CN1847843A - Method of measuring ginsenoside Rb1 content in Chinese medicine - Google Patents
Method of measuring ginsenoside Rb1 content in Chinese medicine Download PDFInfo
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- CN1847843A CN1847843A CN 200510013275 CN200510013275A CN1847843A CN 1847843 A CN1847843 A CN 1847843A CN 200510013275 CN200510013275 CN 200510013275 CN 200510013275 A CN200510013275 A CN 200510013275A CN 1847843 A CN1847843 A CN 1847843A
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- 238000000034 method Methods 0.000 title claims abstract description 31
- UFNDONGOJKNAES-UHFFFAOYSA-N Ginsenoside Rb1 Natural products CC(=CCCC(C)(OC1OC(COC2OC(CO)C(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CC(O)C45C)C UFNDONGOJKNAES-UHFFFAOYSA-N 0.000 title claims abstract description 24
- GZYPWOGIYAIIPV-JBDTYSNRSA-N ginsenoside Rb1 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GZYPWOGIYAIIPV-JBDTYSNRSA-N 0.000 title claims abstract description 24
- TXEWRVNOAJOINC-UHFFFAOYSA-N ginsenoside Rb2 Natural products CC(=CCCC(OC1OC(COC2OCC(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CCC45C)C TXEWRVNOAJOINC-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000003814 drug Substances 0.000 title claims abstract description 23
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000000741 silica gel Substances 0.000 claims abstract description 5
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 120
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000945 filler Substances 0.000 claims description 27
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- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 20
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- 238000012360 testing method Methods 0.000 claims description 15
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 11
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- 241000208340 Araliaceae Species 0.000 claims description 9
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 8
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 8
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- 238000002360 preparation method Methods 0.000 claims description 7
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- IAWPVNMEXASPFO-UHFFFAOYSA-N C(CCCCCCCCCCCCCCCCC)[SiH3].[C] Chemical compound C(CCCCCCCCCCCCCCCCC)[SiH3].[C] IAWPVNMEXASPFO-UHFFFAOYSA-N 0.000 claims description 4
- 230000005526 G1 to G0 transition Effects 0.000 claims description 4
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- 238000000638 solvent extraction Methods 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
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- 241000083547 Columella Species 0.000 abstract 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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Abstract
The method of measuring ginsenoside Rb1 content in Chinese medicine includes extracting the Chinese medicine sample with solvent to obtain sample liquid, treating the sample liquid by means of solid extracting technology to obtain sample solution, and high efficiency liquid chromatography detecting, with the stuffing for solid extracting columella being octodecyl bonded silica gel stuffing. The present invention has less impurity influence, excellent separation between the ginsenoside Rb1 peak and adjacent peaks, and accurate determination of ginsenoside Rb1 content.
Description
Technical field
The present invention relates to content of effective assay method in the Chinese medicine, relate in particular to the content assaying method of ginsenoside Rb1 in the Chinese medicine.
Background technology
Except that adopting thin layer scanning method and micella kapillary electrokinetic chromatography method, adopt high performance liquid chromatography for the assay of ginsenoside Rb1 in Chinese crude drug, Chinese medical extract and the preparation more.In high performance liquid chromatography, adopt ODS (carbon octadecyl silane) stationary phase, acetonitrile-water system more.Such efficient liquid-phase chromatography method for the single medicinal material that contains less composition, can accurately be measured the ginsenoside Rb that wherein contains
1,, also often can be with the accurate ginsenoside Rb that measures wherein of this method for the prescriptions of traditional Chinese medicine preparation that contains less flavour of a drug
1But, when containing more flavour of a drug in the Chinese medicine prescription, contain numerous composition in its Chinese medicine preparation, when adopting above-mentioned high performance liquid chromatography, often there is other composition to disturb ginsenoside Rb
1Mensuration, make ginsenoside Rb
1Chromatographic peak and the chromatographic peak of adjacent impurity can not realize baseline separation, can not accurately measure ginsenoside Rb
1Content.In order to solve the ginsenoside Rb in the Chinese medicine compound prescription
1The assay problem, must in the pre-treatment process, seek technical breakthrough, the impurity that influences efficient liquid phase chromatographic analysis is removed as much as possible.
