CN101806785B - Method for detecting jujuboside content and swertisin content in jujube tincture - Google Patents
Method for detecting jujuboside content and swertisin content in jujube tincture Download PDFInfo
- Publication number
- CN101806785B CN101806785B CN 201010158560 CN201010158560A CN101806785B CN 101806785 B CN101806785 B CN 101806785B CN 201010158560 CN201010158560 CN 201010158560 CN 201010158560 A CN201010158560 A CN 201010158560A CN 101806785 B CN101806785 B CN 101806785B
- Authority
- CN
- China
- Prior art keywords
- jujuboside
- content
- medicine
- standard
- flavonol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method for detecting the jujuboside content and the swertisin content in jujube tincture, which is characterized by using a mixed liquid of acetonitrile and 0.1% aqueous formic acid solution as the mobile phase and adopting a high efficiency liquid chromatography method to carry out the detection, wherein an evaporation light scattering detector (ELSD) is used for the high efficiency liquid chromatography. In the method for detecting the jujuboside content and the swertisin content in jujube tincture, the acetonitrile and the aqueous formic acid solution can be used as the mobile phase and the extracting agent for the sample concurrently, thereby facilitating the pretreatment of the sample; and the evaporation light scattering detector (ELSD) is used for the high efficiency liquid chromatography, the target object to be detected has higher signal intensity on the detector and has better adaptability, and a better function relationship is formed, thereby enhancing the detection accuracy.
Description
Technical field
The present invention relates to a kind ofly detect jujuboside in the jujube tincture and when the method for medicine flavonol content, belong to the trace analysis technical field.
Background technology
Red date is a kind of nutritious fruit, wherein contains the multiple nutrients material, such as saponins, and flavonoids, alkaloids, carbohydrate, amino acids.Can separate in the jujube kernel and obtain jujuboside A and B; Can also extract flavones C-glycoside (namely when medicine flavonol or swertisin) in the seed of red date, when medicine flavonol and jujuboside all are to have the active substance that improves health-care efficacies such as immunity.Jujube tincture is common essence spice for cigarette, often uses in the perfuming of tobacco product, flavoring.Current along with concern is received in the essence spice for cigarette quality control day by day, the principal ingredient of perfume material and endemic element, the analyzing and testing that especially has these compositions with immunizing health effect also becomes focus.
At present at jujuboside A and B commonly used be that high performance liquid chromatography is in conjunction with the detection method of diode array detector (DAD detecting device), but unsatisfactory through contrast jujuboside A and the respective strengths of B on the DAD detecting device, thereby influence detects precision.And detect jujuboside simultaneously and be not reported when the method for medicine flavonol.
Summary of the invention
The purpose of this invention is to provide a kind of accuracy in detection and can detect jujuboside in the jujube tincture simultaneously and when the method for medicine flavonol content.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind ofly detect jujuboside in the jujube tincture and when the method for medicine flavonol content, it is that the mixed liquor with acetonitrile and 0.1% aqueous formic acid is the phase that flows, adopt high performance liquid chromatography to detect, wherein the detecting device that adopts of high performance liquid chromatography is evaporative light-scattering detector (ELSD).
The volume ratio of described mobile middle acetonitrile mutually and 0.1% aqueous formic acid is 60:40 ~ 75:25.
Detection method concrete steps of the present invention are as follows:
1) standard working curve is formulated: contain mixed standard solution when at least three concentration of three kinds of standard items of medicine flavonol, jujuboside A and jujuboside B with the preparation mutually of flowing in the 0.014-0.19mg/ml scope, the recycling high performance liquid chromatograph detects the content of three kinds of standard items in the mixed standard solution of above-mentioned all concentration respectively, and draws the standard working curve of three kinds of standard items respectively and calculate its regression equation according to peak area and the corresponding concentration of three kinds of standard items;
2) The pretreatment: take by weighing the jujube tincture sample in adding the phase that flows, through centrifugal treating after the ultrasonic extraction, get supernatant liquor, filter and obtain sample solution; The recycling high performance liquid chromatograph adopts the condition identical with step 1) respectively sample solution to be detected, and bring into respectively according to the peak area that obtains in the regression equation of standard working curve, calculate the content as medicine flavonol, jujuboside A and jujuboside B in the sample;
Step 1), 2) high-efficient liquid phase chromatogram condition in is: chromatographic column: C18(4.6 * 150mm); Flow velocity: 0.8ml/min;
Evaporative light-scattering detector condition: 79 ~ 81.5 ℃ of drift tube temperatures; Airshed: 2.0 ~ 2.2L/min.
