CN1951408A - Method for detecting saikosaponin A in drop pills of Bupleurum root - Google Patents
Method for detecting saikosaponin A in drop pills of Bupleurum root Download PDFInfo
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- CN1951408A CN1951408A CN 200510015499 CN200510015499A CN1951408A CN 1951408 A CN1951408 A CN 1951408A CN 200510015499 CN200510015499 CN 200510015499 CN 200510015499 A CN200510015499 A CN 200510015499A CN 1951408 A CN1951408 A CN 1951408A
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- preparation process
- test sample
- bupleurum root
- saikoside
- determination step
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 241000202726 Bupleurum Species 0.000 title claims abstract description 22
- 239000006187 pill Substances 0.000 title claims description 21
- KYWSCMDFVARMPN-MSSMMRRTSA-N Saikosaponin A Chemical compound O([C@@H]1[C@@H](O)[C@H](O[C@@H]2[C@@]([C@H]3[C@]([C@@H]4[C@@]([C@@]5(C[C@H](O)[C@]67CO[C@]5([C@@H]6CC(C)(C)CC7)C=C4)C)(C)CC3)(C)CC2)(C)CO)O[C@@H]([C@@H]1O)C)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O KYWSCMDFVARMPN-MSSMMRRTSA-N 0.000 title abstract description 3
- QLPRYZXNWYTFCI-UHFFFAOYSA-N saikosaponin D Natural products CC1OC(OC2CCC3(C)C(CCC4(C)C3C=CC56OCC7(CCC(C)(C)CC57)C(O)CC46C)C2(C)CO)C(O)C(O)C1OC8OC(CO)C(O)C(O)C8O QLPRYZXNWYTFCI-UHFFFAOYSA-N 0.000 title abstract description 3
- PQPVAGWUNWFCJE-UHFFFAOYSA-N saikosaponin a Natural products CC1OC(OC2CCC3(C)C(C2)C(C)(CO)CC4(C)C3C=CC56OCC7(CCC(C)(C)CC57)C(O)CC46C)C(O)C(OC8OC(CO)C(O)C(O)C8O)C1O PQPVAGWUNWFCJE-UHFFFAOYSA-N 0.000 title abstract description 3
- 238000002360 preparation method Methods 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000001514 detection method Methods 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 230000000274 adsorptive effect Effects 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 6
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical group O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 5
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004811 liquid chromatography Methods 0.000 claims description 3
- 239000003463 adsorbent Substances 0.000 claims description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims 3
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 abstract 1
- 239000012488 sample solution Substances 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 27
- 239000013558 reference substance Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000011084 recovery Methods 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000011003 system suitability test Methods 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000012372 quality testing Methods 0.000 description 2
- 238000004809 thin layer chromatography Methods 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002389 essential drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007962 solid dispersion Substances 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a high-effect liquid spectrum method of saikosaponin A in bupleurum root droo. Wherein, it comprises the sample solution preparation and testing step; the first step comprise that (a), selecting some sample; (b), dissolving with alkali solution; (c), using large hole to absorb resin post; (d), washing; (e), collecting organic solvent washed liquid, to be concentrated and dried; (f), dissolving. The invention has high resolution, accuracy and sensitivity.
Description
Technical field
The present invention relates to field of medicaments, be specifically related to a kind of detection method of bupleurum root dropping pills.
Background technology
Radix Bupleuri has long use history, its medical value has obtained affirming of successive dynasties famous expert.Bupleurum root dropping pills is the modern Chinese medicine preparation of Tianjin Tasly Pharmaceutical Co., Ltd's development, is Chinese medicine the 4th kind new medicine (traditional Chinese medicines card word Z19990012), and has taken in country " essential drug list " (2000, serial number 18).Bupleurum root dropping pills is to select first-class Radix Bupleuri for use, utilizes modern high tech method, and the effective ingredient that is extracted by Radix Bupleuri adds a kind of solid dispersion that is the high degree of dispersion state that suitable adjuvant is made through the special preparation process.The stripping of said preparation effective ingredient is fast, and directly through mucous membrane is absorbed into blood, and the bioavailability height is so have efficient, quick-acting and safe advantage.The main effective ingredient of bupleurum root dropping pills is saikoside and total volatile oil, and wherein the activity of saikoside A and D is stronger, therefore, the saikoside A in the bupleurum root dropping pills is carried out quantitative analysis, can be used as the conventional method of bupleurum root dropping pills quality testing.
The detection method of saikoside A commonly used has thin layer chromatography and high performance liquid chromatography (HPLC) at present.The thin layer chromatography accuracy is low, and poor repeatability requires height to operator, and pharmacopeia has substantially been eliminated this detection method.HPLC method accuracy and highly sensitive, good reproducibility, simple to operate.But because saikoside A content is lower, easily decomposition is improper as sample treatment in the bupleurum root dropping pills, can cause the difficulty of detection.
