CN1563975A - Quality control method for 9-staged tea extraction - Google Patents
Quality control method for 9-staged tea extraction Download PDFInfo
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- CN1563975A CN1563975A CN 200410026578 CN200410026578A CN1563975A CN 1563975 A CN1563975 A CN 1563975A CN 200410026578 CN200410026578 CN 200410026578 CN 200410026578 A CN200410026578 A CN 200410026578A CN 1563975 A CN1563975 A CN 1563975A
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- 238000003908 quality control method Methods 0.000 title claims description 6
- 238000000605 extraction Methods 0.000 title description 2
- 241001122767 Theaceae Species 0.000 title 1
- 230000014759 maintenance of location Effects 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 241000736026 Sarcandra Species 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 14
- HOEVRHHMDJKUMZ-UHFFFAOYSA-N Isofraxidin Chemical compound C1=CC(=O)OC2=C1C=C(OC)C(O)=C2OC HOEVRHHMDJKUMZ-UHFFFAOYSA-N 0.000 claims description 11
- ANCHXLMTFNOVDK-UHFFFAOYSA-N Isofraxidin Natural products COC1=C(O)C(OC)=CC2=C1OC=CC2=O ANCHXLMTFNOVDK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000012088 reference solution Substances 0.000 claims description 5
- 230000005526 G1 to G0 transition Effects 0.000 claims description 3
- ZCHPKWUIAASXPV-UHFFFAOYSA-N acetic acid;methanol Chemical compound OC.CC(O)=O ZCHPKWUIAASXPV-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- 238000004811 liquid chromatography Methods 0.000 claims description 2
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 2
- 206010061218 Inflammation Diseases 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- 229940079593 drug Drugs 0.000 description 6
- 239000002775 capsule Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 206010003011 Appendicitis Diseases 0.000 description 1
- 208000004429 Bacillary Dysentery Diseases 0.000 description 1
- 206010007882 Cellulitis Diseases 0.000 description 1
- 208000005577 Gastroenteritis Diseases 0.000 description 1
- 206010017915 Gastroenteritis shigella Diseases 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 206010000269 abscess Diseases 0.000 description 1
- 208000012873 acute gastroenteritis Diseases 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 1
- 201000005113 shigellosis Diseases 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Quality of product is controlled by fingerprint based on high performance liquid chromatography. Standard fingerprint includes more than eight peaks of characteristic fingerprint. Suppose that retention time of chromatographic peak is one, other peaks are 0.22 minus or plus 0.01, 27 minus or plus 0.01, 0.49 minus or plus 0.01, 0.550.01 etc. Degree of similarity between fingerprint of sample to be tested and standard fingerprint must not be lower than 0.90. The method controls quality, reproducibility, stability etc. effectively.
Description
Affiliated technical field
The present invention relates to the drug chemistry analytical approach, specifically the method for quality control of Chinese crude drug sarcandra water extract.
Background technology
Chinese patent drug " heat-clearing inflammation-diminishing " is to carry the Chinese patent drug of being processed into through water by Chinese crude drug " sarcandra ", have clearing heat and detoxicating, anti-inflammatory analgetic, the effect of stimulating the circulation of the blood and cause the muscles and joints to relax, be used for influenza, sphagitis, pneumonia, bacillary dysentery, acute gastroenteritis, appendicitis, burn, sore abscess, cellulitis.Owing to determined curative effect, have no adverse reaction, enjoy doctor, patient's welcome.But, the preparation of making as the water extract of sarcandra exists many shortcomings as the method for quality control of " heat-clearing inflammation-diminishing " capsule: it only has identification, it only is the qualitative identification whether sugar, flavones are arranged in a kind of product, this identification is the non-exclusive reaction, can not reflect well that whether product has used sarcandra is that raw material is made.For this reason, be necessary to seek a kind of method that can control the heat-clearing inflammation-diminishing product quality.
Finger-print is can estimate the Chinese herbal product quality a kind of easy and simple to handle, and is stable, precision is high, the practicable method of favorable reproducibility.