(Solid phase extraction, SPE) technology is a physical extraction technology that comprises liquid phase and solid phase to Solid-Phase Extraction.In Solid-Phase Extraction, solid phase is bigger than the solvent of separated and dissolved thing to the absorption affinity of separator.When sample solution passed through adsorbent bed, separator was concentrated in its surface, and other sample composition passes through adsorbent bed.The adsorbent that does not adsorb other sample composition by an adsorptive separation thing, the separator that can obtain high-purity and concentrate.
The present invention unites use with SPE pretreatment technology and high-efficient liquid phase chromatogram technology, has successfully got rid of in the complex system numerous impurity to ginsenoside Rb
1The interference of assay, the Chinese medicine compound prescription ginsenoside Rb that can accurately measure
1Content.
Summary of the invention
The objective of the invention is for the content assaying method of ginsenoside Rb1 in a kind of Chinese medicine compound prescription is provided.
The present invention is implemented by following scheme: with solvent extraction Chinese medicine sample, the gained sample liquid is handled with solid phase extraction techniques earlier, and the gained need testing solution carries out high-performance liquid chromatogram determination again.Sample extraction can heat or ultrasonic Extraction with methyl alcohol or ethanol, and extract filters, and filtrate waiting done further processing; The condition of high-performance liquid chromatogram determination can adopt carbon octadecyl silane stationary phase, acetonitrile-phosphate aqueous solution system flow phase.
Described sample liquid is handled with solid phase extraction techniques, sample liquid suitably can be concentrated or evaporate to dryness, residue is with methyl alcohol or dissolve with ethanol, on the solid phase extraction column handled well, with 10～50% methyl alcohol or alcohol flushing, at last with methyl alcohol or ethanol elution, collect eluent, constant volume shakes up, and promptly gets need testing solution.Perhaps sample liquid is suitably concentrated or evaporate to dryness, residue is with 0.1%～5% ammonia solvent, on the solid phase extraction column handled well, with the flushing of 0.1%～5% ammoniacal liquor, use 10～50% methyl alcohol or alcohol flushing again, earlier at last with methyl alcohol or ethanol elution, collect eluent, constant volume shakes up, and promptly gets need testing solution.
The disposal route of described solid phase extraction column places in internal diameter 0.5～3cm glass pillar for taking by weighing 30～400 order solid phase extraction fillers, 0.2～5g, adds methyl alcohol or ethanol 5～50mL flushing, and is standby; Perhaps, with 0.1%～5% ammoniacal liquor, 5～50mL flushing, standby again with after methyl alcohol or the ethanol 5～50mL flushing.
The filler of described solid phase extraction column can be graphitic carbon reverse phase filler, ion exchange resin filler, metal complex adsorbent filler, bonded silica gel filler, polymer absorbant filler, immune affinity sorbent filler, molecule embedded polymer thing filler.Preferred bonded silica gel SPE filler.Bonded silica gel SPE filler can be octadecyl silane (ODS) filler or other alkyl linked silica filler; Preferred octadecyl silane SPE filler.
Adopt the present invention to after carrying out the SPE technical finesse for test agent, the impurity that influences ginsenoside Rb1's assay is removed, and the ginsenoside Rb1 peak is better separated with adjacent peak, and peak area is truer, and assay is more accurate.Do not use the ginsenoside Rb1 and the adjacent separate impurities degree of chromatogram of SPE technology gained sample poor, do not reach fully and separate, integration is inaccurate, and the ginsenoside Rb1's peak area that causes recording departs from actual value, causes the result inaccurate.
Description of drawings
Fig. 1: the HPLC chromatogram that uses SPE technical finesse sample.
Fig. 2: the HPLC chromatogram that does not use SPE technical finesse sample.
Fig. 3: the HPLC chromatogram of ginsenoside Rb1's reference substance.
Embodiment
Enumerate embodiment below and further describe the present invention, this embodiment only is used to the present invention is described and the present invention is not limited.
Embodiment one and Comparative Examples
The Chinese medicine preparation of the complicated component that comfortable of three ginsengs are made by American Ginseng, kuh-seng, the red sage root, cassia twig etc. 7 flavor Chinese medicines, wherein monarch drug in a prescription in American Ginseng be the side in common high-efficient liquid phase analysis, is difficult to obtain the good chromatogram of degree of separation, is difficult to accurate quantitative.Chromatography can not accurately be measured ginsenoside Rb wherein
1Adopt method of the present invention that the material of most of interference measurement is effectively removed, improved the accuracy of measuring.
