CN1277117C - Method for determining fingerprint pattern of white atractylodes rhizome as a medicinal material - Google Patents
Method for determining fingerprint pattern of white atractylodes rhizome as a medicinal material Download PDFInfo
- Publication number
- CN1277117C CN1277117C CN 200410028081 CN200410028081A CN1277117C CN 1277117 C CN1277117 C CN 1277117C CN 200410028081 CN200410028081 CN 200410028081 CN 200410028081 A CN200410028081 A CN 200410028081A CN 1277117 C CN1277117 C CN 1277117C
- Authority
- CN
- China
- Prior art keywords
- atractylodes rhizome
- medicinal material
- solution
- acetonitrile
- quality
- 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.)
- Expired - Fee Related
Links
- 241000132012 Atractylodes Species 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N acetonitrile Substances CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000013558 reference substance Substances 0.000 claims description 12
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 9
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 9
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008055 phosphate buffer solution Substances 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 150000002596 lactones Chemical class 0.000 claims description 4
- 239000012982 microporous membrane Substances 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000008363 phosphate buffer Substances 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 238000011156 evaluation Methods 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract 1
- 239000012088 reference solution Substances 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 206010010774 Constipation Diseases 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000002946 Total quality control Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The present invention relates to a measuring method for monitoring the quality of a raw medicinal material (white atractylodes rhizome) in the whole process of each step during a production technical flow by using fingerprint characteristics. The quality of the raw medicinal material (white atractylodes rhizome) is comprehensively monitored by comparing the fingerprint of a reference solution measured by a liquid phase chromatograph and the fingerprint of a sample solution by computer-assisted similarity evaluation software. The present invention can ensure the stability and uniformity of the product technology and the product quality and provide an effective detection method of the product quality and an evaluation reference for technological innovation.
Description
Technical field
The present invention relates to a kind of employing fingerprint figure spectrum signature, the assay method that the quality in the raw medicinal material bighead atractylodes rhizome each step in the technological process of production is monitored.
Background technology
Finger-print acts on great in the Chinese patent drug total quality control, because Chinese medicine finished product and decocting liquid, component content before and after the alcohol precipitation is variant, the employing fingerprint collection of illustrative plates is measured each step in the Chinese medicine technological process of production, can investigate the situation of change of each composition, instruct production technology, guarantee the steady quality of product.With constipation port clothes liquid is example, at present, domesticly still the quality of each step in the whole production technological process of the logical oral liquid of constipation and the raw medicinal material bighead atractylodes rhizome thereof is not carried out overall monitor.
Summary of the invention
The objective of the invention is: the chromatographic fingerprinting that makes up the raw medicinal material bighead atractylodes rhizome, get its finger-print feature, and utilize this finger-print feature, the quality of the overall monitor raw medicinal material bighead atractylodes rhizome is with the raw medicinal material bighead atractylodes rhizome solution finger print measuring method of stable, the homogeneous of guaranteeing product quality.
The objective of the invention is to realize by following approach: with octadecylsilane chemically bonded silica is filling agent, 0.05mol/l potassium dihydrogen phosphate (KH
2PO
4) buffer solution (pH=2.5)-acetonitrile system is moving phase, gradient condition is: T (minute) be 0～80; A% (the 0.05mol/l potassium dihydrogen phosphate buffer solution is than acetonitrile) is 90～95: 45～55; The detection wavelength is 220nm; Column temperature is 35 ℃;
It is an amount of that precision takes by weighing hydroxyl atractylodes lactone reference substance, adds 15～60% acetonitriles and make dissolving, makes the contrast liquid of 200 μ g/ml;
Precision is measured the confession of bighead atractylodes rhizome examination finished product 10ml in the raw material, add water 10ml and be transferred in the separating funnel, extract three times, each 20ml with ethyl acetate, merge extract, decompression and solvent recovery is to doing, and residue quantitatively is transferred in the 10ml measuring bottle with 15～60% acetonitriles, adds 15～60% acetonitriles to the 10ml scale, shake up, with 0.45 μ m filtering with microporous membrane, get filtered fluid, promptly get need testing solution;
Respectively accurate reference substance solution and each 20 μ l of need testing solution of drawing inject liquid chromatograph, measure chromatogram, with the finger-print of need testing solution and reference substance common pattern collection of illustrative plates as calculated the auxiliary similarity evaluation software of machine compare.