Summary of the invention
Technical problem to be solved
The invention provides the high-efficiency liquid chromatography method for detecting of the saikoside A in a kind of bupleurum root dropping pills, solved an important techniques problem in the bupleurum root dropping pills quality testing.
Technical scheme
The invention provides the high-efficiency liquid chromatography method for detecting of the saikoside A in a kind of bupleurum root dropping pills, comprise the preparation process and the determination step of need testing solution, wherein the preparation process of test sample comprises:
A) sample thief is an amount of;
B) dissolve with alkaline solution;
C) pass through macroporous adsorptive resins;
D) eluting;
E) collect the organic solvent eluent, be concentrated near doing;
F) dissolving.
The b of the preparation process of test sample wherein) the used preferred sodium hydroxide solution of alkaline solution, the preferred 0.3-0.6mol/L of the concentration of sodium hydroxide solution, most preferably 0.5mol/L;
The step that can also comprise supersound process the b of the preparation process of test sample wherein);
The c of the preparation process of test sample) preferably adopting macroporous adsorptive resins is AB-8 type macroporous adsorbent resin;
The e of the preparation process of test sample) preferably adopts concentrating under reduced pressure.
The used preferred octadecylsilane chemically bonded silica of filler of determination step wherein, the preferred acetonitrile-water of used mobile phase, ratio is 1: 1.5-2.0, used detection wavelength is 204-212nm, preferred 208nm.
Said method step and technical parameter are determined by a large amount of tests.
Beneficial effect
Adopt the saikoside A in the method detection bupleurum root dropping pills of the present invention, have good resolution, accuracy and highly sensitive, good reproducibility, simple to operate.In 2.5 μ g scopes, sample size and peak area are good linear relation (seeing accompanying drawing) to the sample size of saikoside A at 0.5 μ g.Response rate experiment shows that the average recovery rate of this method is 100.8%, and RSD is 1.9%.
Description of drawings
The preparation of standard curve and linear relationship are investigated
The specific embodiment
Below further specify the present invention with embodiment, but therefore do not limit the present invention in the specific embodiment scope.Embodiment 1
The assay of saikoside A in the bupleurum root dropping pills
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water (1: 1.8) is mobile phase; The detection wavelength is 208nm.Number of theoretical plate calculates with saikoside A peak should be not less than 6000.
The preparation of reference substance solution: it is an amount of to get saikoside A reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.3mg, promptly.
The preparation of need testing solution: get bupleurum root dropping pills (Tianjin Tasly Pharmaceutical Co., Ltd's preparation, lot number 20040408) 0.5g, the accurate title, decide, add 0.5mol/L sodium hydroxide solution 20ml, supersound process makes dissolving, by AB-8 macroporous adsorptive resins (60～100 orders, internal diameter 0.7cm, the high 5cm of post), it is colourless that the about 20ml of water is eluted to eluent, reuse dehydrated alcohol 20ml eluting is collected ethanol elution, is evaporated near doing, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, promptly.
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, to measure, saikoside A content is not less than 0.5mg.
Embodiment 2
The assay of saikoside A in the bupleurum root dropping pills
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water (1: 1.5) is mobile phase; The detection wavelength is 204nm.Number of theoretical plate calculates with saikoside A peak should be not less than 6000.
The preparation of reference substance solution: it is an amount of to get saikoside A reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.3mg, promptly.
The preparation of need testing solution: get bupleurum root dropping pills (Tianjin Tasly Pharmaceutical Co., Ltd's preparation, lot number 20040408) 0.5g, the accurate title, decide, add 0.3mol/L sodium hydroxide solution 20ml, by AB-8 macroporous adsorptive resins (60～100 orders, internal diameter 0.7cm, the high 5cm of post), it is colourless that the about 20ml of water is eluted to eluent, reuse dehydrated alcohol 20ml eluting, collect ethanol elution, be evaporated near doing, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, promptly.
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, to measure, saikoside A content is not less than 0.5mg.
Embodiment 3
The assay of saikosaponin A in the bupleurum root dropping pills
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water (1: 2.0) is mobile phase; The detection wavelength is 212nm.Number of theoretical plate calculates with saikoside A peak should be not less than 6000.
The preparation of reference substance solution: it is an amount of to get saikoside A reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 0.3mg, promptly.
The preparation of need testing solution: get bupleurum root dropping pills (Tianjin Tasly Pharmaceutical Co., Ltd's preparation, lot number 20040408) 0.5g, the accurate title, decide, add 0.6mol/L sodium hydroxide solution 20ml, supersound process makes dissolving, by AB-8 macroporous adsorptive resins (60～100 orders, internal diameter 0.7cm, the high 5cm of post), it is colourless that the about 20ml of water is eluted to eluent, reuse dehydrated alcohol 20ml eluting is collected ethanol elution, and the normal pressure rotary evaporation is concentrated near doing, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, promptly.
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, to measure, saikoside A content is not less than 0.5mg.
Embodiment 4
Recovery test
Get bupleurum root dropping pills (Tianjin Tasly Pharmaceutical Co., Ltd's preparation of known content, lot number 20040408) 5 part, every part of 0.25g, the accurate title, decide, accurate respectively adding concentration is the saikoside A reference substance solution 1.0ml of 0.2502mg/ml, presses the method operation of example 1, the need testing solution that preparation is used for determination of recovery rates, press the analysis of text chromatographic condition, calculate recovery rate.The results are shown in Table 1.Average recovery rate is 100.8%, and RSD is 1.9%.
Table 1: the response rate is investigated the result
| Sampling amount g | Content mg in the sample | Reference substance addition mg | Record total amount mg | The response rate |
| 0.2433 0.2437 0.2434 0.2420 0.2423 | 0.2637 0.2641 0.2638 0.2623 0.2626 | 0.2502 | 0.5164 0.5111 0.5225 0.5170 0.5111 | 101.0％ 98.7％ 103.4％ 101.8％ 99.3％ |
Claims (10)
1. the high-efficiency liquid chromatography method for detecting of the saikoside A in the bupleurum root dropping pills comprises the preparation process and the determination step of need testing solution, and wherein the preparation process of test sample comprises:
A) sample thief is an amount of;
B) dissolve with alkaline solution;
C) pass through macroporous adsorptive resins;
D) eluting;
E) collect the organic solvent eluent, be concentrated near doing;
F) dissolving.
2. according to the process of claim 1 wherein the b of preparation process of test sample) used alkaline solution is sodium hydroxide solution.
3. according to the method for claim 1 or 2, the b of the preparation process of test sample wherein) concentration of used alkaline solution is 0.3-0.6mol/L.
4. according to the method for claim 3, the b of the preparation process of test sample wherein) concentration of used alkaline solution is 0.5mol/L.
5. the step that also comprises supersound process according to the method for claim 1 or 2, the b of the preparation process of test sample wherein).
6. according to the method for claim 1 or 2, the c of the preparation process of test sample wherein) used macroporous adsorptive resins is an AB-8 type macroporous adsorbent resin.
7. according to the method for claim 1 or 2, the e of the preparation process of test sample wherein) used method for concentration is a concentrating under reduced pressure.
8. according to the method for claim 1 or 2, wherein the used filler of determination step is an octadecylsilane chemically bonded silica, and used mobile phase is acetonitrile-water, and used detection wavelength is 204-212nm.
9. according to the method for claim 8, wherein the ratio of acetonitrile and water is 1 in the used mobile phase of determination step: 1.5-2.0.
10. according to the method for claim 8, wherein the used detection wavelength of determination step is 208nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510015499 CN1951408A (en) | 2005-10-18 | 2005-10-18 | Method for detecting saikosaponin A in drop pills of Bupleurum root |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510015499 CN1951408A (en) | 2005-10-18 | 2005-10-18 | Method for detecting saikosaponin A in drop pills of Bupleurum root |
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| Publication Number | Publication Date |
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| CN1951408A true CN1951408A (en) | 2007-04-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510015499 Pending CN1951408A (en) | 2005-10-18 | 2005-10-18 | Method for detecting saikosaponin A in drop pills of Bupleurum root |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062071B (en) * | 2007-06-18 | 2011-08-31 | 石任兵 | Total saponins from radix bupleuri extract and the preparing method thereof |
| CN103364496A (en) * | 2012-04-09 | 2013-10-23 | 天士力制药集团股份有限公司 | Method for simultaneously measuring content of four types of saikoside in bupleurum extract |
-
2005
- 2005-10-18 CN CN 200510015499 patent/CN1951408A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062071B (en) * | 2007-06-18 | 2011-08-31 | 石任兵 | Total saponins from radix bupleuri extract and the preparing method thereof |
| CN103364496A (en) * | 2012-04-09 | 2013-10-23 | 天士力制药集团股份有限公司 | Method for simultaneously measuring content of four types of saikoside in bupleurum extract |
| CN103364496B (en) * | 2012-04-09 | 2016-07-06 | 天士力制药集团股份有限公司 | Measure the method for four kinds of saikoside content in Radix Bupleuri extractum simultaneously |
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