CN100392400C - Method for pre processing sample in use for measuring concentration of salvianolic acid B, in biologic body fluid - Google Patents
Method for pre processing sample in use for measuring concentration of salvianolic acid B, in biologic body fluid Download PDFInfo
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- CN100392400C CN100392400C CNB2005100309393A CN200510030939A CN100392400C CN 100392400 C CN100392400 C CN 100392400C CN B2005100309393 A CNB2005100309393 A CN B2005100309393A CN 200510030939 A CN200510030939 A CN 200510030939A CN 100392400 C CN100392400 C CN 100392400C
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- methyl alcohol
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Abstract
A method for pre-treating analysis sample of red phenolic acid B concentration in body fluid on living beings includes utilizing water- methanol to spray-wash then utilizing aqueous ammonia-methauol to elute Waters Oasis HLB small column obtained by activating sample containing red phenolic acid with water and methanil, enriching eluted liquid, using high efficiency of chromatography to carry out pretreatment on living beings sample containing red phenolic acid B after enriched matter is redissloved by flowing phase of 1% trifluoroacetic acid: methanol: acetonitrile.
Description
Technical field
The present invention relates to the pharmacokinetics research field of Chinese medicine, relate in particular to tanshin polyphenolic acid B and contain tanshin polyphenolic acid B concentration determination The pretreatment method in the pharmacokinetics research field, particularly biological fluid of tanshin polyphenolic acid B Chinese medicine.
Background technology
The red sage root is one of the most frequently used Chinese crude drug, and result of study shows that what work the effect of invigorating blood circulation addiction mainly is water soluble ingredient, and tanshin polyphenolic acid B is a kind of that content is the highest in the water soluble ingredient, the tired activity of invigorating blood circulation is the strongest.
Chinese Pharmacopoeia Commission is decided to be the quality control index of Radix Salviae Miltiorrhizae Tabellae in March, 2002 with tanshin polyphenolic acid B, and further, tanshin polyphenolic acid B may become the quality control index of red sage formulation.
Pharmacological research shows that tanshin polyphenolic acid B has treatment cardiovascular and cerebrovascular disease, hepatopathy and viral disease and tumour etc., is in the new drug development stage.
Up to the present, the relevant tanshin polyphenolic acid B body fluid example preprocess method that contains is studied rarely seen 1 piece of report, as hangJ, YuH, ShengY, et al.HPLC determination and pharmacokineticstudies of salvianolic acid B in rat plasma after oral administrationof Radix Salviae Miltiorrhizae extract.Biomed Chromatogr 2005; 19 (1): 15-8.But what adopt in this research is that traditional liquid-liquid extraction method is carried out sample pretreatment, it transfers to pH 2 with 10% hydrochloric acid with blood plasma earlier, with the cruel extraction of acetate second 3 times, make the sensitivity of method for measurement of concentration lower again, and the tanshin polyphenolic acid B pharmacokinetics rule of result of study reflection have inclined to one side face.Therefore, for the understanding deficiency of the pharmacokinetics rule in vivo of tanshin polyphenolic acid B in tanshin polyphenolic acid B and the red sage formulation, can't and instruct clinical rational drug use that foundation is provided for the tanshin polyphenolic acid B new drug development.
Because tanshin polyphenolic acid B is a water soluble ingredient, when concentration was low in the sample, traditional liquid-liquid extraction method was difficult to fully the tanshin polyphenolic acid B in the sample be extracted in addition.Therefore, the method that prior art adopts, the sensitivity of detection is low, the blood concentration in the time of can't detecting low concentration in pharmacokinetic.
Therefore, because the singularity of salvianolic acid B chemical character if the preprocess method that adopts is improper, can make the sensitivity deficiency of method for measurement of concentration.
Summary of the invention
Technical matters to be solved by this invention is: tanshin polyphenolic acid B concentration determination The pretreatment method in a kind of biological fluid is provided, after adopting new sample pretreating method, make in the biological fluid tanshin polyphenolic acid B method for measurement of concentration sensitive more, the pharmacokinetic that can be used for tanshin polyphenolic acid B helps to illustrate the pharmacokinetics rule of tanshin polyphenolic acid B comprehensively.
The technical matters that the present invention solves can be achieved through the following technical solutions.
Tanshin polyphenolic acid B concentration determination The pretreatment method in a kind of biological fluid, it is characterized in that: after will containing the adding 2.17mol/L of the biological sample elder generation phosphoric acid mixing of tanshin polyphenolic acid B concentration, add again with the Waters Oasis HLB pillar after the activation of first alcohol and water, behind drip washing and wash-out, eluent volatilizes enrichment, is that available high performance liquid chromatography detects after redissolving with moving phase; Wherein drip washing condition is: water and methyl alcohol, and elution requirement is: ammoniacal liquor methyl alcohol; First step water during drip washing, second step was used 80-100% methyl alcohol, and elution requirement is: 0.2-1% ammoniacal liquor methyl alcohol.
The present invention adopts the chromatographic condition of high performance liquid chromatography to be: analytical column is Thermo Hypersil-Keystone ODS Hypersil C
18Post, moving phase are 1% trifluoroacetic acid: methyl alcohol: second eyeball, flow velocity are 1mlmin
-1, column temperature is 30 ℃, the detection wavelength is 315nm.
The present invention adopts solid phase extraction techniques that the biological sample that contains tanshin polyphenolic acid B concentration is carried out pre-service, the biological sample of handling that contains tanshin polyphenolic acid B concentration, the biological sample that contains tanshin polyphenolic acid B concentration than existing method processing, low more than 300 times of the minimum quantitative limit of its tanshin polyphenolic acid B concentration, sensitivity obviously improves; Accuracy 103.7% of the present invention, withinday precision 12.6%, day to day precision 13.0% meet the requirement of biological sample analysis, can measure tanshin polyphenolic acid B concentration in the biological fluid delicately, are suitable for the tanshin polyphenolic acid B pharmacokinetic.
Following table is the comparison in the range of linearity and minimum quantitative limit of the present invention and above-mentioned document:
| Index | This law | Document |
| The range of linearity | 0.035-1.400μg/ml | 10.8-259.4μg/ml |
| Minimum quantitative limit | 0.035μg/ml | 10.8μg/ml |
Embodiment
Tanshin polyphenolic acid B concentration determination The pretreatment method in a kind of biological fluid, be that the volume ratio between biological sample and the phosphoric acid was: 1: 2-3 after the biological sample (comprising blood plasma, urine, tissue homogenate supernatant etc.) that will contain tanshin polyphenolic acid B concentration added 2.17mol/L phosphoric acid mixing earlier; Add again with the Waters oasis HLB pillar after the activation of first alcohol and water, behind drip washing and wash-out, eluent volatilizes enrichment under 25 ℃ of conditions, use 1% trifluoroacetic acid: methyl alcohol: (70: 10: 20, v: v: moving phase v) was that (chromatographic condition is: analytical column is Thermo Hypersil-Keystone ODSHyPersil C to available high performance liquid chromatography after redissolving to the second eyeball
18Post, moving phase are 1% trifluoroacetic acid: methyl alcohol: (70: 10: 20, v: v: v), flow velocity was 1mlmin to the second eyeball
-1, column temperature is 30 ℃, the detection wavelength is 315nm) detect; Wherein drip washing condition is: first step water, and second step was used 80-100% methyl alcohol, and elution requirement is: 0.2-1% ammoniacal liquor methyl alcohol.
Measurement result: typical curve: in tanshin polyphenolic acid B plasma concentration 0.035-1.400 μ g/ml scope, y=-2.5906+261.499x, r=0.9992, the minimum 0.035 μ g/ml that quantitatively is limited to.At tanshin polyphenolic acid B plasma concentration 0.035,0.140,1.400 μ g/ml, accuracy is respectively 106.70%; 95.3%, 109.1%, withinday precision 10.9%, 14.9%, 11.9%, day to day precision 9.8%, 14.7%, 14.5%.
Claims (3)
1. tanshin polyphenolic acid B concentration determination The pretreatment method in the biological fluid, it is characterized in that: after will containing the adding 2.17mol/L of the biological sample elder generation phosphoric acid mixing of tanshin polyphenolic acid B concentration, add again with the Waters Oasis HLB pillar after the activation of first alcohol and water, behind drip washing and wash-out, eluent volatilizes enrichment, is that available high performance liquid chromatography detects after redissolving with moving phase; Wherein drip washing condition is: water and methyl alcohol, and elution requirement is: ammoniacal liquor methyl alcohol; First step water during drip washing, second step was used 80-100% methyl alcohol, and elution requirement is: 0.2-1% ammoniacal liquor methyl alcohol.
2. tanshin polyphenolic acid B concentration determination The pretreatment method in the biological fluid according to claim 1, it is characterized in that: the volume ratio between biological sample and the phosphoric acid is: 1: 2-3.