1, instrument, medicine and reagent
Agilent 1100 type high performance liquid chromatographs, configuration quaternary pump, online vacuum degassing machine, diode array detector, column oven.(a day drug research institute of Shi Li group provides specification: 0.5g) to comfortable of three ginsengs.Ginsenoside Rb1's reference substance is purchased in Nat'l Pharmaceutical ﹠ Biological Products Control Institute (lot number: 110704-200217, assay is used).Methyl alcohol (analyze pure, Tianjin chemical reagent two factories), phosphoric acid (analyze pure, Shanghai chemical reagents corporation of Chinese Medicine group), acetonitrile (chromatographically pure, Merck company), purified water.
2, chromatographic condition
Chromatographic column is Agilent Zorbax SB-C
18(250mm * 4.6mm, 5 μ m), column temperature 40.℃。With acetonitrile-0.1% phosphate aqueous solution (28: 72) is moving phase, and flow velocity is 1.0mLmin-1, and the detection wavelength is 203nm.
3, the preparation of solution
(1) reference substance solution: it is an amount of to get ginsenoside Rb1's reference substance, and weight decided in accurate title is 19.33mg, uses dissolve with methanol, is settled to 25mL, and making concentration is ginsenoside Rb1's reference substance solution of 0.773mgmL-1.
(2)-1 the need testing solution of embodiment one: get comfortable of three ginsengs, porphyrize; Get the about 1g of sheet powder, accurate title is fixed, puts in the 100mL flask, the accurate methyl alcohol 50mL that adds, and weight decided in accurate title; Heating and refluxing extraction 1.5h is put coldly, and accurate again the title decide weight, supplies the weight that subtracts mistake with methyl alcohol, shakes up filtration.Precision is measured subsequent filtrate 25mL, water bath method.Residue is with 1% ammoniacal liquor (get liquor ammoniae fortis 44mL, adding distil water is to 1000mL) dissolving, on the ODS pillar handled well (take by weighing 50～100 order ODS filler 1.5g, place in the internal diameter 1cm glass pillar, add methyl alcohol 20mL flushing, wash with 1% ammoniacal liquor 20mL again, standby), the flow velocity of sample and elution process is not more than 0.7mLmin-1 in the control, washes with 1% ammoniacal liquor 10mL, wash with 30% methyl alcohol 10mL again, use the 10mL washed with methanol at last, collect methanol solution, be settled to 10mL, shake up, promptly.
(2)-2 Comparative Examples need testing solution: get three the ginseng comfortable, porphyrize; Get the about 1g of sheet powder, accurate title is fixed, puts in the 100mL flask, the accurate methyl alcohol 50mL that adds, and weight decided in accurate title; Heating and refluxing extraction 1.5h is put coldly, and accurate again the title decide weight, supplies the weight that subtracts mistake with methyl alcohol, shakes up filtration.Precision is measured subsequent filtrate 25mL, suitably concentrates, and is settled to 10mL with methanol solution, shakes up, promptly.
4, measure
Draw each 15 μ L of reference substance solution and need testing solution respectively, inject high performance liquid chromatograph, measure, promptly.
5, result
The peak area and the degree of separation of comfortable middle ginsenoside Rb1's assay of table 1 three ginsengs
| Batch | Peak area | Degree of separation | ||
| Use SPE | Do not use SPE | Use SPE | Do not use SPE | |
| 041028 041101 | 777.3 781.6 | 957.7 972.7 | 3.4 5.7 | 0.9 0.7 |
| 041103 041105 041109 041112 041121 041204 041215 | 793.8 795.0 806.8 822.2 833.8 839.9 888.0 | 973.4 991.5 1008.3 1043.0 1046.2 1061.2 1070.7 | 5.6 5.6 5.5 6.0 4.2 5.4 5.5 | 0.7 1.0 1.0 0.5 1.1 0.7 0.8 |
Can find out from table, behind the use SPE technical finesse articles for use, the impurity that influences ginsenoside Rb1's assay is removed, and the ginsenoside Rb1 peak is better separated (see figure 1) with adjacent peak, and peak area is truer, and assay is more accurate.Do not use the ginsenoside Rb1 and the adjacent separate impurities degree difference (see figure 2) of the chromatogram of SPE technology gained sample, do not reach fully and separate, integration is inaccurate, and the ginsenoside Rb1's peak area that causes recording departs from actual value, causes the result inaccurate.