Summary of the invention
The quality of the water extract of the objective of the invention is to set up that a kind of method is easy, stable, precision is high, the method for the finger-print of favorable reproducibility and standard finger-print thereof being controlled sarcandra or " heat-clearing inflammation-diminishing " capsule made from water extract.
Technical scheme of the present invention is with extraction process by water conventional in the herbal pharmaceutical industry, get the Chinese crude drug sarcandra and be raw material and get the sarcandra water extract or get the finger-print that QINGRE XIAOYANNING JIAONANG that the sarcandra water extract makes adopts high performance liquid chromatography to establish and come control of quality, its method is carried out as follows:
The preparation of step 1, need testing solution: get sarcandra, the boiling secondary, merging filtrate, be condensed into thick paste, low temperature drying, be ground into fine powder, get fine powder and be made into the aqueous solution that contains the 10mg fine powder among every 1ml, or the content of directly getting QINGRE XIAOYANNING JIAONANG is made into the aqueous solution that contains the 10mg fine powder among every 1ml;
The preparation of step 2, reference substance solution: get isofraxidin and be made into the aqueous solution that contains 0.1mg concentration among every 1ml;
The foundation of step 3, finger-print: precision is got need testing solution and each 10 μ l of object of reference solution respectively, inject high performance liquid chromatograph respectively, according to high effective liquid chromatography for measuring, the record chromatogram, the finger-print (seeing accompanying drawing 1) that settles the standard should have eight above characteristic fingerprint peaks, with the retention time of the chromatographic peak of isofraxidin is 1 to calculate relative relative retention time, and each characteristic peak relative retention time is respectively 0.22+0.01,0.27 ± 0.01,0.49 ± 0.01,0.55 ± 0.01,1.00 (S), 1.12 ± 0.03,1.23 ± 0.01,1.45 ± 0.01; The similarity of test sample finger-print and standard finger-print must not be less than 0.90.
Adopt different high performance liquid chromatographs and select for use the appearance time, retention time, peak area of eight characteristic peaks of its standard finger-print of difference of chromatographic condition can be different, the present invention through repeatedly, repeatedly test and condition grope, establish preferable chromatographic condition to be: octadecylsilane chemically bonded silica is a stationary phase; 0.1% acetate methanol solution-0.1% acetic acid aqueous solution is a moving phase, linear gradient elution; Flow velocity is 0.5ml/min; Detect wavelength 340nm; Column temperature is 40 ℃; Calculate with isofraxidin, theoretical cam curve is not less than 20000.
Superiority of the present invention is: set up the standard finger-print of sarcandra water extract, conveniently distinguished the positive vacation of heat-clearing inflammation-diminishing product, can control the quality of product effectively; This method reappearance, good stability, method of operating is easy, precision is high.
Elaborate technical scheme of the present invention below in conjunction with embodiment and accompanying drawing thereof.
Description of drawings
Fig. 1, be the standard finger-print of sarcandra water extract.
Fig. 2, be the high-efficient liquid phase chromatogram of object of reference isofraxidin.
Fig. 3,13 batches of finger-prints for test agent.
Fig. 4,5 batches of finger-prints for test agent.
Specific embodiments
The foundation of embodiment 1, standard finger-print.
Concrete operation method is as follows:
The formulations prepared from solutions of step 1, test sample: sample 1, get sarcandra 2192kg, decocting twice each two hours, filters merging filtrate, be condensed into thick paste, fine powder is worn in low temperature drying, gets fine powder 219kg, be settled to 25ml after getting the dissolving of fine powder 0.25g water, promptly get the aqueous solution that contains the 10mg fine powder among the 1ml;
The preparation of step 2, object of reference solution: precision takes by weighing the isofraxidin standard items 1mg that the calibrating of Chinese biological goods is provided, and places the 10ml measuring bottle, and water dissolving and rare pool promptly get the aqueous solution that contains 0.1mg concentration among the 1ml to scale;
The foundation of step 3, standard finger-print:
Adopt Agilent 1100 high performance liquid chromatographs, with Agilent Hypersil ODS post (5-Micron, 4.0mm * 250mm), octadecylsilane chemically bonded silica is a stationary phase, 0.1% acetate methanol solution-0.1% acetic acid aqueous solution is a moving phase, linear gradient elution; Flow velocity is 0.5ml/min; Detect wavelength 340nm; Column temperature is 40 ℃; Calculate with isofraxidin, theoretical cam curve is 24576.
