CN110243979A - A kind of adenosine quantitative approach of purslane extract - Google Patents
A kind of adenosine quantitative approach of purslane extract Download PDFInfo
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- CN110243979A CN110243979A CN201910666218.3A CN201910666218A CN110243979A CN 110243979 A CN110243979 A CN 110243979A CN 201910666218 A CN201910666218 A CN 201910666218A CN 110243979 A CN110243979 A CN 110243979A
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- G—PHYSICS
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- 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
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Abstract
The invention discloses a kind of adenosine quantitative approach of purslane extract, quantitative by drawing the adenosine that standard curve carries out in purslane extract.The adenosine quantitative approach of purslane extract of the invention can efficiently and accurately realize quantifying for purslane extract, and easily promote.
Description
Technical field
The present invention relates to a kind of adenosine quantitative approach of purslane extract.
Background technique
Purslane (Portulaca oleracea L.) is the annual meat herbaceous plant of Portulacaceae Portulaca, first
It is loaded in Shennong's Herbal.Yin Qiye is green, stalk is red, spends yellow, root is white, son is black to be also known as five-element's grass or five-element's dish, purslane conduct
Vegetables are widely cultivated in worldwide.Purslane extract is extensive with its good biological characteristics and safety
Exploitation uses, and is added it with the ingredient of anti-inflammatory Shu Min in many cosmetics.
China's pharmacopeia records Portulaca oleracea aerial parts as medicinal, has effects that clearing heat and detoxicating, cooling blood and hemostasis, Ke Yiyong
In toxic-heat and blood stasis, carbuncle swells furunculosis, eczema, erysipelas etc., rich in ingredients such as alkaloid, organic acid, terpene, flavones.Wherein also contain
The hormones such as norepinephrine and dopamine constituents (Liu Di etc., grind in purslane by the measurement of norepinephrine and dopamine
Study carefully), these ingredients 15 years are disabling ingredient in version in " cosmetics safety technical specification ", and hormonal substance can cause skin
Further damage, and then ' hormone face ' is formed, aggravate sensitivity.Safely and effectively, the purslane of reliable in quality extracts product
Have to be developed and perfect.
Purslane contains 3% carbohydrate content, and document report Polysaccharide from Portulaca oleracea has Immune enhancement, anti-inflammatory, anti-oxidant, anti-
The effects of aging (Zhu Xiao official, Polysaccharide from Portulaca oleracea isolate and purify and activity research)；Contain more malic acid, Chinese holly in purslane
(bright red refined, Portulaca oleracea L effective component mentions the low molecular organic acids such as rafter acid, niacin, citric acid, ascorbic acid, succinic acid
System analysis and its quality control new method research), it is considered that aliphatic organic acid is without special bioactivity, but some organic acids
As tartaric acid, citric acid can make it is medicinal.Have report think the comprehensive functions such as malic acid, citric acid, tartaric acid, ascorbic acid in
Nervous centralis, some special acid are certain medium-height grass the effective elements of the medicines.
Contain Adenosine (Liu Jing etc., purslane active site chemical constitution study) in purslane, adenine
Ribonucleotide abbreviation adenosine, adenosine is interior in worldwide widely to be studied as a kind of active constituent, has and releives
Blood vessel, anti-inflammatory and other effects (Petra Ondrackova, Adenosine modulates LPS-induced cytokine
Production in porcine monocytes), it can be used as a kind of active marker to control the matter of Purslane extract
Amount.But quantitative method, purslane extract conduct are carried out to the adenosine in purslane extract there is presently no standard
Anti-inflammatory Shu Min functional component using when usage amount can not accurately estimate.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies of existing technologies, the adenosine for providing a kind of purslane extract is quantitative
Method can efficiently and accurately realize quantifying for purslane extract, and easily promote.