3. tanshin polyphenolic acid B concentration determination The pretreatment method in the biological fluid according to claim 1, it is characterized in that: described moving phase is 1% trifluoroacetic acid: methyl alcohol: second eyeball, the volume ratio between the three are 70: 10: 20.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100309393A CN100392400C (en) | 2005-11-01 | 2005-11-01 | Method for pre processing sample in use for measuring concentration of salvianolic acid B, in biologic body fluid |
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| CNB2005100309393A CN100392400C (en) | 2005-11-01 | 2005-11-01 | Method for pre processing sample in use for measuring concentration of salvianolic acid B, in biologic body fluid |
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| CN1959409A CN1959409A (en) | 2007-05-09 |
| CN100392400C true CN100392400C (en) | 2008-06-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539220A (en) * | 2012-01-21 | 2012-07-04 | 华中农业大学 | Analysis method for metabolin of A-type proanthocyanidins |
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| CN101334386B (en) | 2007-04-27 | 2012-07-11 | 上海现代中医药股份有限公司 | Determination method for plant medicine blood plasma amygdalin for strengthening the body resistance |
| CN101042380A (en) | 2007-04-27 | 2007-09-26 | 上海现代中医药技术发展有限公司 | Method for measuring strengthen the body resistance and absorbing clots plant medicine plasma gamma-schizandrin |
| CN101078712A (en) | 2007-04-27 | 2007-11-28 | 上海现代中医药技术发展有限公司 | Method for determining plasma tanshinol and salvianolic acid B for strengthening body resistance and eliminating stasis |
| CN101045092A (en) | 2007-04-29 | 2007-10-03 | 上海现代中医药技术发展有限公司 | Application of plant medicine composition for strengthening the body resistance and resolving stagnate |
| CN106018636B (en) * | 2016-06-30 | 2018-08-24 | 中国水产科学研究院长江水产研究所 | A kind of kit, sample-pretreating method and dithiocyano-methane detection method |
| CN109939659A (en) * | 2019-04-22 | 2019-06-28 | 西北大学 | A kind of efficient hydrophobic interaction chromatograph medium, preparation method and its extracting the application in tanshin polyphenolic acid B |
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| CN1153778A (en) * | 1995-12-08 | 1997-07-09 | 中国医科大学 | Rosemary acid dimer compound and its separation process |
| CN1425659A (en) * | 2002-12-31 | 2003-06-25 | 南京虹桥医药技术研究所 | Process for preparing danshen salviandic acid |
| EP1371368A1 (en) * | 2002-06-11 | 2003-12-17 | N.V. Nutricia | Salvianolic acid components as lipase inhibitors |
| WO2003103614A2 (en) * | 2002-06-11 | 2003-12-18 | Carlo Ghisalberti | Method and compositions for the treatment of edematous-firbrsclerotic panniculopathy |
| US20050037094A1 (en) * | 2003-07-31 | 2005-02-17 | Xijun Yan | Composition for heart disease, its active ingredients, method to prepare same and uses thereof |
| CN1669573A (en) * | 2004-03-17 | 2005-09-21 | 天津天士力制药股份有限公司 | Chinese medicine preparation for treating cardiovascular and cerebrovascular diseases and preparing process thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1153778A (en) * | 1995-12-08 | 1997-07-09 | 中国医科大学 | Rosemary acid dimer compound and its separation process |
| EP1371368A1 (en) * | 2002-06-11 | 2003-12-17 | N.V. Nutricia | Salvianolic acid components as lipase inhibitors |
| WO2003103614A2 (en) * | 2002-06-11 | 2003-12-18 | Carlo Ghisalberti | Method and compositions for the treatment of edematous-firbrsclerotic panniculopathy |
| CN1425659A (en) * | 2002-12-31 | 2003-06-25 | 南京虹桥医药技术研究所 | Process for preparing danshen salviandic acid |
| US20050037094A1 (en) * | 2003-07-31 | 2005-02-17 | Xijun Yan | Composition for heart disease, its active ingredients, method to prepare same and uses thereof |
| CN1669573A (en) * | 2004-03-17 | 2005-09-21 | 天津天士力制药股份有限公司 | Chinese medicine preparation for treating cardiovascular and cerebrovascular diseases and preparing process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539220A (en) * | 2012-01-21 | 2012-07-04 | 华中农业大学 | Analysis method for metabolin of A-type proanthocyanidins |
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