CN107702964A - The method that GLA determines saponification esterification in phytosterol and evening primrose oil - Google Patents
The method that GLA determines saponification esterification in phytosterol and evening primrose oil Download PDFInfo
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- CN107702964A CN107702964A CN201711207529.0A CN201711207529A CN107702964A CN 107702964 A CN107702964 A CN 107702964A CN 201711207529 A CN201711207529 A CN 201711207529A CN 107702964 A CN107702964 A CN 107702964A
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- phytosterol
- gla
- evening primrose
- primrose oil
- solution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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- Steroid Compounds (AREA)
Abstract
The method that the present invention provides GLA measure saponification esterification in a kind of phytosterol and evening primrose oil, which solve the inaccurate technical problem of existing phytosterol and evening primrose oil GLA measurement results, it first takes 0.5g samples to be put into 25mL volumetric flask, then it is used as solvent constant volume by the use of n-hexane, 2ml sample solutions are taken to carry out saponification esterification again after well mixed, present invention can apply to the measure of GLA contents in phytosterol and evening primrose oil.
Description
Technical field
The present invention relates to the method that GLA in a kind of health food determines saponification esterification, more particularly, to a kind of plant steroid
The method of GLA saponification esterification in alcohol evening primrose oil.
Background technology
GLA (gamma-Linolenic acid) is commonly called as vitaminF, is before forming the structural material that human body respectively organizes biomembrane, and synthesis
The precursor of row parathyrine.As required unrighted acid in human body, adult's daily requirement amount is about 36mg/kg.Such as intake
Amount deficiency, can cause the disorder of internal function, cause some diseases, such as diabetes, high fat of blood.
Phytosterol and evening primrose oil can obviously reduce blood fat and liver fat content, has to hyperlipemia-fatty liver and preferably controls
Treatment acts on.When the content of GLA in phytosterol and evening primrose oil is measured, the phytosterol and evening primrose oil of half curdled appearance
Can not completely saponification esterification, so as to have impact on the measurement result of GLA contents.
The content of the invention
The present invention is aiming at the inaccurate technical problem of existing phytosterol and evening primrose oil GLA measurement results, there is provided one
The method of GLA saponification esterifications in the high phytosterol and evening primrose oil of kind precision.
The method that the present invention provides GLA measure saponification esterification in a kind of phytosterol and evening primrose oil, step are as follows:
(1) pre-process:Take 0.5g samples to be put into 25mL volumetric flask, then by the use of n-hexane as solvent constant volume, be vortexed
Mix.
(2) saponification:Take the sample solution of pretreatment in 2mL steps (1) to be put into 10mL ground flasks, then add 4mL
0.5mol/L potassium hydroxide methanol solutions, ground flask are fixed on magnetic stirring apparatus, and the top of flask is connected with reflux condensation mode
Pipe, imports nitrogen into solution from condenser pipe open top, makes to be full of nitrogen in reaction bulb all the time.Open magnetic stirring apparatus and add
Heat, reaction solution is kept for 65 ± 5 DEG C, be stirred at reflux about 15min.
(3) formicester:4mL boron trifluoride methanol solution is added from condenser pipe open top, is stirred (65 ± 5 DEG C), backflow
2min, continue to stir 5min from condenser pipe open top addition 5mL n-hexanes after being cooled to room temperature, remove condenser pipe, add 5mL
Saturated sodium-chloride water solution, shake 1~5 minute, be transferred to separation water and organic phase in 25mL separatory funnels, add 3mL n-hexanes
Wash water phase, separation, aqueous phase is abandoned, merge organic phase and be settled to 10mL, for measure.
Preferably, 0.5mol/L potassium hydroxide methanol solutions in step (2):Weigh 28g KOH and be dissolved in 1000mL methanol.
Preferably, boron trifluoride methanol solution (1+4) in step (3):1 part of 40% boron trifluoride ether solution is taken, adds first
4 parts of alcohol, mixing.
The present invention pre-processes by using n-hexane to phytosterol and evening primrose oil, and the mode for the mixing that is then vortexed makes sample
GLA in product fully dissolves, and greatly improves the precision of GLA assays in phytosterol and evening primrose oil soft capsule.
Embodiment
Phytosterol and evening primrose oil soft capsule, manufacturer:Weihai lily biology technical concern Co., Ltd.
The present invention is as follows to the saponification esterification method of GLA assays in phytosterol and evening primrose oil soft capsule:
(1) pre-process:Take 0.5g samples to be put into 25ml volumetric flask, then by the use of n-hexane as solvent constant volume, be vortexed
Mix.
