CN109596746A - A kind of application of new content assaying method in the control of Radix Bupleuri quality - Google Patents
A kind of application of new content assaying method in the control of Radix Bupleuri quality Download PDFInfo
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- CN109596746A CN109596746A CN201811618130.6A CN201811618130A CN109596746A CN 109596746 A CN109596746 A CN 109596746A CN 201811618130 A CN201811618130 A CN 201811618130A CN 109596746 A CN109596746 A CN 109596746A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The present invention relates to the analysis technical fields of effective component in Chinese medicine, and in particular to application of the new content assaying method of one kind in the control of Radix Bupleuri quality；The content assaying method of the new saikosaponin a of one kind provided by the invention realizes the separation of saikosaponin a structural material similar to its, sensitivity with higher and specificity, easy to operate, and separating degree meets States Pharmacopoeia specifications (i.e. separating degree is greater than 1.5)；The quality control that can be used for Radix Bupleuri, medicine materical crude slice, extract powder, granule, has realistic meaning.
Description
Technical field
The present invention relates to the analysis technical fields of effective component in Chinese medicine, and in particular to the new content assaying method of one kind exists
Application in the control of Radix Bupleuri quality.
Background technique
Saikosaponin a is crystalline powder, soluble easily in water, dilute alcohol, especially hot water and hot alcohol, is dissolved in butanol and amylalcohol
Property it is big, indissoluble or do not dissolve in benzene, ether, chloroform equal solvent.
It is widely used in treating cold, fever saikosaponin a, and fevers and chills alternate, distending pain in the chest and hypochondrium, irregular menstruation, uterus takes off
It hangs down, the diseases such as rectal prolapse.There are antitumor (EAC), anti-liver malicious (big white mouse, the hepatotoxin as caused by CCl4), antiviral (prevalence
Property common cold virus A2invitro, 50 μ g/ml, inhibiting rate 69%), lipidemia, anti-endotoxin effect；With immunological regulation function
The effect of energy, there are also the anti-platelet activity factors, anti-allergic effects, anti-cellular adhesion effect.
However, the measurement for saikosaponin a content in medicinal material especially Chinese patent drug at present, is deposited at the extraction by similar knot
The interference of structure substance leads to the defects of chromatographic peak separation is difficult, detection accuracy is not high.It would therefore be highly desirable to develop a kind of step letter
Just, saikosaponin a content assaying method with high accuracy.
Based on this, the present invention provides a kind of application of new content assaying method in the control of Radix Bupleuri quality.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of new content assaying methods controls in Radix Bupleuri quality
In application, to solve the problems mentioned in the above background technology.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of application of new content assaying method in the control of Radix Bupleuri quality, includes the following steps:
(1) reference substance solution is prepared:
Standard items saikosaponin a is taken, using methanol as solvent, prepares standard solution；
(2) test solution is prepared:
Sample to be tested is taken, it is accurately weighed, it sets in stuffed conical flask, methanol solution 25ml of the addition containing strong ammonia solution, close plug,
30 DEG C of water temperatures are ultrasonically treated (power 900W, frequency 60kHz) 30 minutes, filtration, with methanol 20ml points of 2 washing containers and medicines
Slag, washing lotion merge with filtrate, and for recycling design to doing, residue adds methanol to dissolve, and is transferred in 5ml measuring bottle, adds methanol to scale, shakes
It is even, it is filtered with 0.22 μm of organic filter membrane, taking subsequent filtrate to get concentration is 0.04g/ml test solution；
(3) chromatographic condition:
Chromatographic column: Shiseido CAPCELLPAKADME chromatographic column (4.6mm × 250mm × 5 μm), Shimadzu
ODS-3 chromatographic column (4.6mm × 250mm × 5 μm) or Agilent ZORBAXEclipsePlusC18 chromatographic column (4.6mm × 250mm
×5μm)；Chromatographic column temperature: 30 DEG C；Flow rate of mobile phase: 1.0ml/min；Detection wavelength: 210nm；Detector: UV detector or
Diode array detector；20 μ L of sample volume；Flow phase composition: A phase is acetonitrile, B Xiang Weishui；Eluent gradient elution, flowing
Phase gradient elution program is as follows:
| T(min) | 0→40 | 40→50 | 50→55 |
| A phase (%) | 30→43 | 43→90 | 90 |
| B phase (%) | 70→57 | 57→10 | 10 |
(4) characteristic spectrum is established:
Reference substance solution and each 20 μ l of test solution respectively inject high performance liquid chromatograph, measure to get characteristic pattern
Spectrum.