Get object of reference solution 10 μ l and inject high performance liquid chromatograph, get high-efficient liquid phase chromatogram, see accompanying drawing 2;
Get need testing solution 10 μ l and inject high performance liquid chromatograph, get high-efficient liquid phase chromatogram;
With need testing solution sample 1, continuous sample introduction is totally 5 times in one day, writes down the retention time and the area of each chromatographic peak, is reference with the isofraxidin, calculates relative retention time and peak area ratio and RSD such as table 1 and table 2
Table 1 relative retention time variation situation
| Relative retention time | On average | ????RSD％ | ||||
| ????1 | ????2 | ????3 | ????4 | ????5 | ||
| ????0.224 | ????0.222 | ????0.225 | ????0.225 | ????0.225 | ??0.224 | ????0.58％ |
| ????0.27 | ????0.271 | ????0.271 | ????0.271 | ????0.271 | ??0.271 | ????0.17％ |
| ????0.485 | ????0.49 | ????0.488 | ????0.488 | ????0.488 | ??0.488 | ????0.37％ |
| ????0.544 | ????0.547 | ????0.547 | ????0.547 | ????0.545 | ??0.546 | ????0.26％ |
| ????1 | ????1 | ????1 | ????1 | ????1 | ??1 | ????0.00％ |
| ????1.116 | ????1.111 | ????1.111 | ????1.114 | ????1.114 | ??1.113 | ????0.19％ |
| ????1.226 | ????1.222 | ????1.222 | ????1.225 | ????1.225 | ??1.224 | ????0.15％ |
| ????1.447 | ????1.444 | ????1.442 | ????1.444 | ????1.444 | ??1.444 | ????0.12％ |
Table 2 peak area ratio precision
| Peak area ratio | On average | ????RSD％ | ||||
| ????1 | ????2 | ????3 | ????4 | ????5 | ||
| ????0.432 | ????0.427 | ????0.427 | ????0.432 | ????0.427 | ??0.429 | ????0.64％ |
| ????1.351 | ????1.333 | ????1.333 | ????1.351 | ????1.333 | ??1.34 | ????0.74％ |
| ????2.189 | ????2.16 | ????2.16 | ????2.176 | ????2.147 | ??2.166 | ????0.75％ |
| ????2.338 | ????2.32 | ????2.32 | ????2.338 | ????2.307 | ??2.325 | ????0.57％ |
| ????1 | ????1 | ????1 | ????1 | ????1 | ??1 | ????0.00％ |
| ????1.986 | ????2 | ????1.973 | ????2 | ????1.987 | ??1.989 | ????0.57％ |
| ????5.73 | ????5.667 | ????5.627 | ????5.689 | ????5.613 | ??5.665 | ????0.84％ |
| ????0.257 | ????0.253 | ????0.253 | ????0.257 | ????0.253 | ??0.255 | ????0.86％ |
As seen from table, the RSD of each chromatographic peak relative retention time and peak area ratio illustrates instrument stabilizer all less than 2%; Need testing solution has good stability within one day at normal temperatures.
