination, writes down 80 minutes chromatogram, promptly.With eucalyptol (No. 10) chromatographic peak relative retention time and peak area is 1, calculates relative retention time and relative peak area, and the accurate finger-print I of pain decals promptly obtains disappearing.
2.2.2 determining of total peak
Paste the powder determining fingerprint pattern by 10 batches of pains that disappear, compare its chromatogram, determine 18 at total peak, be object of reference wherein with No. 10 fingerprint peakses (characteristic peak of eucalyptol), its peak area surpasses 10% of total peak area, enumerates that total peak relative retention time of 10 batch samples and relative peak area statistics see the following form 1, table 2.
The method for building up of embodiment 2 QIZHENG XIAOTONG TIE standard finger-print II
1. instrument and reagent
1.1 instrument
The TRACEMS gas chromatograph-mass spectrometer; The NIST02 mass spectral database.
1.2 reagent
Ether is analyzed pure; Methyl alcohol, chromatographically pure; The syringe-type nuclepore membrane filter, organic system, diameter 13mm, 0.45um; The pain that disappears is pasted the production for Tibet Linzhi's Qizheng Tibetan Medicine factory.
2. method and result
2.1 look-mass spectrometry condition
Chromatographic column is SE-54 (0.25 μ m, the fused-silica capillary column of 30m * 0.25mm), a sample size: 0.5 μ L; Injector temperature: 280 ℃; Temperature programme: injector temperature is 250 ℃, and detector temperature is 280 ℃, temperature programme:
Adopt split sampling; Sample size 0.5 μ L; Split ratio is 20: 1; Ionization mode: EI; Ion source temperature: 200 ℃; Electron energy: 70eV; Quality of scanning scope: 3～400amu; Transmitter current: 150mA; Electron multiplication voltage: 350V.
3. result
(1) GC/MS total ion current figure constitutes the obedient standard finger-print II (see figure 2) of pain that disappears.
(2) test sample carries out GC-MS and analyzes, machine examination rope N IST 02 spectrum library as calculated, and with standard diagram (EPA/N IH Mass Spectral Data Base) contrast, identify No. 10 total peaks (retention time is 21.96min) and be the characteristic peak of eucalyptol.
Table 1:10 criticizes the relative retention time statistics that the pain that disappears is pasted the total peak of powder
| Sample | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
| Total peak number | 1 | 3.78 | 3.85 | 3.86 | 3.81 | 3.74 | 3.79 | 3.77 | 3.81 | 3.78 | 3.84 |
| 2 | 2.42 | 2.44 | 2.44 | 2.43 | 2.41 | 2.43 | 2.40 | 2.44 | 2.43 | 2.43 | |
| 3 | 1.61 | 1.61 | 1.61 | 1.61 | 1.61 | 1.59 | 1.60 | 1.59 | 1.61 | 1.60 | |
| 4 | 1.33 | 1.34 | 1.34 | 1.34 | 1.33 | 1.33 | 1.33 | 1.34 | 1.33 | 1.34 | |
| 5 | 1.22 | 1.23 | 1.23 | 1.23 | 1.24 | 1.25 | 1.24 | 1.23 | 1.24 | 1.25 | |
| 6 | 1.21 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.20 | 1.19 | 1.20 | |
| 7 | 1.06 | 1.06 | 1.06 | 1.06 | 1.06 | 1.06 | 1.05 | 1.06 | 1.06 | 1.06 | |
| 8 | 1.03 | 1.03 | 1.04 | 1.03 | 1.03 | 1.03 | 1.03 | 1.03 | 1.03 | 1.03 | |
| 9 | 1.02 | 1.02 | 1.02 | 1.02 | 1.02 | 1.02 | 1.02 | 1.02 | 1.02 | 1.02 | |