Embodiment two
The preparation of need testing solution: get comfortable of three ginsengs, porphyrize; Get the about 1g of sheet powder, accurate title is fixed, puts in the 100mL flask, the accurate methyl alcohol 50mL that adds, and weight decided in accurate title; Ultrasonic Extraction 0.5h is put coldly, and accurate again the title decide weight, supplies the weight that subtracts mistake with methyl alcohol, shakes up filtration.Precision is measured subsequent filtrate 25mL, on macroreticular weakly base styrene anion exchange resins (D8590) pillar handled well (take by weighing 50～100 order D8590 filler 1.5g, place in the internal diameter 1cm glass pillar, add methyl alcohol 20mL flushing,, wash with 1% ammoniacal liquor 20mL again, standby), the flow velocity of sample and elution process is not more than 0.7mLmin-1 in the control, with the 20mL washed with methanol, collects methanol solution, suitably concentrate, be settled to 10mL, shake up, promptly.
Other is all with embodiment one
The result: the degree of separation of ginsenoside Rb1 peak and adjacent peak is greater than 3.0.
Claims (10)
1. ginsenoside Rb1's content assaying method in the Chinese medicine compound prescription, comprise and use earlier the solvent extraction sample, the gained sample liquid is handled with solid phase extraction techniques, the gained need testing solution carries out high-performance liquid chromatogram determination again, it is characterized in that, described sample liquid is treated to solid phase extraction techniques sample liquid is suitably concentrated or evaporate to dryness, residue is with methyl alcohol or dissolve with ethanol, on the solid phase extraction column handled well, with 10～50% methyl alcohol or alcohol flushing, at last with methyl alcohol or ethanol elution, collect eluent, constant volume shakes up, and promptly gets need testing solution.
2. content assaying method according to claim 1, it is characterized in that described sample liquid is treated to solid phase extraction techniques sample liquid is suitably concentrated or evaporate to dryness, residue is with 0.1%～5% ammonia solvent, on the solid phase extraction column handled well, with the flushing of 0.1%～5% ammoniacal liquor, use 10～50% methyl alcohol or alcohol flushing again, earlier at last with methyl alcohol or ethanol elution, collect eluent, constant volume shakes up, and promptly gets need testing solution.
3. content assaying method according to claim 1 and 2 is characterized in that, described is to get Chinese medicine preparation 0.2～2g to be measured with the solvent extraction sample earlier, adds methyl alcohol or ethanol, heating or ultrasonic Extraction, and extract filters, and filtrate waiting done further processing.
4. content assaying method according to claim 1 and 2 is characterized in that, the condition of described high-performance liquid chromatogram determination adopts carbon octadecyl silane stationary phase, acetonitrile-phosphate aqueous solution system flow phase.
5. content assaying method according to claim 1 and 2, it is characterized in that the disposal route of described solid phase extraction column places in internal diameter 0.5～3cm glass pillar for taking by weighing 30～400 order solid phase extraction fillers, 0.2～5g, add methyl alcohol or ethanol 5～50mL flushing, standby; Perhaps, with 0.1%～5% ammoniacal liquor, 5～50mL flushing, standby again with after methyl alcohol or the ethanol 5～50mL flushing.
6. content assaying method according to claim 1 and 2, it is characterized in that the filler of described solid phase extraction column can be graphitic carbon reverse phase filler, ion exchange resin filler, metal complex adsorbent filler, bonded silica gel filler, polymer absorbant filler, immune affinity sorbent filler, molecule embedded polymer thing filler.
7. content assaying method according to claim 6 is characterized in that, the filler of described solid phase extraction column is the octadecyl silane filler.
8. content assaying method according to claim 1 and 2 is characterized in that, described sample is comfortable of three ginsengs.
9. content assaying method according to claim 8 is characterized in that, gets comfortable 0.2～2g of three ginsengs, adds methyl alcohol or ethanol, heating or ultrasonic Extraction, and extract filters; Filtrate evaporate to dryness, residue be with 0.1%～5% ammonia solvent, on the solid phase extraction column handled well, wash with 0.1%～5% ammoniacal liquor earlier, use 10～50% methyl alcohol or alcohol flushing again,, collect eluent at last with methyl alcohol or ethanol elution, constant volume shakes up, and promptly gets need testing solution; Get ginsenoside Rb1's reference substance and be mixed with reference substance solution; It is moving phase that high-efficient liquid phase chromatogram condition adopts carbon octadecyl silane stationary phase, acetonitrile-phosphate aqueous solution system; Need testing solution and reference substance solution are injected high performance liquid chromatograph respectively, measure, promptly.
10. content assaying method according to claim 9 is characterized in that, described need testing solution is prepared as gets comfortable 0.2～2g of three ginsengs, and accurate title is fixed, puts in the flask, the accurate methyl alcohol 5～100mL that adds, and weight decided in accurate title; Heating or ultrasonic Extraction 0.2～2.5h are put coldly, and accurate again the title decide weight, supplies the weight that subtracts mistake with methyl alcohol or ethanol, shakes up filtration; Precision is measured subsequent filtrate 5～50mL, water bath method; Residue is with 0.1%～5% ammonia solvent, on the octadecyl silane pillar handled well, the flow velocity of sample and elution process is in 0.3～2mLmin-1 scope in the control, with 0.1%～5% ammoniacal liquor, 2～30mL flushing, with 10～50% methyl alcohol or ethanol 10mL flushing, use 10mL methyl alcohol or alcohol flushing at last again, collect methyl alcohol or ethanol liquid, be settled to 10mL, shake up, promptly get need testing solution.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102058645A (en) * | 2009-11-17 | 2011-05-18 | 天津天士力制药股份有限公司 | Ginseng glycoside H extractive and preparation method thereof |
| CN102166512A (en) * | 2011-03-03 | 2011-08-31 | 刘庆山 | Ginsenoside Rg1 molecular imprinting material and preparation method and application thereof |
| CN105651925A (en) * | 2016-04-15 | 2016-06-08 | 广西壮族自治区梧州食品药品检验所 | Determination method of ginsenosides Rg1 and Re in ginseng leaves |
| CN105738537A (en) * | 2016-04-22 | 2016-07-06 | 广西壮族自治区梧州食品药品检验所 | Analyzing method for ginsenoside in ginseng leaves |
| CN105929088A (en) * | 2016-04-22 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Extraction method for ginsenoside in ginseng leaf |
| CN112014489A (en) * | 2019-05-31 | 2020-12-01 | 中国科学院大连化学物理研究所 | Method for enriching protopanaxadiol type saponin and analyzing protopanaxadiol type saponin by high performance liquid chromatography |
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2005
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Cited By (8)
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| CN102058645A (en) * | 2009-11-17 | 2011-05-18 | 天津天士力制药股份有限公司 | Ginseng glycoside H extractive and preparation method thereof |
| CN102058645B (en) * | 2009-11-17 | 2013-09-11 | 天士力制药集团股份有限公司 | Ginseng glycoside H extractive and preparation method thereof |
| CN102166512A (en) * | 2011-03-03 | 2011-08-31 | 刘庆山 | Ginsenoside Rg1 molecular imprinting material and preparation method and application thereof |
| CN102166512B (en) * | 2011-03-03 | 2012-10-31 | 刘庆山 | Ginsenoside Rg1 molecular imprinting material and application thereof |
| CN105651925A (en) * | 2016-04-15 | 2016-06-08 | 广西壮族自治区梧州食品药品检验所 | Determination method of ginsenosides Rg1 and Re in ginseng leaves |
| CN105738537A (en) * | 2016-04-22 | 2016-07-06 | 广西壮族自治区梧州食品药品检验所 | Analyzing method for ginsenoside in ginseng leaves |
| CN105929088A (en) * | 2016-04-22 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Extraction method for ginsenoside in ginseng leaf |
| CN112014489A (en) * | 2019-05-31 | 2020-12-01 | 中国科学院大连化学物理研究所 | Method for enriching protopanaxadiol type saponin and analyzing protopanaxadiol type saponin by high performance liquid chromatography |
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| CN1847843B (en) | 2012-10-10 |
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