The finger-print of sample 2～14 is seen accompanying drawing 3.The fingerprint peaks retention time sees Table 3; The relative retention time of fingerprint peaks sees Table 4; The peak area value of fingerprint peaks sees Table 5; The fingerprint peaks area ratio sees Table 6;
Table 3 heat-clearing inflammation-diminishing fingerprint peaks retention time (min)
| Lot number | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| ??011114 | ??6.55 | ??7.97 | ??14.44 | ??16.12 | ??29.49 | ??33.04 | ??36.30 | ??42.76 |
| ??011241 | ??6.57 | ??7.96 | ??14.42 | ??16.1 | ??29.38 | ??32.86 | ??36.11 | ??42.56 |
| ??011242 | ??6.59 | ??7.95 | ??14.35 | ??15.95 | ??29.18 | ??32.73 | ??36.09 | ??42.55 |
| ??020101 | ??6.57 | ??7.99 | ??14.48 | ??16.16 | ??29.45 | ??32.94 | ??36.19 | ??42.66 |
| ??010202 | ??6.59 | ??7.96 | ??14.38 | ??15.95 | ??29.21 | ??32.84 | ??36.18 | ??42.67 |
| ??020103 | ??6.59 | ??7.95 | ??14.34 | ??15.95 | ??29.17 | ??32.7 | ??36.06 | ??42.56 |
| ??020104 | ??6.59 | ??8.08 | ??14.64 | ??16.3 | ??29.59 | ??32.36 | ??36.36 | ??42.78 |
| ??020105 | ??6.57 | ??7.97 | ??14.43 | ??16.11 | ??29.42 | ??32.93 | ??36.18 | ??42.63 |
| ??020106 | ??6.58 | ??8.04 | ??14.58 | ??16.26 | ??29.56 | ??33.02 | ??36.28 | ??42.75 |
| ??020107 | ??6.59 | ??7.98 | ??14.39 | ??16.01 | ??29.23 | ??32.8 | ??36.13 | ??42.6 |
| ??020108 | ??6.59 | ??7.98 | ??14.43 | ??16.01 | ??29.22 | ??32.83 | ??36.17 | ??42.63 |
| ??020109 | ??6.6 | ??8.09 | ??14.66 | ??16.33 | ??29.58 | ??33.1 | ??36.37 | ??42.8 |
| ??020110 | ??6.59 | ??7.97 | ??14.38 | ??15.98 | ??29.19 | ??32.75 | ??36.08 | ??42.57 |
Table 4 heat-clearing inflammation-diminishing fingerprint peaks relative retention time
| Lot number | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| ????011114 | ??0.22 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.23 | ??1.45 |
| ????011241 | ??0.22 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.23 | ??1.45 |
| ????011242 | ??0.23 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.24 | ??1.46 |
| ????020101 | ??0.22 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.23 | ??1.45 |
| ????010202 | ??0.23 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.24 | ??1.46 |
| ????020103 | ??0.23 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.24 | ??1.46 |
| ????020104 | ??0.22 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.09 | ??1.23 | ??1.45 |
| ????020105 | ??0.22 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.23 | ??1.45 |
| ????020106 | ??0.22 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.23 | ??1.45 |
| ????020107 | ??0.23 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.24 | ??1.46 |
| ????020108 | ??0.23 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.24 | ??1.46 |
| ????020109 | ??0.22 | ??0.27 | ??0.50 | ??0.55 | ??1.00 | ??1.12 | ??1.23 | ??1.45 |
| ????020110 | ??0.23 | ??0.27 | ??0.49 | ??0.55 | ??1.00 | ??1.12 | ??1.24 | ??1.46 |
From the analysis result of 13 batches of heat-clearing inflammation-diminishing products, fingerprint peaks retention time and relative retention time are more stable
Table 5 heat-clearing inflammation-diminishing fingerprint peaks area value
| Lot number | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| ??011114 | ??253.04 | ??611 | ??1024.31 | ??1049.86 | ??811.83 | ??950.12 | ??2434.14 | ??114.74 |
| ??011241 | ??101.07 | ??553.21 | ??960.38 | ??997.13 | ??633.08 | ??398.73 | ??1443.87 | ??75.37 |
| ??011242 | ??196.8 | ??761.71 | ??1292.26 | ??1343.28 | ??865.36 | ??679.72 | ??2861.92 | ??143.37 |
| ??020101 | ??127.42 | ??739.22 | ??1246.12 | ??1284.74 | ??882.85 | ??730.82 | ??2780.9 | ??152.06 |
| ??020202 | ??140.59 | ??715.88 | ??1251.68 | ??1443.95 | ??687.08 | ??697.88 | ??2807.33 | ??151.34 |
| ?020103 | ?175.38 | ?875.85 | ?1397.09 | ?1446.98 | ?967.64 | ?907.3 | ?3650.31 | ?183.18 |
| ?020104 | ?105.78 | ?762.14 | ?1235.33 | ?1248.18 | ?779.44 | ?666.46 | ?3144.95 | ?174.03 |
| ?020105 | ?111.6 | ?820.59 | ?1300.95 | ?1318.68 | ?935.19 | ?722.42 | ?3195.28 | ?183.23 |
| ?020106 | ?102.11 | ?740.53 | ?1209.13 | ?1215.38 | ?179.29 | ?565.21 | ?3233.44 | ?177.34 |
| ?020107 | ?151.64 | ?757.19 | ?1255.38 | ?1298.67 | ?861.17 | ?787.38 | ?3111.7 | ?156.38 |
| ?020108 | ?120.23 | ?557.96 | ?923.45 | ?974.46 | ?597.48 | ?594.09 | ?2439.05 | ?122.54 |
| ?020109 | ?190.64 | ?581.5 | ?951 | ?1015.51 | ?513.64 | ?886.36 | ?2405.18 | ?107.53 |
| ?020110 | ?116.16 | ?541.65 | ?896.04 | ?964.52 | ?424.12 | ?545.52 | ?2378.97 | ?111.94 |
Table 6 heat-clearing inflammation-diminishing fingerprint peaks area ratio
| Lot number | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| ??011114 | ??0.312 | ??0.753 | ??1.262 | ??1.293 | ??1.000 | ??1.170 | ??2.998 | ??0.141 |
| ??011241 | ??0.160 | ??0.874 | ??1.517 | ??1.575 | ??1.000 | ??0.630 | ??2.281 | ??0.119 |
| ??011242 | ??0.227 | ??0.880 | ??1.493 | ??1.552 | ??1.000 | ??0.785 | ??3.307 | ??0.166 |
| ??020101 | ??0.144 | ??0.837 | ??1.411 | ??1.455 | ??1.000 | ??0.828 | ??3.150 | ??0.172 |
| ??020202 | ??0.205 | ??1.042 | ??1.822 | ??2.102 | ??1.000 | ??1.016 | ??4.086 | ??0.220 |
| ??020103 | ??0.181 | ??0.905 | ??1.444 | ??1.495 | ??1.000 | ??0.938 | ??3.772 | ??0.189 |
| ??020104 | ??0.136 | ??0.978 | ??1.585 | ??1.601 | ??1.000 | ??0.855 | ??4.035 | ??0.223 |
| ??020105 | ??0.119 | ??0.877 | ??1.391 | ??1.410 | ??1.000 | ??0.772 | ??3.417 | ??0.196 |
| ??020106 | ??0.570 | ??4.130 | ??6.744 | ??6.779 | ??1.000 | ??3.152 | ??18.035 | ??0.989 |
| ??020107 | ??0.176 | ??0.879 | ??1.458 | ??1.508 | ??1.000 | ??0.914 | ??3.613 | ??0.182 |
| ??020108 | ??0.201 | ??0.934 | ??1.546 | ??1.631 | ??1.000 | ??0.994 | ??4.082 | ??0.205 |
| ??020109 | ??0.371 | ??1.132 | ??1.851 | ??1.977 | ??1.000 | ??1.726 | ??4.683 | ??0.209 |
| ??020110 | ??0.274 | ??1.277 | ??2.113 | ??2.274 | ??1.000 | ??1.286 | ??5.609 | ??0.264 |
Can know that from The above results the RSD of relative retention time, peak area ratio is less, illustrate that the reappearance of this method is good.