Preferably, the sample to be tested for preparing in test solution is Bupleurum Chinese medicinal material, medicine materical crude slice, bupleurum extract or contains
The Chinese patent drug of saikosaponin a.
Preferably, the sampling amount of the sample to be tested is 0.1-0.6g.
It is preferably, described that prepare test solution be dense amine test solution content is 5%.
Preferably, the detection method in the characteristic spectrum foundation is reversed-phased high performace liquid chromatographic.
Preferably, the standard items saikosaponin a positions saikosaponin a chromatographic peak in product to be tested, described to be measured
Saikosaponin a chromatographic peak and adjacent chromatographic peak separating degree > 1.5 in sample.
The utility model has the advantages that
The content assaying method of the new saikosaponin a of one kind provided by the invention realizes saikosaponin a knot similar to its
The separation of structure substance, sensitivity with higher and specificity, easy to operate, separating degree meets States Pharmacopoeia specifications, and (i.e. separating degree is big
In 1.5).The quality control that can be used for Radix Bupleuri, medicine materical crude slice, extract powder, granule, has realistic meaning.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will be described below to embodiment required
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is liquid chromatogram in embodiment 2；
Fig. 2 is liquid chromatogram in embodiment 3；
Fig. 3 is liquid chromatogram in embodiment 4；
Fig. 4 is liquid chromatogram in embodiment 5；
Fig. 5 is liquid chromatogram in embodiment 6；
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of application of new content assaying method in the control of Radix Bupleuri quality, includes the following steps:
(1) reference substance solution is prepared:
Standard items saikosaponin a is taken, using methanol as solvent, prepares standard solution；
(2) test solution is prepared:
Sample to be tested is taken, it is accurately weighed, it sets in stuffed conical flask, methanol solution 25ml of the addition containing strong ammonia solution, close plug,
30 DEG C of water temperatures are ultrasonically treated (power 900W, frequency 60kHz) 30 minutes, filtration, with methanol 20ml points of 2 washing containers and medicines
Slag, washing lotion merge with filtrate, and for recycling design to doing, residue adds methanol to dissolve, and is transferred in 5ml measuring bottle, adds methanol to scale, shakes
It is even, it is filtered with 0.22 μm of organic filter membrane, taking subsequent filtrate to get concentration is 0.04g/ml test solution；
(3) chromatographic condition:
Chromatographic column: Shiseido CAPCELLPAKADME chromatographic column (4.6mm × 250mm × 5 μm), Shimadzu
ODS-3 chromatographic column (4.6mm × 250mm × 5 μm) or Agilent ZORBAXEclipsePlusC18 chromatographic column (4.6mm × 250mm
×5μm)；Chromatographic column temperature: 30 DEG C；Flow rate of mobile phase: 1.0ml/min；Detection wavelength: 210nm；Detector: UV detector or
Diode array detector；20 μ L of sample volume；Flow phase composition: A phase is acetonitrile, B Xiang Weishui；Eluent gradient elution, flowing
Phase gradient elution program is as follows:
| T(min) | 0→40 | 40→50 | 50→55 |
| A phase (%) | 30→43 | 43→90 | 90 |
| B phase (%) | 70→57 | 57→10 | 10 |
(4) characteristic spectrum is established:
Reference substance solution and each 20 μ l of test solution respectively inject high performance liquid chromatograph, measure to get characteristic pattern
Spectrum.
Preparing in test solution sample to be tested is Bupleurum Chinese medicinal material, medicine materical crude slice, bupleurum extract or containing saikosaponin a
Chinese patent drug.
The sampling amount that sample to be tested chooses Radix Bupleuri, medicine materical crude slice takes is 0.5g, and sample to be tested is chosen bupleurum extract or contained
The sampling amount for having the Chinese patent drug of saikosaponin a to take is 0.2g.
It is 5% that prepare test solution, which be dense amine test solution content,.
Detection method in characteristic spectrum foundation is reversed-phased high performace liquid chromatographic.
Standard items saikosaponin a positions saikosaponin a chromatographic peak in product to be tested, radix bupleuri soap in the sample to be tested
Glycosides a chromatographic peak and adjacent chromatographic peak separating degree > 1.5.