| 10 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | |
| 11 | 0.98 | 0.98 | 0.98 | 0.98 | 0.98 | 0.98 | 0.98 | 0.98 | 0.98 | 0.98 | |
| 12 | 0.95 | 0.95 | 0.96 | 0.96 | 0.95 | 0.95 | 0.96 | 0.96 | 0.96 | 0.95 | |
| l3 | 0.88 | 0.87 | 0.88 | 0.87 | 0.87 | 0.87 | 0.88 | 0.87 | 0.88 | 0.88 | |
| 14 | 0.86 | 0.86 | 0.86 | 0.86 | 0.86 | 0.86 | 0.86 | 0.86 | 0.86 | 0.86 | |
| 15 | 0.82 | 0.82 | 0.82 | 0.82 | 0.82 | 0.82 | 0.82 | 0.82 | 0.82 | 0.82 | |
| 16 | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 | 0.78 | |
| 17 | 0.72 | 0.72 | 0.72 | 0.72 | 0.72 | 0.72 | 0.72 | 0.72 | 0.72 | 0.72 | |
| 18 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | |
Table 2:10 criticizes the peak area statistics that the pain that disappears is pasted the total peak of powder
| Sample | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | |
| Total peak number | 1 | 3.06 | 22.28 | 6.89 | 12.41 | 10.27 | 19.29 | 19.96 | 12.79 | 29.82 | 44.03 |
| 2 | 7.88 | 70.16 | 13.96 | 44.12 | 42.08 | 144.56 | 38.68 | 46.23 | 452.88 | 369.31 | |
| 3 | 14.04 | 62.96 | 23.86 | 37.10 | 14.68 | 22.13 | 20.44 | 12.57 | 202.54 | 99.57 | |
| 4 | 12.15 | 43.85 | 16.34 | 22.07 | 8.73 | 11.92 | 14.23 | 8.6 | 27.99 | 24.28 | |
| 5 | 63.51 | 368.68 | 178.03 | 119.43 | 70.88 | 144.56 | 118.05 | 191.44 | 109.16 | 60.69 | |
| 6 | 146.96 | 35.20 | 53.60 | 62.37 | 68.91 | 126.01 | 113.64 | 73.43 | 52.92 | 45.22 | |
| 7 | 33.26 | 162.56 | 35.36 | 80.11 | 30.31 | 36.47 | 44.47 | 30.80 | 162.99 | 116.20 | |
| 8 | 6.67 | 6.66 | 4.74 | 6.04 | 5.07 | 5.44 | 5.12 | 4.75 | 5.38 | 3.36 | |
| 9 | 163.28 | 43.31 | 20.80 | 47.31 | 22.94 | 31.12 | 22.28 | 24.66 | 31.44 | 29.84 | |
| 10 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | |
| 11 | 10.99 | 15.42 | 18.85 | 23.34 | 13.73 | 14.24 | 17.26 | 14.60 | 149.74 | 41.47 | |
| 12 | 26.13 | 18.17 | 24.61 | 18.02 | 15.42 | 18.38 | 14.18 | 19.35 | 16.75 | 22.03 | |
| 13 | 12.11 | 55.57 | 15.35 | 31.45 | 12.34 | 13.91 | 17.61 | 15.96 | 116.00 | 47.75 | |
| 14 | 12.25 | 17.11 | 11.76 | 19.81 | 8.12 | 8.16 | 22.29 | 29.23 | 40.78 | 16.93 | |
| 15 | 1.61 | 2.28 | 1.84 | 2.18 | 1.81 | 1.72 | 1.87 | 3.69 | 5.09 | 2.92 | |
| 16 | 23.16 | 88.33 | 30.68 | 86.48 | 16.73 | 23.67 | 19.97 | 27.22 | 103.66 | 460.90 | |
| 17 | 41.88 | 191.52 | 24.97 | 151.84 | 78.28 | 145.28 | 294.89 | 45.22 | 129.08 | 66.03 | |
| 18 | 163.28 | 368.68 | 238.20 | 151.84 | 331.72 | 145.28 | 298.89 | 239.69 | 56.94 | 68.41 | |
Claims (10)
1, a kind of pain that disappears is pasted the method for quality control of powder or cream or extract, it is characterized in that this method comprises the steps:
The preparation of need testing solution: it is an amount of that the cancellation pain is pasted sample, the accurate title, decide, add ether or chloroform, put in the apparatus,Soxhlet's, refluxing extraction 1～12 hour or ultrasonic Extraction 5～60 minutes or refluxing extraction 0.5～8 hour or microwave abstracting 0.1～4 hour, filter, the filtrate evaporate to dryness adds methanol constant volume as need testing solution.