Test according to above-mentioned sample, finger-print settles the standard, see accompanying drawing 1, eight above characteristic fingerprint peaks are arranged, with the retention time of the chromatographic peak of isofraxidin is 1 to calculate relative relative retention time, and each characteristic peak relative retention time is respectively 0.22 ± 0.01,0.27 ± 0.01,0.49 ± 0.01,0.55 ± 0.01,1.00 (S), 1.12 ± 0.03,1.23 ± 0.01,1.45 ± 0.01; The finger-print of 13 batch samples and the similarity of standard finger-print are calculated result such as table 7 with area of computer aided similarity computer software
Table 7.13 batch heat-clearing inflammation-diminishing finger-print similarity result of calculation
| 011114 | ?011241 | ?011242 | ?020101 | ?020102 | ?020103 | ?020104 |
| 0.9933 | ?0.9680 | ?0.9986 | ?0.9984 | ?0.9987 | ?0.9984 | ?0.9987 |
| ?020105 | ?020106 | ?020107 | ?020108 | ?020109 | ?020110 |
| ?0.9992 | ?0.9760 | ?0.9992 | ?0.9994 | ?0.9950 | ?0.9978 |
From table as can be known, each batch products finger-print overall similarity is higher, all more than 0.9.
The chromatographic peak relative retention time of the finger-print of embodiment 2,5 batches of commercial production samples of investigation and the variation situation of peak area ratio reach the similarity with standard finger-print.
Method of operating: the preparation of step 1, need testing solution: the lot number of getting Jingxiutang's production respectively is the heat-clearing inflammation-diminishing of C07202, C07203, C08205, C08206, C08207, be settled to 25ml after getting the dissolving of capsule 's content fine powder 0.25g water, that is, prepare 5 parts of test samples altogether;
The finger-print of 5 duplicate samples is seen accompanying drawing 4, and the variation situation and the similarity of its chromatographic peak relative retention time and peak area ratio are as table 8～10.
Table 8 relative retention time reappearance
| Relative retention time | On average | ????RSD％ | ||||
| ????1 | ????2 | ????3 | ????4 | ????5 | ||
| ????0.220 | ????0.222 | ????0.222 | ????0.220 | ????0.221 | ??0.221 | ????0.50％ |
| ????0.272 | ????0.271 | ????0.270 | ????0.271 | ????0.272 | ??0.271 | ????0.31％ |
| ????0.495 | ????0.493 | ????0.492 | ????0.493 | ????0.496 | ??0.494 | ????0.31％ |
| ????0.549 | ????0.550 | ????0.549 | ????0.550 | ????0.553 | ??0.550 | ????0.32％ |
| ????1.000 | ????1.000 | ????1.000 | ????1.000 | ????1.000 | ??1.000 | ????0.00％ |
| ????1.122 | ????1.119 | ????1.119 | ????1.119 | ????1.120 | ??1.120 | ????0.12％ |
| ????1.234 ????1447 | ????1.230 ????1.444 | ????1.230 ????1.442 | ????1.230 ????1.446 | ????1.232 ????1.444 | ??1.231 ??1.445 | ????0.13％ ????0.13％ |
Table 9 peak area ratio reappearance
| Peak area ratio | On average | ?RSD％ | ||||
| ????1 | ????2 | ????3 | ????4 | ????5 | ||
| ????0.81 | ????0.77 | ????0.78 | ????0.78 | ????0.78 | ??0.78 | ?1.93％ |
| ????1.59 | ????1.54 | ????1.56 | ????1.56 | ????1.56 | ??1.56 | ?1.15％ |
| ????2.63 | ????2.63 | ????2.59 | ????2.59 | ????2.59 | ??2.61 | ?0.84％ |
| ????2.60 | ????2.60 | ????2.56 | ????2.58 | ????2.55 | ??2.58 | ?0.88％ |
| ????1.00 | ????1.00 | ????1.00 | ????1.00 | ????1.00 | ??0 | ?0％ |
| ????2.46 | ????2.38 | ????2.42 | ????2.42 | ????2.44 | ??2.42 | ?1.22％ |
| ????6.36 ????0.68 | ????6.17 ????0.68 | ????6.28 ????0.67 | ????6.28 ????0.68 | ????6.28 ????0.68 | ??6.27 ??0.68 | ?1.08％ ?0.66％ |
Can know that from The above results the RSD of relative retention time, peak area ratio is less, illustrate that the reappearance of this method is good.