This raw medicinal material bighead atractylodes rhizome finger print measuring method, the finished product, the half-finished quality monitoring that go for the use raw medicinal material bighead atractylodes rhizomes such as the logical oral liquid of constipation are measured.
The present invention compares background technology following advantage: can carry out quality monitoring in the overall process of producing to the raw medicinal material bighead atractylodes rhizome, effectively control the quality of the raw medicinal material bighead atractylodes rhizome, guarantee the product process stabilizing, guarantee constant product quality, homogeneous.
Embodiment
Raw medicinal material bighead atractylodes rhizome finger print measuring method of the present invention: with octadecylsilane chemically bonded silica is filling agent, 0.05mol/l potassium dihydrogen phosphate (KH
2PO
4) buffer solution (pH=2.5)-acetonitrile system is moving phase, gradient condition is: T (minute) be 0～80; A% (the 0.05mol/l potassium dihydrogen phosphate buffer solution is than acetonitrile) is 90～95: 45～55; The detection wavelength is 220nm; Column temperature is 35 ℃;
It is an amount of that precision takes by weighing hydroxyl atractylodes lactone reference substance, adds 15～60% acetonitriles and make dissolving, makes the contrast liquid of 200 μ g/ml;
Precision is measured the confession of bighead atractylodes rhizome examination finished product 10ml in the raw material, add water 10ml and be transferred in the separating funnel, extract three times, each 20ml with ethyl acetate, merge extract, decompression and solvent recovery as for, residue quantitatively is transferred in the 10ml measuring bottle with 15～60% acetonitriles, adds 15～60% acetonitriles to the 10ml scale, shake up, with 0.45 μ m filtering with microporous membrane, get filtered fluid, promptly get need testing solution;
Respectively accurate reference substance solution and each 20 μ l of need testing solution of drawing inject liquid chromatograph, measure chromatogram, with the finger-print of need testing solution and reference substance common pattern collection of illustrative plates as calculated the auxiliary similarity evaluation software of machine compare.
The most preferred embodiment of raw medicinal material bighead atractylodes rhizome solution finger print measuring method of the present invention is: with octadecylsilane chemically bonded silica is filling agent, 0.05mol/l potassium dihydrogen phosphate (KH
2PO
4) buffer solution (pH=2.5)-acetonitrile system is moving phase, gradient condition is: T (minute) be 0～80; A% (the 0.05mol/l potassium dihydrogen phosphate buffer solution is than acetonitrile) is 90: 55.The detection wavelength is 220nm; Column temperature is 35 ℃.
It is an amount of that precision takes by weighing hydroxyl atractylodes lactone reference substance, adds 30% acetonitrile and make dissolving, makes the contrast liquid of 200 μ g/ml.
Precision is measured raw medicinal material bighead atractylodes rhizome solution 10ml again, add water 10ml and be transferred in the separating funnel, extract three times, each 20ml with ethyl acetate, merge extract, decompression and solvent recovery is to doing, and residue quantitatively is transferred in the 10ml measuring bottle with 30% acetonitrile, adds 30% acetonitrile to the 10ml scale, shake up, with 0.45 μ m filtering with microporous membrane, get filtered fluid, promptly get raw medicinal material bighead atractylodes rhizome need testing solution.
Then, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure chromatogram, the chromatogram of need testing solution should detect with reference to the identical vindication art chromatographic peak of finger-print, finger-print and the auxiliary similarity evaluation software of machine (as " the area of computer aided similarity evaluation system " of the Central South University's exploitation) comparison as calculated of reference substance common pattern collection of illustrative plates with need testing solution, similarity coefficient should be lower than 0.85, illustrates that like this content of the bighead atractylodes rhizome is qualified in the need testing solution.
Claims (2)
1, a kind of employing fingerprint collection of illustrative plates method that the quality of the raw medicinal material bighead atractylodes rhizome in production technology monitored, it is characterized in that: with octadecylsilane chemically bonded silica is filling agent, pH is that 0.05mol/l potassium dihydrogen phosphate buffer solution-acetonitrile system of 2.5 is a moving phase, and gradient condition is: T is 0～80 minute; 0.05mol/l potassium dihydrogen phosphate buffer solution: acetonitrile is 90～95: 45～55; The detection wavelength is 220nm; Column temperature is 35 ℃;
It is an amount of that precision takes by weighing hydroxyl atractylodes lactone reference substance, adds 15～60% acetonitriles and make dissolving, makes the contrast liquid of 200 μ g/ml; Precision is measured the confession of bighead atractylodes rhizome examination finished product 10ml in the raw material, add water 10ml and be transferred in the separating funnel, extract three times, each 20ml with ethyl acetate, merge extract, decompression and solvent recovery is to doing, and residue quantitatively is transferred in the 10ml measuring bottle with 15～60% acetonitriles, adds 15～60% acetonitriles to the 10ml scale, shake up, with 0.45 μ m filtering with microporous membrane, get filtered fluid, promptly get need testing solution;
Respectively accurate reference substance solution and each 20 μ l of need testing solution of drawing inject liquid chromatograph, measure chromatogram, with the finger-print of need testing solution and reference substance common pattern collection of illustrative plates as calculated the auxiliary similarity evaluation software of machine compare.
2, employing fingerprint collection of illustrative plates according to claim 1 method that the quality of the raw medicinal material bighead atractylodes rhizome in production technology monitored, it is characterized in that: in the moving phase, the 0.05mol/l potassium dihydrogen phosphate buffer solution is 90: 55 than the value of acetonitrile; Employed acetonitrile solution content is 30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410028081 CN1277117C (en) | 2004-07-15 | 2004-07-15 | Method for determining fingerprint pattern of white atractylodes rhizome as a medicinal material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410028081 CN1277117C (en) | 2004-07-15 | 2004-07-15 | Method for determining fingerprint pattern of white atractylodes rhizome as a medicinal material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1595145A CN1595145A (en) | 2005-03-16 |
| CN1277117C true CN1277117C (en) | 2006-09-27 |
Family
ID=34664136
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410028081 Expired - Fee Related CN1277117C (en) | 2004-07-15 | 2004-07-15 | Method for determining fingerprint pattern of white atractylodes rhizome as a medicinal material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1277117C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078713B (en) * | 2007-06-28 | 2010-08-11 | 上海现代中医药技术发展有限公司 | Fingerprint detection method of gynostemma pentaphylla medicine added with internal standard |
| CN102680631B (en) * | 2012-05-24 | 2014-02-26 | 成都中医药大学 | Detection method for atractylodes macrocephala koidz medicinal materials |
| CN102798686A (en) * | 2012-07-23 | 2012-11-28 | 山西省肿瘤医院 | Method for building high performance liquid chromatography (HPLC) fingerprint spectrum of largehead atractylodes rhizome essential oil after oxygenolysis |
| CN109061024B (en) * | 2018-10-17 | 2021-02-23 | 湖南时代阳光药业股份有限公司 | Construction method and application of standard fingerprint spectrum of infant spleen-supporting granules |
| CN109507356B (en) * | 2018-12-30 | 2020-01-07 | 鲁南制药集团股份有限公司 | Quality detection method of 'Hui Tongbiang' capsule |
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2004
- 2004-07-15 CN CN 200410028081 patent/CN1277117C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
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| CN1595145A (en) | 2005-03-16 |
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Owner name: GUANGZHOU BAIYUNSHAN ZHONGYI PHARMACEUTICAL CO., L Free format text: FORMER NAME: GUANGZHOU ZHONGYI PHARMACEUTICAL CO., LTD. |
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Address after: 510530, No. 32, Po pan Road, Guangzhou, Guangdong, Luogang District Patentee after: GUANGZHOU BAIYUNSHAN ZHONGYI PHARMACEUTICAL Co.,Ltd. Address before: 11, building 510620, west block, Times Square, 28 Tianhe North Road, Guangzhou, Guangdong Patentee before: GUANGZHOU ZHONGYI PHARMACEUTICAL Co.,Ltd. |
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Granted publication date: 20060927 |