The mensuration of finger-print I: chromatographic condition and system suitability test: with SE-54 or OV-1701 or OV-11 is immobile liquid; Chromatographic column is a quartz capillary column, and column temperature is temperature programme, and initial column temperature is 100～170 ℃, after constant 1～15 minute with 1～30 ℃/minute rise to 170～230 ℃ constant 1～30 minute, carrier gas is high purity nitrogen, and detecting device is a hydrogen flame detector, adopts and does not shunt or the split sampling mode; Accurate need testing solution 0.5～5 μ L that draws, use gas chromatograph for determination, the relative retention time and the relative peak area of No. 10 chromatographic peaks (characteristic peak of eucalyptol) are 1, calculate relative retention time and relative peak area, promptly obtain the standard finger-print I that disappears and paste bitterly.
The mensuration of finger-print II: measure identical chromatographic condition according to the preparation method of described need testing solution and GC and carry out GC/MS and analyze and obtain No. 10 with reference to the structural information at peak and identify characteristic peak into eucalyptol; Obtain GC/MS total ion current figure simultaneously and constitute the standard finger-print II that the pain that disappears is pasted.
2, according to claim 1 disappear the pain paste powder or cream or extract method of quality control, it is characterized in that: this method is, it is an amount of that the cancellation pain is pasted sample, accurate claim fixed, add ether or chloroform, put in the apparatus,Soxhlet's, 0.5～8 hour microwave abstracting of refluxing extraction 1～12 hour or ultrasonic Extraction 5～60 minutes or refluxing extraction 0.1～4 hour filters, the filtrate evaporate to dryness, add methanol constant volume, miillpore filter (0.45 μ m) filters, as the need testing solution of the pain subsides that disappear; According to an appendix VIE of Chinese Pharmacopoeia version in 2005 vapor-phase chromatography test, be immobile liquid with SE-54 or OV-1701 or OV-11; Chromatographic column is a quartz capillary column, and column temperature is temperature programme, and initial column temperature is 100～170 ℃, after constant 1～15 minute with 1～30 ℃/minute rise to 170～230 ℃ constant 1～30 minute, carrier gas is high purity nitrogen, detecting device is a hydrogen flame detector; Draw need testing solution 0.5 μ L～5 μ L, inject gas chromatograph, the relative retention time and the relative peak area of No. 10 chromatographic peaks (characteristic peak of eucalyptol) they are 1, calculate relative retention time and relative peak area, promptly obtain the standard finger-print I that disappears and paste bitterly.
3, according to claim 1 disappear the pain paste powder or cream or extract method of quality control, it is characterized in that: this method is, it is an amount of that the cancellation pain is pasted sample, accurate claim fixed, add ether or chloroform, put in the apparatus,Soxhlet's, recessed stream extraction 1～12 hour or ultrasonic Extraction 5～60 minutes or refluxing extraction 0.5～8 hour or Microwave Extraction 0.1～4 hour are filtered, the filtrate evaporate to dryness, add methanol constant volume, miillpore filter (0.45 μ m) filters, as the need testing solution of the pain subsides that disappear; According to the test of an appendix VIE of Chinese Pharmacopoeia version in 2005 vapor-phase chromatography, be immobile liquid with SE-54; Chromatographic column is a quartz capillary column, and column temperature is temperature programme, and initial column temperature is 100 ℃, rises to 140 ℃ with 10 ℃/minute after constant 1 minute, after constant again 2 minutes 2 ℃/minute rise to 230 ℃ constant 30 minutes; Draw need testing solution 0.5 μ L, inject gas chromatograph, the relative retention time and the relative peak area of No. 10 chromatographic peaks (characteristic peak of eucalyptol) they are 1, calculate relative retention time and relative peak area, promptly obtain analgesic plaster extract standard finger-print I.