Concentration range when the medicine flavonol in the described mixed standard solution is 0.038-0.19mg/ml, and the concentration range of jujuboside A is 0.01-0.1mg/ml, and the concentration range of jujuboside B is 0.014-0.14mg/ml.
Jujuboside and when the method for medicine flavonol content in the detection jujube tincture of the present invention, acetonitrile and aqueous formic acid can be simultaneously as the extractant that flows mutually with sample, make the pre-treatment of sample comparatively simple, and the detecting device of high performance liquid chromatography adopts evaporative light-scattering detector (ELSD), the signal of measured target thing on this detecting device is stronger, better matching property is arranged, and formed function corresponding relation preferably, improved the accuracy that detects.In addition, the present invention reaches temperature and the carrier gas flux of ELSD drift tube by optimizing the middle organic phase ratio mutually that flows, improved the degree of separation of measured target thing on chromatographic column, reduced the Chromatogram Baseline noise, obtained and to have improved accuracy in detection for tangible chromatographic peak.
Description of drawings
Fig. 1 is the chromatogram of mixed standard solution;
Fig. 2 is the standard working curve figure when the medicine flavonol;
Fig. 3 is the standard working curve figure of jujuboside A;
Fig. 4 is the standard working curve figure of jujuboside B;
Fig. 5 is the standard log-log graph when the medicine flavonol;
Fig. 6 is the standard log-log graph of jujuboside A;
Fig. 7 is the standard log-log graph of jujuboside B;
Fig. 8 is contrast experiment's synoptic diagram.
Embodiment
Below in conjunction with specific embodiment method of the present invention is done detailed introduction:
Jujuboside and specifically comprise the steps: when the method for medicine flavonol content in the detection jujube tincture of the present invention
High-efficient liquid phase chromatogram condition:
Chromatographic column: YMC-ODS-A C18(4.6 * 150mm, 5 μ m);
Phase flows: acetonitrile-0.1% aqueous formic acid=60: 40;
Flow velocity: 0.8ml/min;
Sample size: 5 μ l;
The evaporative light-scattering detector condition:
81.5 ℃ of drift tube temperatures;
Airshed: 2.2L/min.
1) formulation of standard working curve:
Accurately take by weighing respectively when the medicine flavonol, jujuboside A and jujuboside B standard items 4.8mg, 2.5mg, 3.5mg in same 25ml volumetric flask, with the dilution of mobile phased soln and be settled to scale mark, obtain the standard solution storing solution of three kinds of standard items, adopt this storing solution to prepare the mixed standard solution of series concentration with the phase dilution that flows, make when the medicine flavonol, the concentration range of jujuboside A and jujuboside B is respectively 0.038-0.19mg/ml, 0.01-0.1mg/ml, 0.014-0.14mg/ml, standard mixed solution to this series concentration carries out the high performance liquid chromatography detection, the preparation of concrete mixed standard solution and peak area such as the table 1 and shown in Figure 1 of corresponding detection: peak 1 and peak 2 are the chromatographic peak when the medicine flavonol among Fig. 1, peak 3 and peak 4 are respectively the chromatographic peak of jujuboside A and jujuboside B, chromatographic peak among Fig. 1 is obvious and sharp keen, steady and the noiselessness of baseline illustrates that the ELSD detecting device that the present invention adopts has produced analytical effect preferably after optimal conditions.
The concentration of table 1 standard mixed solution and corresponding testing result
According to the concentration in the table 1 and the mapping of respective peaks area data, wherein to work as the medicine flavonol and go out peak 1 and peak 2 simultaneously, working curve calculates according to two peak area sums.Concrete result of calculation is shown in Fig. 2-4 and table 2.
Table 2 standard working curve parameter
When medicine flavonol, jujuboside A and B in concentration range separately, concentration/peak area presents the power exponential function relation, shown in Fig. 2,3,4.Jujuboside A and each concentration of B standard items and peak area are taken from right logarithm respectively, mapping then, shown in Fig. 5,6,7, jujuboside A and B meet the double-log linear relationship between the signal on the ELSD detecting device and standard items concentration, measured target thing and ELSD detecting device have better matching property.