Embodiment 2:
Instrument and testing conditions
Waters2695 high performance liquid chromatograph, Waters996 diode array detector, autosampler, WatersC18 column (4.6mm × 250mm × 5 μm)；Detection wavelength: 210nm；Flow rate of mobile phase: 1.0ml/min；Column
Temperature: 30 DEG C；Sample volume: 20 μ L；Flowing phase composition: A (acetonitrile): B (water), gradient elution program:
Table 1:2015 version " Chinese Pharmacopoeia " method
| T(min) | 0→50 | 50→55 |
| A phase (%) | 25→90 | 90 |
| B phase (%) | 75→10 | 10 |
Experimental procedure: test solution injects high performance liquid chromatograph in Example 1, records chromatogram, as a result sees figure
1, Fig. 1 (sample chromatogram figure and its purity figure) shows that saikosaponin a and its structure similar substance merge into a chromatographic peak, peak
Type is good, is not easy to find that the chromatographic peak includes two kinds of substances.
Embodiment 3:
Instrument and testing conditions
Waters2695 high performance liquid chromatograph, Waters996 diode array detector, autosampler, WatersC18 column (4.6mm × 250mm × 5 μm)；Detection wavelength: 210nm；Flow rate of mobile phase: 1.0ml/min；Column
Temperature: 30 DEG C；Sample volume: 20 μ L；Flowing phase composition: A (acetonitrile): B (water), gradient elution program:
Table 2: gradient elution program optimization method
| T(min) | 0→40 | 40→41 | 41→45 |
| A phase (%) | 35→45 | 45→90 | 90 |
| B phase (%) | 65→55 | 55→10 | 10 |
Experimental procedure: test solution injects high performance liquid chromatograph in Example 1, records chromatogram, as a result sees figure
2, Fig. 2 show saikosaponin a and its structure similar substance in acromion, inferior separating effect.
Embodiment 4:
Instrument and testing conditions
Waters2695 high performance liquid chromatograph, Waters996 diode array detector, autosampler, Shiseido
CAPCELLPAKADME chromatographic column (4.6mm × 250mm × 5 μm)；Detection wavelength: 210nm；Flow rate of mobile phase: 1.0ml/min；
Column temperature: 30 DEG C；Sample volume: 20 μ L；Flowing phase composition: A (acetonitrile): B (water), gradient elution program:
Table 3: gradient elution program optimization method
| T(min) | 0→40 | 40→50 | 50→55 | 55→56 | 56→70 |
| A phase (%) | 30→43 | 43→90 | 90 | 90→30 | 30 |
| B phase (%) | 70→57 | 57→10 | 10 | 10→70 | 70 |
Experimental procedure: test solution injects high performance liquid chromatograph in Example 1, records chromatogram, as a result sees figure
3, Fig. 3 show saikosaponin a and its structure similar substance good separation, and separating degree is greater than 1.5 and meets States Pharmacopoeia specifications.
Embodiment 5
Serviceability test is carried out according to 4 condition of embodiment, records chromatogram:
Chromatographic column used in the same high performance liquid chromatograph of serviceability test are as follows: Shiseido CAPCELLPAKADME chromatographic column
(4.6mm × 250mm × 5 μm), ShimadzuODS-3 chromatographic column (4.6mm × 250mm × 5 μm), Agilent
ZORBAXEclipsePlusC18 chromatographic column (4.6mm × 250mm × 5 μm).
High performance liquid chromatograph used in the same chromatographic column of serviceability test are as follows: Waters2695 high performance liquid chromatograph,
Agilent1200 high performance liquid chromatograph (G1315A detector).
Table 4, table 5, Fig. 4 are serviceability test result
Table 4: the chromatographic column of same 3 different brands of instrument
Table 5: the instrument of same two different brands of root chromatogram column
Conclusion: experiment results proved, method containing survey are resistance in different brands chromatographic column and different brands high performance liquid chromatograph
It is good with property.
Embodiment 6
Specificity test is carried out according to 4 condition of embodiment:
Experimental procedure
Auxiliary material (Icing Sugar, dextrin), saikosaponin a reference substance, bupleurum formulation particle are taken, prepares test sample according to embodiment 1,
Sample introduction measurement, records chromatogram.
Fig. 5 is specificity test result.
The result shows that auxiliary material does not interfere this product assay, when granule test sample and saikosaponin a reference substance retain
Between it is identical.
Embodiment 7
Repetitive test is carried out according to 4 condition of embodiment:
Experimental procedure
Accurately weighed 6 parts of test sample of same bupleurum formulation particle (Bupleurum Chinese) systems by the progress test solution of embodiment 1
Standby, injecting chromatograph records chromatogram, calculates saikosaponin a content RSD.
Table 6 is repeated test result
Table 6: repetitive test result (n=6)
Conclusion: this method repeatability is good as can be seen from the results, meets the requirement of assay.
Embodiment 8
Recovery test is carried out according to 4 condition of embodiment:
Experimental procedure
6 conical flasks are taken to be numbered with 1~No. 6, respectively to 1~No. 6 addition saikosaponin a contrast solution (0.4237mgml-
1,91.72%) 1ml, low temperature volatilize, and weigh granule test sample that known saikosaponin a content is 0.323% respectively about
0.1g, it is accurately weighed, the preparation of test solution is carried out by embodiment 1 respectively, sample introduction measurement calculates the rate of recovery.
Table 7 is recovery test result
Table 7: recovery test result (n=6)
Conclusion: the rate of recovery is good as can be seen from the results, is suitable as the assay of this product.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of application of new content assaying method in the control of Radix Bupleuri quality, which comprises the steps of:
(1) reference substance solution is prepared:
Standard items saikosaponin a is taken, using methanol as solvent, prepares standard solution；
(2) test solution is prepared:
Sample to be tested is taken, it is accurately weighed, it sets in stuffed conical flask, methanol solution 25ml of the addition containing strong ammonia solution, close plug, 30 DEG C
Water temperature is ultrasonically treated (power 900W, frequency 60kHz) 30 minutes, and filtration is washed with methanol 20ml points of 2 washing containers and the dregs of a decoction
Liquid merges with filtrate, and for recycling design to doing, residue adds methanol to dissolve, and is transferred in 5ml measuring bottle, adds methanol to scale, shakes up, use
0.22 μm of organic filter membrane filtration, taking subsequent filtrate to get concentration is 0.04g/ml test solution；
(3) chromatographic condition:
Chromatographic column: Shiseido CAPCELL PAK ADME chromatographic column (4.6mm × 250mm × 5 μm), ShimadzuODS-3
Chromatographic column (4.6mm × 250mm × 5 μm) or Agilent ZORBAX Eclipse Plus C18 chromatographic column (4.6mm × 250mm ×
5μm)；Chromatographic column temperature: 30 DEG C；Flow rate of mobile phase: 1.0ml/min；Detection wavelength: 210nm；Detector: UV detector or two
Pole pipe array detector；20 μ L of sample volume；Flow phase composition: A phase is acetonitrile, B Xiang Weishui；Eluent gradient elution, mobile phase
Gradient elution program is as follows:
(4) characteristic spectrum is established:
Reference substance solution and each 20 μ l of test solution respectively inject high performance liquid chromatograph, measure to get characteristic spectrum.
2. application of the new content assaying method of one kind according to claim 1 in the control of Radix Bupleuri quality, special
Sign is, described to prepare sample to be tested in test solution and be Bupleurum Chinese medicinal material, medicine materical crude slice, bupleurum extract or contain saikoside
The Chinese patent drug of a.
3. application of the new content assaying method of one kind according to claim 2 in the control of Radix Bupleuri quality, special
Sign is: the sampling amount of the sample to be tested is 0.1-0.6g.
4. application of the new content assaying method of one kind according to claim 1 in the control of Radix Bupleuri quality, special
Sign is: described to prepare test solution be dense amine test solution content is 5%.
5. application of the new content assaying method of one kind according to claim 1 in the control of Radix Bupleuri quality, special
Sign is: the detection method in the characteristic spectrum foundation is reversed-phased high performace liquid chromatographic.
6. application of the new content assaying method of one kind according to claim 1 in the control of Radix Bupleuri quality, special
Sign is: the standard items saikosaponin a positions saikosaponin a chromatographic peak in product to be tested, bavin in the sample to be tested
Hu saponin(e a chromatographic peak and adjacent chromatographic peak separating degree > 1.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113917009A (en) * | 2021-09-13 | 2022-01-11 | 山西大学 | Construction method and application of bupleurum chinense non-saponin component HPLC fingerprint |
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| JPS6289620A (en) * | 1985-10-16 | 1987-04-24 | Tsumura Juntendo Inc | Methylguanidine production inhibitor |
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| CN102565272A (en) * | 2012-03-01 | 2012-07-11 | 吉林人参研究院 | Quality standard of standardized bupleurum extract |
| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113917009A (en) * | 2021-09-13 | 2022-01-11 | 山西大学 | Construction method and application of bupleurum chinense non-saponin component HPLC fingerprint |
| CN113917009B (en) * | 2021-09-13 | 2024-03-12 | 山西大学 | Construction method and application of HPLC fingerprint of non-saponin component of radix bupleuri |
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Application publication date: 20190409 |