Similarity result is as follows:
| Lot number | ??C07202 | ??C07203 | ??C08205 | ??C08206 | ??C08207 |
| Similarity | ??0.9985 | ??0.9963 | ??0.9992 | ??0.9958 | ??0.9928 |
Claims (2)
1, a kind of method of quality control of sarcandra water extract is characterized in that adopting the finger-print control of quality, carries out as follows:
Step 1, be the preparation of need testing solution: get sarcandra, the boiling secondary, merging filtrate, be condensed into thick paste, low temperature drying, be ground into fine powder, get fine powder and be made into the aqueous solution that contains the 10mg fine powder among every 1ml, or the content of directly getting QINGRE XIAOYANNING JIAONANG is made into the aqueous solution that contains the 10mg fine powder among every 1ml;
Step 2, be the preparation of object of reference solution: get isofraxidin and be made into the aqueous solution that contains 0.1mg concentration among every 1ml;
Step 3, be the foundation of fingerprint collection of illustrative plates: precision is got need testing solution and each 10 μ 1 of object of reference solution respectively, inject high performance liquid chromatograph respectively, according to high effective liquid chromatography for measuring, the record chromatogram, the finger-print that settles the standard should have eight above characteristic fingerprint peaks, with the retention time of the chromatographic peak of isofraxidin is 1 to calculate relative relative retention time, and each characteristic peak relative retention time is respectively 0.22 ± 0.01,0.27 ± 0.01,0.49 ± 0.01,0.55 ± 0.01,1.00 (S), 1.12 ± 0.03,1.23 ± 0.01,1.45 ± 0.01; The similarity of test sample finger-print and standard finger-print must not be less than 0.90.
2, the method for quality control of sarcandra water extract according to claim 1 is characterized in that the chromatographic condition in the step 3 is: octadecylsilane chemically bonded silica is a stationary phase; 0.1% acetate methanol solution is moving phase, linear gradient elution; Flow velocity is 0.5ml/min; Detect wavelength 340nm; Column temperature is 40 ℃; Calculate with isofraxidin, theoretical cam curve is not less than 20000.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410026578 CN1266473C (en) | 2004-03-24 | 2004-03-24 | Quality control method for 9-staged tea extraction |
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| CN 200410026578 CN1266473C (en) | 2004-03-24 | 2004-03-24 | Quality control method for 9-staged tea extraction |
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| CN1563975A true CN1563975A (en) | 2005-01-12 |
| CN1266473C CN1266473C (en) | 2006-07-26 |
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| CN 200410026578 Expired - Lifetime CN1266473C (en) | 2004-03-24 | 2004-03-24 | Quality control method for 9-staged tea extraction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665479B (en) * | 2009-09-22 | 2012-05-16 | 三明华健生物工程有限公司 | Technology for synchronously extracting isofraxidin and flavonoids compounds from sarcandra glabra and applications thereof |
| CN111721880A (en) * | 2020-07-02 | 2020-09-29 | 江中药业股份有限公司 | Method for establishing fingerprint of sarcandra glabra by using double-column tandem HPLC-MS |
-
2004
- 2004-03-24 CN CN 200410026578 patent/CN1266473C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665479B (en) * | 2009-09-22 | 2012-05-16 | 三明华健生物工程有限公司 | Technology for synchronously extracting isofraxidin and flavonoids compounds from sarcandra glabra and applications thereof |
| CN111721880A (en) * | 2020-07-02 | 2020-09-29 | 江中药业股份有限公司 | Method for establishing fingerprint of sarcandra glabra by using double-column tandem HPLC-MS |
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| Publication number | Publication date |
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| CN1266473C (en) | 2006-07-26 |
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