According to claim 2 or the 3 described pains that disappear paste powder or cream or extract method of quality control described in need testing solution the preparation method and measure identical GC chromatographic condition with finger-print I and advance GC/MS and analyze the accurate finger-print II of decals bitterly that disappears that resulting GC/MS total ion current figure constitutes.
5, paste the method for quality control of powder or cream or extract bitterly according to claim 2 or 3 described disappearing, it is characterized in that: this method is: the pain that disappears is pasted powder or cream or extract sample test liquid according to gas chromatography determination, chromatographic column is a quartz capillary column, adopt and do not shunt (or shunting) input mode, theoretical cam curve is calculated with No. 10 peaks, theoretical cam curve is calculated with No. 10 peaks, is not less than 40000.
6, the pain that disappears according to claim 5 is pasted the method for quality control of powder or cream or extract, it is characterized in that: this method is middle packed column with SE-54 or OV-1701 or OV-11 is immobile liquid; Chromatographic column is a quartz capillary column, and column parameter is φ 0.22mm * (20m～35m).
7, according to claim 1 disappear the pain paste powder or cream or extract method of quality control, it is characterized in that: the preparation method of need testing solution is: the cancellation pain is pasted sample 0.5～2g, the accurate title, decide, add ether, put in the apparatus,Soxhlet's, refluxing extraction 1～12 hour, the extract evaporate to dryness adds methanol constant volume as need testing solution.
8, paste the method for quality control of powder or cream or extract bitterly according to claim 2 or 3 described disappearing, it is characterized in that the common characteristic fingerprint peaks has 18 among described disappear pain accurate finger-print I of decals or the II, its peak area summation accounts for more than 90% of total peak area.
9, paste the method for quality control of powder or cream or extract according to claim 2,3, the 8 described pains that disappear, it is characterized in that among described disappear pain accurate finger-print I of decals or the II, chromatographic peak relative retention time and relative peak area with eucalyptol are 1, and the common characteristic fingerprint peaks is selected from:
No. 1 peak: relative retention time 2.08～3.86, relative peak area 2.06～685.73;
No. 2 peaks: relative retention time 2.00～3.68, relative peak area 5.88～552.83;
No. 3 peaks: relative retention time 1.00～2.00, relative peak area 54.04～604.21;
No. 4 peaks: relative retention time 1.00～2.00, relative peak area 9.60～560.99;
No. 5 peaks: relative retention time 0.99～1.99, relative peak area 8.30～604.11;
No. 6 peaks: relative retention time 0.89～1.55, relative peak area 10.44～86.90;
No. 7 peaks: relative retention time 0.87～1.54, relative peak area 10.31～640.7;
No. 8 peaks: relative retention time 0.86～1.53, relative peak area 1.05～20.78;
No. 9 peaks: relative retention time 0.85～1.51, relative peak area 5.72～218.28;
No. 10 peaks (with reference to the peak): relative retention time 1, relative peak area 1;
No. 11 peaks: relative retention time 0.81～1.50, relative peak area 3.90～384.76;
No. 12 peaks: relative retention time 0.80～1.49, relative peak area 2.84～444.0;
No. 13 peaks: relative retention time 0.78～1.47, relative peak area 6.98～311.99;
No. 14 peaks: relative retention time 0.76～1.45, relative peak area 5.89～80.98;
No. 15 peaks: relative retention time 0.64～1.43, relative peak area 0.64～20.99;
No. 16 peaks: relative retention time 0.53～1.40, relative peak area 8.98～560.04;
No. 17 peaks: relative retention time 0.52～1.38, relative peak area 14.77～523.15;
No. 18 peaks: relative retention time 0.48～1.20, relative peak area 22.32～600.34.
10, paste the method for quality control of powder or cream or extract according to claim 2,3, the 6 described pains that disappear, it is characterized in that among described the disappear accurate finger-print I of pain decals, the II, chromatographic peak relative retention time and relative peak area with eucalyptol are 1, and the common characteristic fingerprint peaks is selected from:
No. 1 peak: relative retention time 3.78, relative peak area 3.06～585.73;
No. 2 peaks: relative retention time 2.42, relative peak area 7.88～452.88;
No. 3 peaks: relative retention time 1.61, relative peak area 14.04～504.20;
No. 4 peaks: relative retention time 1.33, relative peak area 8.60～460.90;
No. 5 peaks: relative retention time 1.22, relative peak area 18.30～504.20;
No. 6 peaks: relative retention time 1.21, relative peak area 20.44～146.96;
No. 7 peaks: relative retention time 1.06, relative peak area 30.31～540.7;
No. 8 peaks: relative retention time 1.03, relative peak area 2.17～8.23;
No. 9 peaks: relative retention time 1.02, relative peak area 15.22～163.28;
No. 10 peaks (with reference to the peak): relative retention time 1, relative peak area 1;
No. 11 peaks: relative retention time 0.98, relative peak area 10.99～218.24;
No. 12 peaks: relative retention time 0.95, relative peak area 11.84～349.75;
No. 13 peaks: relative retention time 0.88, relative peak area 12.11;
No. 14 peaks: relative retention time 0.86, relative peak area 12.25～40.78;
No. 15 peaks: relative retention time 0.82, relative peak area 1.61～9.97;
No. 16 peaks: relative retention time 0.78, relative peak area 16.73～460.90;
No. 17 peaks: relative retention time 0.72, relative peak area 24.97～425.14;
No. 18 peaks: relative retention time 0.60, relative peak area 52.71～486.48.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638444A (en) * | 2012-12-20 | 2014-03-19 | 浙江农林大学 | Effective part of cheezheng pain relieving plaster and preparation method therefor |
| CN107102070A (en) * | 2017-03-25 | 2017-08-29 | 甘肃奇正藏药有限公司 | Analgesic plaster finger print quality detecting method |
| CN115128201A (en) * | 2022-07-26 | 2022-09-30 | 吉首大学 | Gas chromatography-mass spectrometry fingerprint identification method for paulownia leaves |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1141575C (en) * | 2001-06-29 | 2004-03-10 | 天津市金士力药物研究开发有限公司 | Red sage medicine fingerprint establishing method and standard fingerprint atlas |
| CN100339706C (en) * | 2003-06-19 | 2007-09-26 | 北京中医药大学 | Quality control method of injection agent for treating apoplexia |
| CN1538170A (en) * | 2003-08-07 | 2004-10-20 | 广州市香雪制药股份有限公司 | Finger print atlas detection technique for antivirus oral liquid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638444A (en) * | 2012-12-20 | 2014-03-19 | 浙江农林大学 | Effective part of cheezheng pain relieving plaster and preparation method therefor |
| CN103638444B (en) * | 2012-12-20 | 2020-07-14 | 浙江农林大学 | Effective part of Qizheng pain-relieving plaster and its preparation method |
| CN107102070A (en) * | 2017-03-25 | 2017-08-29 | 甘肃奇正藏药有限公司 | Analgesic plaster finger print quality detecting method |
| CN115128201A (en) * | 2022-07-26 | 2022-09-30 | 吉首大学 | Gas chromatography-mass spectrometry fingerprint identification method for paulownia leaves |
| CN115128201B (en) * | 2022-07-26 | 2023-08-25 | 吉首大学 | Gas chromatography-mass spectrometry fingerprint identification method for paulownia tomentosa leaves |
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