CN107831243A - The method of Astragaloside content in HPLC-ELSD measure Kang ' ai injections - Google Patents
The method of Astragaloside content in HPLC-ELSD measure Kang ' ai injections Download PDFInfo
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- CN107831243A CN107831243A CN201711369841.XA CN201711369841A CN107831243A CN 107831243 A CN107831243 A CN 107831243A CN 201711369841 A CN201711369841 A CN 201711369841A CN 107831243 A CN107831243 A CN 107831243A
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- Prior art keywords
- astragaloside
- reference substance
- kang
- injection
- elsd
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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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention discloses a kind of method that HPLC ELSD determine Astragaloside content in Kang ' ai injection, comprise the following steps：(1) reference substance solution is prepared：Take Astragaloside IV reference substance that reference substance solution is made with methanol；(2) testing sample solution is prepared：Precision, which takes, determines Kang ' ai injection sample and adds methanol dilution, and testing sample solution is made；(3) reference substance solution injection high performance liquid chromatograph and EISD are taken, establishes Astragaloside IV standard curve；(4) testing sample solution injection high performance liquid chromatograph and EISD measure are taken, the peak area of Astragaloside IV is obtained, so as to obtain Astragaloside content according to standard curve；The step (3) and the chromatographic condition of (4)：4.6mm × 250mm Shimadzu VP ODS posts；Mobile phase：Acetonitrile:Water=30:70；Flow velocity：1.0ml/min；Column temperature：30℃；Sample size：10ul；ELSD parameters：Atomizer temperature 60 C, drift tube temperature are 89 DEG C, nitrogen pressure 0.70Mpa, gas flow 1.15L/min.
Description
Technical field
The present invention relates to the method for Astragaloside content in measure Kang ' ai injection, more particularly to a kind of HPLC-ELSD
The method for determining Astragaloside content in Kang ' ai injection.
Background technology
Kang ' ai injection can QI invigorating righting, strengthen body's immunity.Available for primary carcinoma of liver, lung cancer, the carcinoma of the rectum,
Malignant lymphoma, gynecologic malignant tumor；Leucocyte caused by a variety of causes is low and reduces disease.The treatment of chronic hepatitis B
Chinese traditional compound medicine, recorded in the kind of national drug Chinese medicine standard, be made up of the Radix Astragali, ginseng and the taste Chinese medicine of kushenin three.
It there are no the assay report of astragalus root components Astragaloside IV
The content of the invention
The method that the purpose of the present invention aims to provide Astragaloside content in a kind of HPLC-ELSD measure Kang ' ai injection.
The purpose of the present invention is achieved through the following technical solutions：The Radix Astragali in a kind of HPLC-ELSD measure Kang ' ai injection
The method of glucoside content, comprises the following steps：
(1) reference substance solution is prepared：Take Astragaloside IV reference substance that reference substance solution is made with methanol；
(2) testing sample solution is prepared：Precision, which takes, determines Kang ' ai injection sample and adds methanol dilution, and it is molten that testing sample is made
Liquid；
(3) reference substance solution injection high performance liquid chromatograph and EISD (ELSD) are taken, establishes Radix Astragali first
Glycosides standard curve；
(4) testing sample solution injection high performance liquid chromatograph and EISD (ELSD) measure are taken, is obtained
The peak area of Astragaloside IV, so as to obtain Astragaloside content according to standard curve；
The step (3) and the chromatographic condition of (4)：4.6mmX250mm Shimadzu VP-ODS posts；Mobile phase：Acetonitrile:Water=
30:70；Flow velocity：1.0ml/min；Column temperature：30℃；Sample size：10ul；ELSD parameters：Atomizer temperature 60 C, drift tube temperature
Spend for 89 DEG C, nitrogen pressure 0.70Mpa, gas flow 1.15L/min.
In the step (1), precision weighs Astragaloside IV reference substance 4.17mg and put in 10ml volumetric flasks, adds methanol dissolving simultaneously
Scale is diluted to, is shaken up, produces the reference substance solution that concentration is 0.417mg/ml.
In the step (2), precision measures Kang ' ai injection 10ml and put in 125ml separatory funnel, adds water 20ml, uses water
The n-butanol shaking extraction 3 times, each 20ml of saturation, merges n-butanol liquid, water bath method, residue adds methanol to dissolve and be settled to
In 5ml volumetric flasks, shake up, filtered with 0.22 μm of miillpore filter, produce testing sample solution.
Compared with prior art, the invention has the advantages that：
Compared with prior art, method provided by the invention is simple to operate, high efficiency and time conservation, and qualification result is objective and accurate.
Embodiment
Embodiment 1
(1) reference substance solution is prepared：Precision weighs Astragaloside IV reference substance 4.17mg and put in 10ml volumetric flasks, adds methanol molten
Solve and be diluted to scale, shake up, produce the reference substance solution that concentration is 0.417mg/ml.