Realizing the technical solution of above-mentioned purpose is: a kind of adenosine quantitative approach of purslane extract, including with
Lower step:
S1 selectes analysis condition: carrying out quantitative analysis, the type of chromatographic column using the Agilent LC-MS instrument of 6545 models
Number and specification be Eclipse Plus C18, the size of chromatographic column is 2.1mm × 50mm, and the packing material size in chromatographic column is 1.8 μ
m；Column temperature is 40 DEG C；1 μ L of sample volume；Eluent gradient is shown in Table 1, Q-TOF method condition and is shown in Table 2；
1. eluent gradient of table, wherein mobile phase A is water, and Mobile phase B is acetonitrile:
| Time (min) | Mobile phase A % | Mobile phase B % | Flow velocity |
| 0 | 95 | 5 | 0.4mL/min |
| 8 | 95 | 5 | 0.4mL/min |
| 8.01 | 5 | 95 | 0.4mL/min |
| 10 | 5 | 95 | 0.4mL/min |
| 10.01 | 95 | 5 | 0.4mL/min |
| 14 | 95 | 5 | 0.4mL/min |
Table 2.Q-TOF method condition:
| Scanning speed | 2spectra/sec |
| Atomization gas temperature | 325℃ |
| Atomization gas flow velocity | 8L/min |
| Atomizing pressure | 35psi |
| Sheath gas | 12L/min |
| Sheath temperature degree | 350℃ |
S2, standard items are prepared: weighing adenosine standard items 2.05mg, distilled water is added to be settled to 25mL, obtain adenosine mark
Quasi- product mother liquor；
Adenosine standard items mother liquor 1mL is measured, being diluted to adenosine content with distilled water is 131.20 × 10-6Mg/mL's
Then solution is diluted to the solution of various concentration in table 3 successively with distilled water up to the standard items of six kinds of various concentrations；
The standard items of 3. 6 kinds of various concentrations of table:
| Serial number | T1 | T2 | T3 | T4 | T5 | T6 |
| Concentration mg/mL | 131.20×10-6 | 65.60×10-6 | 52.48×10-6 | 39.36×10-6 | 26.24×10-6 | 13.12×10-6 |
Specification Curve of Increasing: S3 detects T1~T6 standard items using the analysis condition that step S1 is selected, each
In the total ion current figure of standard items, extract adenosine parent ion signal [M+H]: 268.1040, parent ion signal is accumulated respectively
Point, using adenosine parent ion signal integration area as Y-axis, adenosine concentration (× 10-6Mg/mL) it is X-axis, draws standard curve, obtain
Calibration curve formula:
Y=10235X+5263.6
R2=0.9998；
X is adenosine concentration in above formula, and Y is adenosine parent ion signal integration area, R2For data dependence coefficient；
S4, calibration to be measured are standby: precision weighs purslane extract 30.00mg~50.00mg, is settled to distilled water
10ml is to get to test sample；
S5, to test sample analysis detection: using step S1 select analysis condition in step S4 it is ready to test sample into
Row detection, obtains the total ion current figure to test sample, extracts adenosine parent ion signal [M+H] in the total ion current figure to test sample:
268.1040, and parent ion signal is integrated, obtain adenosine parent ion signal integration area；
S6 is calculated to adenosine content in test sample:
Adenosine parent ion signal integration area to test sample is substituted into Y=10235X+5263.6, is calculated up to test sample
Middle adenosine concentration, the numerical value and the respectively ratio of actual concentrations when test sample is prepared be in each purslane extract adenosine contain
Amount.
A kind of adenosine quantitative approach of above-mentioned purslane extract, wherein gland in the purslane extract
Glycosides content is controlled in 20ppm~30ppm.
The adenosine quantitative approach of purslane extract of the invention can efficiently and accurately realize that purslane mentions
Quantifying for object is taken, and is easily promoted.
Detailed description of the invention
Fig. 1 is the adenosine quantitative approach of purslane extract of the invention；
Fig. 2 is the adenosine content figure using six batches of purslane extracts of adenosine quantitative approach of the present invention measurement.
Specific embodiment
It is right with reference to the accompanying drawing in order to make those skilled in the art be better understood when technical solution of the present invention
Its specific embodiment is described in detail:
Embodiment 1:
Referring to Fig. 1, the embodiment of the present invention, a kind of adenosine quantitative approach of purslane extract, including with
Lower step:
S1 selectes analysis condition: carrying out quantitative analysis, the type of chromatographic column using the Agilent LC-MS instrument of 6545 models
Number and specification be Eclipse Plus C18, the size of chromatographic column is 2.1mm × 50mm, and the packing material size in chromatographic column is 1.8 μ
m；Column temperature is 40 DEG C；1 μ L of sample volume；Eluent gradient is shown in Table 1, and wherein mobile phase A is water, and Mobile phase B is acetonitrile:
| Time (min) | Mobile phase A % | Mobile phase B % | Flow velocity |
| 0 | 95 | 5 | 0.4mL/min |
| 8 | 95 | 5 | 0.4mL/min |
| 8.01 | 5 | 95 | 0.4mL/min |
| 10 | 5 | 95 | 0.4mL/min |
| 10.01 | 95 | 5 | 0.4mL/min |
| 14 | 95 | 5 | 0.4mL/min |
Table 1
Q-TOF method condition is shown in Table 2:
| Scanning speed | 2spectra/sec |
| Atomization gas temperature | 325℃ |
| Atomization gas flow velocity | 8L/min |
| Atomizing pressure | 35psi |
| Sheath gas | 12L/min |
| Sheath temperature degree | 350℃ |
Table 2
S2, standard items are prepared: weighing adenosine standard items 2.05mg, distilled water is added to be settled to 25mL, obtain adenosine mark
Quasi- product mother liquor；
Adenosine standard items mother liquor 1mL is measured, being diluted to adenosine content with distilled water is 131.2 × 10-6Mg/mL's is molten
Then liquid is diluted to the solution of various concentration in table 3 successively with distilled water up to the standard items of six kinds of various concentrations；
| Serial number | T1 | T2 | T3 | T4 | T5 | T6 |
| Concentration mg/mL | 131.20×10-6 | 65.60×10-6 | 52.48×10-6 | 39.36×10-6 | 26.24×10-6 | 13.12×10-6 |
Table 3
Specification Curve of Increasing: S3 detects T1~T6 standard items using the analysis condition that step S1 is selected, each
In the total ion current figure of standard items, extract adenosine parent ion signal [M+H]: 268.1040, parent ion signal is accumulated respectively
Point, using adenosine parent ion signal integration area as Y-axis, adenosine concentration (× 10-6Mg/mL) it is X-axis, draws standard curve, obtain
Calibration curve formula:
Y=10235X+5263.6
R2=0.9998；
X is adenosine concentration in above formula, and Y is adenosine parent ion signal integration area, R2For data dependence coefficient；
S4, calibration to be measured are standby: precision weighs purslane extract 30.00mg~50.00mg, is settled to distilled water
10ml is to get to test sample；
S5, to test sample analysis detection: using step S1 select analysis condition in step S4 it is ready to test sample into
Row detection, obtains the total ion current figure to test sample, extracts adenosine parent ion signal [M+H] in the total ion current figure to test sample:
268.1040, and parent ion signal is integrated, obtain adenosine parent ion signal integration area；
S6 is calculated to adenosine content in test sample:
Adenosine parent ion signal integration area to test sample is substituted into Y=10235X+5263.6, is calculated up to test sample
Middle adenosine concentration, the numerical value and the respectively ratio of actual concentrations when test sample is prepared be in each purslane extract adenosine contain
Amount.
Embodiment 2:
Using the adenosine quantitative approach of purslane extract of the invention, precision weighs purslane extract
45.60mg is settled to 10ml with distilled water to get to test sample.The analysis condition selected using step S1 in embodiment 1 is to be measured
Sample is detected, and the total ion current figure to test sample is obtained, and adenosine parent ion signal [M+ is extracted in the total ion current figure to test sample
H]: 268.1040, and parent ion signal is integrated, obtaining adenosine parent ion signal integration area is 1187088.51, will
The integral area is substituted into embodiment 1 and is calculated in the standard curve of step S3, and the concentration of available adenosine is 115.47
×10-6Mg/ml, content=adenosine concentration/purslane extract concentration of adenosine in the batch purslane extract=
115.47×10-6Mg/ml/4.56mg/ml=25.322ppm.
Embodiment 3:
Referring to Fig. 2, precision weighs six respectively using the adenosine quantitative approach of purslane extract of the invention
It is corresponding to get six batches to be settled to 10ml with distilled water by purslane extract 30.00mg~50.00mg of a batch A1~A6
To test sample, test sample, which is tested, to be waited for six batches respectively, test result is shown in Fig. 2, can be seen that each batch from the testing result of Fig. 2
The adenosine content of secondary middle purslane extract is stablized in 20ppm~30ppm.It therefore can be as an internal control index to horse
The quality of sativa extract is controlled.
In conclusion the adenosine quantitative approach of purslane extract of the invention, can efficiently and accurately realize
Purslane extract quantifies, and easily promotes.
Those of ordinary skill in the art it should be appreciated that more than embodiment be intended merely to illustrate the present invention,
And be not used as limitation of the invention, as long as the change in spirit of the invention, to embodiment described above
Change, modification will all be fallen within the scope of claims of the present invention.
Claims (2)
1. a kind of adenosine quantitative approach of purslane extract, which comprises the following steps:
S1, select analysis condition: using 6545 models Agilent LC-MS instrument carry out quantitative analysis, the model of chromatographic column and
Specification is Eclipse Plus C18, and the size of chromatographic column is 2.1mm × 50mm, and the packing material size in chromatographic column is 1.8um；Column
Temperature is 40 DEG C；Sample volume 1uL；Eluent gradient is shown in Table 1, Q-TOF method condition and is shown in Table 2；
1. eluent gradient of table, wherein mobile phase A is water, and Mobile phase B is acetonitrile:
Table 2.Q-TOF method condition:
S2, standard items are prepared: weighing adenosine standard items 2.05mg, distilled water is added to be settled to 25mL, obtain adenosine standard items
Mother liquor；
Adenosine standard items mother liquor 1mL is measured, being diluted to adenosine content with distilled water is 131.20 × 10-6The solution of mg/mL,
Then it is diluted to the solution of various concentration in table 3 successively with distilled water up to the standard items of six kinds of various concentrations；
The standard items of 3. 6 kinds of various concentrations of table:
Specification Curve of Increasing: S3 detects T1~T6 standard items using the analysis condition that step S1 is selected, in each standard
In the total ion current figure of product, extract adenosine parent ion signal [M+H]: 268.1040, parent ion signal is integrated respectively, with
Adenosine parent ion signal integration area is Y-axis, adenosine concentration (× 10-6Mg/mL) it is X-axis, draws standard curve, obtains standard song
Line formula:
Y=10235X+5263.6
R2=0.9998；
X is adenosine concentration in above formula, and Y is adenosine parent ion signal integration area, R2For data dependence coefficient；
S4, calibration to be measured are standby: precision weighs purslane extract 30.00mg~50.00mg, is settled to 10ml with distilled water, i.e.,
It obtains to test sample；
S5, to test sample analysis detection: being examined to ready in step S4 to test sample using the analysis condition that step S1 is selected
It surveys, obtains the total ion current figure to test sample, extract adenosine parent ion signal [M+H] in the total ion current figure to test sample:
268.1040, and parent ion signal is integrated, obtain adenosine parent ion signal integration area；
S6 is calculated to adenosine content in test sample:
Adenosine parent ion signal integration area to test sample is substituted into Y=10235X+5263.6, is calculated up to gland in test sample
The ratio of glycosides concentration, the numerical value and the actual concentrations respectively when test sample is prepared is the content of adenosine in each purslane extract.
2. a kind of adenosine quantitative approach of purslane extract according to claim 1, which is characterized in that described
Adenosine content control is in 20ppm~30ppm in purslane extract.
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| US20160058680A1 (en) * | 2014-08-28 | 2016-03-03 | Aphrozone Co., Ltd. | Method and apparatus of manufacturing cosmetic products for regenerating skin cell |
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2019
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160058680A1 (en) * | 2014-08-28 | 2016-03-03 | Aphrozone Co., Ltd. | Method and apparatus of manufacturing cosmetic products for regenerating skin cell |
| CN104359968A (en) * | 2014-11-14 | 2015-02-18 | 通化华夏药业有限责任公司 | Research for realizing quick classification and identification of chemical components in ixeris sonchifolia hance injection based on UPLC-Q-TOF-MS technology |
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Application publication date: 20190917 |