2) detection of sample:
Get about jujube tincture sample 0.1 gram and place tool plug triangular flask, pipetting 40ml flows to triangular flask, place the ultrasonic extraction of ultrasonic auxiliary extraction device more than 30 minutes, get solution 10ml to the centrifuge tube in 4000rpm centrifugal 10 minutes, get supernatant liquor, filter through 0.45 μ m pin type filter, obtain sample solution.
Adopt the high performance liquid chromatograph of step 1) the same terms to detect sample solution, the chromatographic peak as medicine flavonol, jujuboside A and jujuboside B that obtains is brought into respectively in the corresponding regression equation, obtain working as in the sample solution concentration of medicine flavonol, jujuboside A and jujuboside B, thereby calculate the content of working as medicine flavonol, jujuboside A and jujuboside B in the sample.
Detection effect of the present invention:
1, detectability and quantitative limit
Get each standard items working curve least concentration duplicate detection, calculate standard deviation and relative standard deviation.Respectively with 3 times and 10 times of standard deviations as detectability and quantitative limit.Concrete data are as shown in table 3.
Table 3 detectability and quantitative limit
2, precision and recovery of standard addition:
Get concentration known jujube tincture sample, add three kinds of standard items, assay method recovery of standard addition respectively according to varying level.The result of mark-on level and actual detected is as shown in table 4.
Table 4 mark-on level and recovery of standard addition
3, contrast experiment
The present invention is example with jujuboside A, adopt ELSD detecting device and DAD detecting device to compare experiment respectively with identical condition, its result as shown in Figure 8, have type good chromatographic peak in peak to occur in the chromatogram that ELSD obtains about 4 minutes, and identical retention time is not found effective chromatographic peak in the chromatogram that the DAD detecting device obtains.As seen, for measured target thing jujuboside A, ELSD is the detecting device more suitable than DAD, and DAD necessarily requires the measured target thing to have to absorb just in the UV, visible light optical band to be suitable for, and service condition is harshness comparatively.
4, to the detection of actual sample
Adopt the described method of embodiment, certain company's jujube tincture sample detected, detect when the content of medicine flavonol, jujuboside A and B as shown in table 5.
The testing result of table 5 actual sample
Claims (2)
1. one kind is detected jujuboside in the jujube tincture and when the method for medicine flavonol content, it is characterized in that: the mixed liquor with acetonitrile and 0.1% aqueous formic acid is the phase that flows, adopt high performance liquid chromatography to detect, wherein the detecting device that adopts of high performance liquid chromatography is evaporative light-scattering detector (ELSD); The volume ratio of described mobile middle acetonitrile mutually and 0.1% aqueous formic acid is 60:40-75:25; Concrete steps are as follows:
1) standard working curve is formulated: contain mixed standard solution when at least three concentration of three kinds of standard items of medicine flavonol, jujuboside A and jujuboside B with the preparation mutually of flowing in the 0.014-0.19mg/ml scope, the recycling high performance liquid chromatograph detects the content of three kinds of standard items in the mixed standard solution of above-mentioned all concentration respectively, and draws the standard working curve of three kinds of standard items respectively and calculate its regression equation according to peak area and the corresponding concentration of three kinds of standard items;
2) The pretreatment: take by weighing the jujube tincture sample in adding the phase that flows, through centrifugal treating after the ultrasonic extraction, get supernatant liquor, filter and obtain sample solution; The recycling high performance liquid chromatograph adopts the condition identical with step 1) respectively sample solution to be detected, and bring into respectively according to the peak area that obtains in the regression equation of standard working curve, calculate the content as medicine flavonol, jujuboside A and jujuboside B in the sample;
Step 1), 2) high-efficient liquid phase chromatogram condition in is: chromatographic column: C18(4.6 * 150mm); Flow velocity: 0.8ml/min;
Evaporative light-scattering detector condition: drift tube temperature 79-81.5 ℃; Carrier gas is nitrogen, airshed: 2.0-2.2L/min.