(2) saponification:Take the sample solution of pretreatment in 2ml steps (1) to be put into 10mL ground flasks, then add
4ml0.5mol/L potassium hydroxide methanol solutions, ground flask are fixed on magnetic stirring apparatus, and the top of flask is connected with returned cold
Solidifying pipe, imports nitrogen into solution from condenser pipe open top, makes to be full of nitrogen in reaction bulb all the time.Open magnetic stirring apparatus simultaneously
Heating, reaction solution is kept for 65 ± 5 DEG C, be stirred at reflux about 15min.
(3) formicester:4mL boron trifluoride methanol solution is added from condenser pipe open top, is stirred (65 ± 5 DEG C), backflow
2min, continue to stir 5min from condenser pipe open top addition 5mL n-hexanes after being cooled to room temperature, remove condenser pipe, add 5mL
Saturated sodium-chloride water solution, shake 1~5 minute, be transferred to separation water and organic phase in 25mL separatory funnels, add 3mL n-hexanes
Wash water phase, separation, aqueous phase is abandoned, merge organic phase and be settled to 10mL (1.0mL is concentrated into when concentration is low), for measure.
0.5mol/L potassium hydroxide methanol solutions in step (2):Weigh 28g KOH and be dissolved in 1000mL methanol.
Boron trifluoride methanol solution (1+4) in step (3):1 part of 40% boron trifluoride ether solution is taken, adds 4 parts of methanol, is mixed
It is even.
The present invention compared with directly taking the assay method of 0.1g phytosterol and evening primrose oil sample saponification esterifications, detection
Numerical value is respectively 5.66 and 4.17, and assay is more accurate.
Only as described above, be only the present invention specific embodiment, when the model implemented of the present invention can not be limited with this
Enclose, therefore the displacement of its equivalent assemblies, or the equivalent variations made according to scope of patent protection of the present invention and modification, it all should still belong to this hair
The category that bright claims are covered.
Claims (3)
1. a kind of method that GLA determines saponification esterification in phytosterol and evening primrose oil, it is characterised in that step is as follows:
(1) pre-process:Take 0.5g samples to be put into 25mL volumetric flask, then by the use of n-hexane as solvent constant volume, be vortexed and mix;
(2) saponification:Take the sample solution of pretreatment in 2mL steps (1) to be put into 10mL ground flasks, then add 4mL
0.5mol/L potassium hydroxide methanol solutions, ground flask are fixed on magnetic stirring apparatus, and the top of flask is connected with reflux condensation mode
Pipe, imports nitrogen into solution from condenser pipe open top, makes to be full of nitrogen in reaction bulb all the time.Open magnetic stirring apparatus and add
Heat, reaction solution is kept for 65 ± 5 DEG C, be stirred at reflux about 15min;
(3) formicester:4mL boron trifluoride methanol solution is added from condenser pipe open top, is stirred (65 ± 5 DEG C), flow back 2min,
Continue to stir 5min from condenser pipe open top addition 5mL n-hexanes after being cooled to room temperature, remove condenser pipe, add 5mL saturations
Sodium-chloride water solution, shake 1~5 minute, be transferred to separation water and organic phase in 25mL separatory funnels, add 3mL n-hexane wash waters
Phase, separation, aqueous phase is abandoned, merge organic phase and be settled to 10mL, for measure.
2. the method that GLA determines saponification esterification in phytosterol and evening primrose oil according to claim 1, it is characterised in that
0.5mol/L potassium hydroxide methanol solutions in step (2):Weigh 28gKOH and be dissolved in 1000mL methanol.
3. the method for GLA measure saponification esterifications, its feature exist in a kind of phytosterol and evening primrose oil as claimed in claim 1
The boron trifluoride methanol solution (1+4) in step (3):1 part of 40% boron trifluoride ether solution is taken, adds 4 parts of methanol, mixing is
Can.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104162537A (en) * | 2014-06-10 | 2014-11-26 | 南京农业大学 | Method for utilizing copper contaminated soil reasonably |
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2017
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Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104162537A (en) * | 2014-06-10 | 2014-11-26 | 南京农业大学 | Method for utilizing copper contaminated soil reasonably |
Non-Patent Citations (1)
Title |
---|
张淑秀: "《最新保健食品注册手册》", 31 December 2005 * |
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Application publication date: 20180216 |