(2) testing sample solution is prepared：Precision measures Kang ' ai injection 10ml and put in 125ml separatory funnel, adds water
20ml, with water saturated n-butanol shaking extraction 3 times, each 20ml, merge n-butanol liquid, water bath method, residue adds methanol molten
Solve and be settled in 5ml volumetric flasks, shake up, filtered with 0.22 μm of miillpore filter, produce testing sample solution.
(3) solution by contrast solution methanol dilution into concentration 0.160mg/m1, the accurate draw solution 4,5 of difference,
10,15,20 μ l inject Shimadzu LC-2010A HT high performance liquid chromatographs and EISD (ELSD) is measured,
Using the logarithm of sample size as abscissa x, using the logarithm of Astragaloside IV peak area as ordinate Y, it is Y=to obtain equation of linear regression
1.412x+9.0692 r=0.9999.
Chromatographic column：4.6mmX250mm Shimadzu VP-ODS posts；Mobile phase：Acetonitrile:Water=30:70；Flow velocity：1.0ml/min；
Column temperature：30℃；Sample size：10ul；ELSD parameters：Atomizer temperature 60 C, drift tube temperature are 89 DEG C, nitrogen pressure
0.70Mpa, gas flow 1.15L/min.
(4) testing sample solution injection Shimadzu LC-2010A HT high performance liquid chromatographs and EISD are taken
(ELSD) it is measured, obtains Astragaloside IV peak area, the content of Astragaloside IV is obtained according to regression equation calculation.Take different batches
Number Kang ' ai injection 3 batches be measured respectively, Astragaloside content is respectively：0.09mg/ml、0.102 mg/ml、
0.12mg/ml。
The present invention can be summarized with others without prejudice to the concrete form of the spirit or essential characteristics of the present invention.The present invention's
The embodiment above can only all be considered the description of the invention rather than limitation, therefore every substantial technological according to the present invention
Any subtle modifications, equivalent variations and modifications made to above example, are belonged in the range of technical solution of the present invention.
Claims (3)
1. a kind of method of Astragaloside content in HPLC-ELSD measure Kang ' ai injection, it is characterized in that, comprise the following steps：
(1) reference substance solution is prepared：Take Astragaloside IV reference substance that reference substance solution is made with methanol；
(2) testing sample solution is prepared：Precision, which takes, determines Kang ' ai injection sample and adds methanol dilution, and testing sample solution is made；
(3) reference substance solution injection high performance liquid chromatograph and EISD are taken, establishes Astragaloside IV standard curve；
(4) testing sample solution injection high performance liquid chromatograph and EISD measure are taken, obtains Astragaloside IV
Peak area, so as to obtain Astragaloside content according to standard curve；
The step (3) and the chromatographic condition of (4)：4.6mmX250mm Shimadzu VP-ODS posts；Mobile phase：Acetonitrile:Water=30:70；
Flow velocity：1.0ml/min；Column temperature：30℃；Sample size：10ul；ELSD parameters：Atomizer temperature 60 C, drift tube temperature 89
DEG C, nitrogen pressure 0.70Mpa, gas flow 1.15L/min.
2. the method for Astragaloside content, its feature in HPLC-ELSD measure Kang ' ai injection according to claim 1
It is that in the step (1), precision weighs Astragaloside IV reference substance 4.17mg and put in 10ml volumetric flasks, adds methanol to dissolve and dilute
To scale, shake up, produce the reference substance solution that concentration is 0.417mg/ml.
3. the method for Astragaloside content, its feature in HPLC-ELSD measure Kang ' ai injection according to claim 1
It is that in the step (2), precision measures Kang ' ai injection 10ml and put in 125ml separatory funnel, adds water 20ml, uses water saturation
N-butanol shaking extraction 3 times, each 20ml, merge n-butanol liquid, water bath method, residue adds methanol to dissolve and be settled to 5ml
In volumetric flask, shake up, filtered with 0.22 μm of miillpore filter, produce testing sample solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711369841.XA CN107831243A (en) | 2017-12-19 | 2017-12-19 | The method of Astragaloside content in HPLC-ELSD measure Kang ' ai injections |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711369841.XA CN107831243A (en) | 2017-12-19 | 2017-12-19 | The method of Astragaloside content in HPLC-ELSD measure Kang ' ai injections |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113230385A (en) * | 2021-05-08 | 2021-08-10 | 深圳市保尔医疗服务有限公司 | Pharmaceutical formulation for relieving cancer pain and cancer and use method thereof |
| WO2022127051A1 (en) * | 2020-12-19 | 2022-06-23 | 无锡济煜山禾药业股份有限公司 | Method for measuring content of tween 80 in xingnaojing injection |
-
2017
- 2017-12-19 CN CN201711369841.XA patent/CN107831243A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022127051A1 (en) * | 2020-12-19 | 2022-06-23 | 无锡济煜山禾药业股份有限公司 | Method for measuring content of tween 80 in xingnaojing injection |
| CN113230385A (en) * | 2021-05-08 | 2021-08-10 | 深圳市保尔医疗服务有限公司 | Pharmaceutical formulation for relieving cancer pain and cancer and use method thereof |
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Application publication date: 20180323 |