2. jujuboside and when the method for medicine flavonol content in the detection jujube tincture according to claim 1, it is characterized in that: the concentration range when the medicine flavonol in the described mixed standard solution is 0.038-0.19mg/ml, the concentration range of jujuboside A is 0.01-0.1mg/ml, and the concentration range of jujuboside B is 0.014-0.14mg/ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010158560 CN101806785B (en) | 2010-04-28 | 2010-04-28 | Method for detecting jujuboside content and swertisin content in jujube tincture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010158560 CN101806785B (en) | 2010-04-28 | 2010-04-28 | Method for detecting jujuboside content and swertisin content in jujube tincture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101806785A CN101806785A (en) | 2010-08-18 |
| CN101806785B true CN101806785B (en) | 2013-08-14 |
Family
ID=42608675
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010158560 Active CN101806785B (en) | 2010-04-28 | 2010-04-28 | Method for detecting jujuboside content and swertisin content in jujube tincture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101806785B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952241B (en) * | 2014-05-22 | 2015-08-05 | 嘉兴市得百科新材料科技有限公司 | A kind of red date spice mixt and preparation method thereof |
| KR102331257B1 (en) * | 2020-03-27 | 2021-11-25 | 경희대학교 산학협력단 | Composition for preventing or treating metabolic diseases, including jujuboside A or a pharmaceutically acceptable salt thereof as an active ingredient |
-
2010
- 2010-04-28 CN CN 201010158560 patent/CN101806785B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN101806785A (en) | 2010-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103163244B (en) | Method for simultaneously detecting sesquiterpene and curcumin components | |
| Kwon et al. | Determination of astragalin and astragaloside content in Radix Astragali using high-performance liquid chromatography coupled with pulsed amperometric detection | |
| CN103913528B (en) | Quantitative detection method for pyrethriods pesticides in fresh tea | |
| CN105467055A (en) | Method for determining alkaloids in tea leaves by using GC-MS (Gas Chromatography-Mass Spectrometer) method | |
| CN104237414A (en) | Method for simultaneously detecting various preservatives remaining in orange with liquid chromatograph/mass spectrometer | |
| CN106124639A (en) | The multicomponent content assaying method of Eucommia ulmoides | |
| Ma et al. | Rapid resolution liquid chromatography (RRLC) analysis for quality control of Rhodiola rosea roots and commercial standardized products | |
| CN103926347A (en) | Quantitative detection method for organophosphorus pesticide in soil | |
| CN104374854B (en) | A kind of method of multiple phenolic content in HPLC wavelength handoff technique Simultaneously test Noni juice | |
| CN104215705B (en) | A kind of method detecting Organochlorine Pesticides Residues In Agricultural Products | |
| CN103913538B (en) | The quantitative detecting method of organophosphorus insecticide in a kind of tea fresh leaves | |
| CN101806785B (en) | Method for detecting jujuboside content and swertisin content in jujube tincture | |
| CN103063752A (en) | Gas chromatography-mass spectrometry determination method for residual amount of dibromochloropropane in grain | |
| CN105277642A (en) | Method for simultaneously quantitatively determining content of multiple phenols compositions in gastrodia elata Bl. | |
| CN106324167B (en) | Method for determining flavonoid components in astragalus extract by UPLC | |
| Li et al. | An accurate and reliable analytical strategy for simultaneous determination of target furanocoumarins and flavonoids in cosmetic and pharmaceutical samples by ultra-high performance supercritical fluid chromatography | |
| CN102539572A (en) | Method for detecting rutin and quercetol through ionic liquid-accelerating solvent extraction and high performance liquid chromatograph chemiluminescence | |
| CN103149311B (en) | Measuring method of sesame phenol content in tobacco essence perfume | |
| CN106198826B (en) | With the method for tocopherol and tocotrienols content in the positive chemical source mass Spectrometry for Determination edible vegetable oil of gas-chromatography | |
| CN105572237A (en) | High performance liquid chromatographic method for rapid quantitative assessment of honey quality | |
| CN107389814A (en) | A kind of method that RP HPLC DAD quickly analyze sea-buckthorn Main Flavonoids aglycon | |
| CN104090043B (en) | A kind of method measuring methyl eugenol in cigarette mainstream flue gas | |
| CN106596740A (en) | Method for adopting gas chromatography method to determine residual quantity of pendimethalin in garlic | |
| CN104215614A (en) | Method for detecting aloin A, aloin B and aloe-emodin in series through high performance liquid chromatography-diode array/fluorescent detector | |
| CN103792301A (en) | Method for measuring content of epigoitrin in anti-virus granules |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |