CN102451206A - Quality control method of acanthopanax root and antler blood oral liquid - Google Patents
Quality control method of acanthopanax root and antler blood oral liquid Download PDFInfo
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- CN102451206A CN102451206A CN2010105929389A CN201010592938A CN102451206A CN 102451206 A CN102451206 A CN 102451206A CN 2010105929389 A CN2010105929389 A CN 2010105929389A CN 201010592938 A CN201010592938 A CN 201010592938A CN 102451206 A CN102451206 A CN 102451206A
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Abstract
The invention discloses a quality control method of an acanthopanax root and antler blood oral liquid. The quality control method comprises a method for measuring the content of isofraxidin and/or syringin. The acanthopanax root and antler blood oral liquid is composed of acanthopanax root, antler blood, antler, vitamin B1 and a plurality of adjuvants. The root and stem of the main raw material namely acanthopanax root contain multiple active chemical ingredients, and contain multiple saponin and alkaloids compounds until now; and the separated important ingredients are glycoside compounds, the main ingredient syringin is beta-sitosterol glycoside and is a typical glycoside compound, and the other main ingredient is isofraxidin the content of which in a medicine is relatively easy to measure. According to the invention, isofraxidin in acanthopanax root and antler blood is selected as a content measuring index, and the content of isofraxidin in the oral liquid is measured by adopting high-performance liquid chromatography; and at the same time, the syringin content is also measured. Therefore, the quality control method is simple and convenient, accurate, high in precision and good in repeatability, and provides a reliable basis for controlling the quality standard of the acanthopanax root and antler blood oral liquid.
Description
Technical field
The present invention relates to a kind of method of quality control of Chinese medicine, particularly the method for quality control of slender acanthopanax Sanguis cervi oral liquid.
Background technology
Slender acanthopanax Sanguis cervi oral liquid prescription is made up of Radix Et Caulis Acanthopanacis Senticosi, Sanguis Cornu Cervi Pantotrichum, Cornu Cervi Pantotrichum, vitamin B1 and several kinds of adjuvants.Have brain-strengthening and increase marrow, the strong waist of enriching blood, sleep improving and stomach strengthening, kidney-tonifying health-care, the merit of mind refreshing and rejuvenating.Be used for the empty anemia of body, sexual impotence renal cold, diseases such as neurasthenia.Primary raw material Radix Et Caulis Acanthopanacis Senticosi Radix Et Caulis Acanthopanacis Senticosi is the dry root and rhizome of Araliaceae Radix Et Caulis Acanthopanacis Senticosi Acanthopanax Senticosus (Puper.etMaxim) Harms; Mainly be distributed in the ground such as Heilungkiang, Jilin, Hebei, Shanxi, Ningxia, Shaanxi and Sichuan of China, also there are distribution and plantation in ground such as Korea, Far-east Area of Russia and Hokkaido, Japan.Radix Et Caulis Acanthopanacis Senticosi has the effect of replenishing QI to invigorate the spleen, tonifying the kidney for tranquilization, is mainly used in diseases such as deficiency of spleen-YANG and kidneyYANG, body void are weak, inappetence, soreness of waist and knee joint, insomnia and dreamful sleep.In addition; Pharmacological research to Radix Et Caulis Acanthopanacis Senticosi also shows both at home and abroad; But Radix Et Caulis Acanthopanacis Senticosi enhancing body nonspecific defense ability except that having immunomodulating, antitumor, defying age, Antiradiation injury and fatigue-resisting function, also can be treated diseases such as cardiovascular and cerebrovascular disease, diabetes, neurasthenia.The root of Radix Et Caulis Acanthopanacis Senticosi and stem portion contain the various active chemical constituent, up to the present, contain multiple Saponin class, alkaloid compound, and isolated important component is a glycosides compound.Syringoside is the cupreol glucoside, is a kind of comparatively typical glycosides compound.One of main component is an isofraxidin, and its content in medical material also relatively is prone to measure.The present invention is an index with the isofraxidin in the slender acanthopanax Sanguis cervi; Adopt HPLC; Measure the content in the oral liquid; Increase the assay to syringoside simultaneously, this method of quality control is easy, accurate, precision is high, favorable reproducibility, for control slender acanthopanax Sanguis cervi oral liquid quality standard provides reliable foundation.
Summary of the invention
The method of quality control of the open slender acanthopanax Sanguis cervi oral liquid of the object of the invention comprises the content assaying method to isofraxidin and/or syringoside.
The content assaying method of isofraxidin is following:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the isofraxidin reference substance, adds methanol and process the solution that contains 5-10 μ g among every 1ml, promptly gets; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10-30ml, supersound process 10-30 minute, adds chloroform extraction 1-4 time; Add chloroform 10-20ml, combined chloroform extracting solution, evaporate to dryness at every turn; Residue adds dissolve with methanol, and is transferred to the 25ml volumetric flask, adds methanol to scale; Shake up, filter with microporous filter membrane, both; Accurate respectively reference substance and the need testing solution drawn injects chromatograph of liquid, measures, and promptly gets.
The content assaying method of syringoside is following:
The preparation of reference substance solution: get the syringoside reference substance and add water in right amount and process the solution that every 1ml contains 10-20 μ g, both; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10-30ml, and supersound process 10-30 minute, add chloroform extraction 1-4 time, add chloroform 10-20ml at every turn, subsequent filtrate is got in the water intaking metafiltration, both; Precision is measured reference substance solution, need testing solution, negative control article solution respectively, injects chromatograph of liquid, measures, and promptly gets.
Optimal technical scheme of the present invention is following
The content assaying method of isofraxidin:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the isofraxidin reference substance, adds methanol and process the solution that contains 10 μ g among every 1ml, promptly gets; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10-30ml, supersound process 10-30 minute, adds chloroform extraction 1-4 time; Add chloroform 10-20ml at every turn, the combined chloroform extracting solution, evaporate to dryness, residue adds dissolve with methanol; And be transferred to the 25ml volumetric flask, and add methanol to scale, shake up; Filter with microporous filter membrane 0,45 μ m, both; Chromatographic column: the C18 post, mobile phase: acetonitrile: 0.1% phosphoric acid solution, volume ratio are 20-30: 70-80, flow velocity: 1.0ml min, detect wavelength 344nm; Column temperature: room temperature; Accurate respectively reference substance and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and promptly get.
The content assaying method of syringoside:
The preparation of reference substance solution: get the syringoside reference substance and add water in right amount and process the solution that every 1ml contains 20 μ g, both; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10ml, and supersound process 10 minutes adds chloroform extraction 1-4 time, adds chloroform 10-20ml at every turn, and subsequent filtrate is got in the water intaking metafiltration, both; Chromatographic column: the C18 post, mobile phase: acetonitrile: water, volume ratio are 5-10: 90-95, flow velocity: 1.0ml min, detect wavelength: 265n m; Column temperature: 30-40 ℃; Number of theoretical plate calculates by the syringoside peak should be not less than 4000; Precision is measured reference substance solution, need testing solution, each 10 μ l of negative control article solution respectively, injects chromatograph of liquid, measures, and promptly gets.
The present invention is to the content assaying method of pyridine of piperazine skin and/or syringoside; Not only can measure slender acanthopanax Sanguis cervi oral liquid formulation; Can be applied in simultaneously other dosage form of slender acanthopanax Sanguis cervi kind, for example: the dosage form of clinical practices such as tablet, granule, capsule, injection.
Isofraxidin content assaying method of the present invention is learned and is investigated; Utilize UV-2401PC type uv-spectrophotometric appearance,, under 200～400nm wavelength, carry out UV scanning the isofraxidin reference substance; The result has absorption maximum in the 342nm wavelength, therefore selects 342nm to detect wavelength.Make an experiment with 4 kinds of mobile phases, the result shows when mobile phase is acetonitrile-0.1% phosphoric acid solution (75: 25), best results, and post forces down, and the peak type is sharp-pointed, and is negative noiseless.Accurate sample (061201) the test liquid 10 μ l that draw repeat sample introduction 5 times, measure its peak area, the RSD=0.99% of isofraxidin peak area value, and result of the test shows that precision is good.Stability test is the result show, the sample test liquid of isofraxidin assay is good at the 8h internal stability.To same lot sample article (061201) preparation sample test liquid, record peak area value and calculate content, the RSD=0.84% of its isofraxidin peak area value; The RSD=0.85% of isofraxidin content, result of the test shows that the content assaying method repeatability is good.It is noiseless that the blank assay result is illustrated in the retention time place of tested composition isofraxidin.
Syringoside content assaying method of the present invention is learned and is investigated; Utilize UV-2401PC type uv-spectrophotometric appearance,, under 200～400nm wavelength, carry out UV scanning the syringoside reference substance; The result has absorption maximum in the 265nm wavelength, therefore selects 342nm to detect wavelength.Make an experiment with 4 kinds of mobile phases, the result shows when mobile phase is acetonitrile-water (9: 91), best results, and post forces down, and the peak type is sharp-pointed, and is negative noiseless.The accurate sample test liquid 10 μ l that draw repeat sample introduction 5 times, measure its peak area, the RSD=0.96% of syringoside peak area value, and result of the test shows that precision is good.Stability test is the result show, the sample test liquid of syringoside assay is good at the 8h internal stability.To same lot sample article preparation sample test liquid, record peak area value and calculate content, the RSD=0.80% of its syringoside peak area value; The RSD=0.77% of syringoside content, result of the test shows that the content assaying method repeatability is good.It is noiseless that the blank assay result is illustrated in the retention time place of tested composition syringoside.
Experimental example 1: the investigation of the range of linearity of isofraxidin
Instrument and reagent day island proper Tianjin LC-10Avp series of high efficiency chromatograph of liquid, the SPD-10Avp Ultraviolet Detector; The CLASS-VP data process machine; Reference substance isofraxidin (lot number: 0837-200203; Confession assay usefulness is provided by Nat'l Pharmaceutical & Biological Products Control Institute).Methanol, acetonitrile are chromatographically pure, and water is water for injection, and base is alarmmed reagent and is analytical pure.Slender acanthopanax Sanguis cervi oral liquid is provided by Changchun, Jilin Xin An pharmaceutcal corporation, Ltd
Chromatographic condition chromatographic column: KromasilC18 post (150mmx4.6mmID, 5 μ m); Mobile phase: acetonitrile-0.1% phosphoric acid solution (20: 80); Detect wavelength: 342nm; Column temperature: 30 ℃; Flow velocity 1.0ml.min; Sensitivity: 0.08AUFS.
Precision takes by weighing the about in right amount 10mg of isofraxidin reference substance, puts in the 100ml volumetric flask, adds dissolve with methanol and dilutes scale making; Shake up; Accurate again absorption 1ml puts in the 10ml volumetric flask, adds methanol and is diluted to scale, shakes up; Be made into every 1ml and contain the solution of 10 μ g, accurate isofraxidin (9.376 μ g.ml) reference substance solution 2,4,8,12,16, the 20 μ l that draw annotate appearance.The record chromatogram is measured its peak area, and the result sees table 1.And with peak area value (A) sample size (C) is returned, the standard curve equation.To sample size (C) mapping, get a straight line, A=3.31071e-007C, r=0.9997 with peak area value (A).The result shows that in 18.752～187.52 * 10-3 μ g scope, isofraxidin peak area value and sample size have good linear relationship.
Experimental example 2: the recovery test of isofraxidin
Precision is measured sample (061203) 25ml of known content, adds isofraxidin (25.52 μ g.ml) reference substance solution 0.85ml respectively, 1.03ml; 1.20ml by above-mentioned sample preparation methods and chromatographic condition; The preparation application of sample reclaims need testing solution and injects high performance liquid chromatograph, calculate recovery rate, and result of the test shows; The response rate is between 95%～100%, and application of sample reclaims good.
Specific embodiment is following
Embodiment 1 isofraxidin assay
The preparation of reference substance solution: it is an amount of that precision takes by weighing the isofraxidin reference substance, adds methanol and process the solution that contains 10 μ g among every 1ml, promptly gets.The preparation of need testing solution: precision is measured test sample 10ml, adds water 10ml, supersound process 10-30 minute, adds chloroform extraction 1-4 time; Add chloroform 10-20ml at every turn, the combined chloroform extracting solution, evaporate to dryness, residue adds dissolve with methanol; And be transferred to the 25ml volumetric flask, and add methanol to scale, shake up; Filter with microporous filter membrane 0,45 μ m, both; Chromatographic column: the C18 post, mobile phase: acetonitrile: 0.1% phosphoric acid solution, volume ratio are 20-30: 70-80, flow velocity: 1.0ml min, detect wavelength 344nm; Column temperature: room temperature; Accurate respectively reference substance and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and promptly get.
Algoscopy: accurate respectively isofraxidin (9.376 μ g.ml) reference substance solution and each 10 μ l of 10 lot sample article test liquids of drawing, measure by above-mentioned chromatographic condition.
Embodiment 2: the assay of isofraxidin
The preparation of reference substance solution: it is an amount of that precision takes by weighing the isofraxidin reference substance, adds methanol and process the solution that contains 10 μ g among every 1ml, promptly gets; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10ml, and supersound process 10 minutes adds chloroform extraction 1-4 time; Add chloroform 10-20ml at every turn, the combined chloroform extracting solution, evaporate to dryness, residue adds dissolve with methanol; And be transferred to the 25ml volumetric flask, and add methanol to scale, shake up; Filter with microporous filter membrane 0,45 μ m, both; Chromatographic column: C18 post (250mm * 4.6mm, 5 μ m), mobile phase: acetonitrile: 0.1% phosphoric acid solution, volume ratio are 25: 75, flow velocity: 1.0ml min, detect wavelength 344nm; Column temperature: room temperature; Accurate respectively reference substance and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and promptly get.
Embodiment 3: the assay of syringoside
The preparation of reference substance solution: get the syringoside reference substance and add water in right amount and process the solution that every 1ml contains 20 μ g, both; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10ml, and supersound process 10 minutes adds chloroform extraction 1-4 time, adds chloroform 10-20ml at every turn, and subsequent filtrate is got in the water intaking metafiltration, both; Chromatographic column: C18 post (250mm * 4.6mm, 5 μ m), mobile phase: acetonitrile: water, volume ratio are 9: 91, flow velocity: 1.0ml min, detect wavelength: 265nm; Column temperature: 40 ℃; Number of theoretical plate calculates by the syringoside peak should be not less than 4000; Precision is measured reference substance solution, need testing solution, each 10 μ l of negative control article solution respectively, injects chromatograph of liquid, measures, and promptly gets.
Claims (4)
1. the method for quality control of a slender acanthopanax Sanguis cervi oral liquid comprises the content assaying method to isofraxidin and/or syringoside, and wherein the content assaying method of isofraxidin is following:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the isofraxidin reference substance, adds methanol and process the solution that contains 5-10 μ g among every 1ml, promptly gets; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10-30ml, supersound process 10-30 minute, adds chloroform extraction 1-4 time; Add chloroform 10-20ml, combined chloroform extracting solution, evaporate to dryness at every turn; Residue adds dissolve with methanol, and is transferred to the 25ml volumetric flask, adds methanol to scale; Shake up, filter with microporous filter membrane, both; Accurate respectively reference substance and the need testing solution drawn injects chromatograph of liquid, measures, and promptly gets.
2. method of quality control as claimed in claim 1, wherein the content assaying method of syringoside is following:
The preparation of reference substance solution: get the syringoside reference substance and add water in right amount and process the solution that every 1ml contains 10-20 μ g, both; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10-30ml, and supersound process 10-30 minute, add chloroform extraction 1-4 time, add chloroform 10-20ml at every turn, subsequent filtrate is got in the water intaking metafiltration, both; Precision is measured reference substance solution, need testing solution, negative control article solution respectively, injects chromatograph of liquid, measures, and promptly gets.
3. method of quality control as claimed in claim 1, wherein the content assaying method of isofraxidin is following:
The preparation of reference substance solution: it is right that precision takes by weighing the isofraxidin reference substance, adds methanol to process the solution that contains 10 μ g among every 1ml, promptly gets; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10-30ml, supersound process 10-30 minute, adds chloroform extraction 1-4 time; Add chloroform 10-20ml at every turn, the combined chloroform extracting solution, evaporate to dryness, residue adds dissolve with methanol; And be transferred to the 25ml volumetric flask, and add methanol to scale, shake up; Filter with microporous filter membrane 0,45 μ m, both; Chromatographic column: the C18 post, mobile phase: acetonitrile: 0.1% phosphoric acid solution, volume ratio are 20-30: 70-80, flow velocity: 1.0ml min, detect wavelength 344nm; Column temperature: room temperature; Accurate respectively reference substance and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, and promptly get.
4. method of quality control as claimed in claim 2, wherein the content assaying method of syringoside is following:
The preparation of reference substance solution: get the syringoside reference substance and add water in right amount and process the solution that every 1ml contains 20 μ g, both; The preparation of need testing solution: precision is measured oral liquid 10ml, adds water 10ml, and supersound process 10 minutes adds chloroform extraction 1-4 time, adds chloroform 10-20ml at every turn, and subsequent filtrate is got in the water intaking metafiltration, both; Chromatographic column: the C18 post, mobile phase: acetonitrile: water, volume ratio are 5-10: 90-95, flow velocity: 1.0ml min, detect wavelength: 265nm; Column temperature: 30-40 ℃; Number of theoretical plate calculates by the syringoside peak should be not less than 4000; Precision is measured reference substance solution, need testing solution, each 10 μ l of negative control article solution respectively, injects chromatograph of liquid, measures, and promptly gets.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053706A (en) * | 2016-06-24 | 2016-10-26 | 广西灵峰药业有限公司 | Production quality control method of three-snake-gall fritillariae cirrhosae bulbus syrup |
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2010
- 2010-12-17 CN CN2010105929389A patent/CN102451206A/en active Pending
Non-Patent Citations (2)
| Title |
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| 李春实等: "五加参归芪精质量标准研究", 《中国现代中药》 * |
| 金光日、洪海: "高效液相色谱法测定五加茸血口服液中异嗪皮啶的含量", 《长春中医药大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106053706A (en) * | 2016-06-24 | 2016-10-26 | 广西灵峰药业有限公司 | Production quality control method of three-snake-gall fritillariae cirrhosae bulbus syrup |
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Application publication date: 20120516 |