CN103884813B - Method for detecting content of phosphatidylserine in food - Google Patents
Method for detecting content of phosphatidylserine in food Download PDFInfo
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- CN103884813B CN103884813B CN201410145181.7A CN201410145181A CN103884813B CN 103884813 B CN103884813 B CN 103884813B CN 201410145181 A CN201410145181 A CN 201410145181A CN 103884813 B CN103884813 B CN 103884813B
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Abstract
The invention discloses a method for detecting the content of phosphatidylserine in food. The method comprises the following steps: (1) weighing food to be detected, preparing a sample aqueous solution, extracting with a mixed solution of trichloromethane and methyl alcohol, filtering and evaporating filtrate to dryness; (2) extracting the dried substance obtained in the step (1) by a mixed solution of trichloromethane, methyl alcohol and water, filtering and standing filtrate; and (3) carrying out high performance liquid chromatography detection on a solution at an under layer. The method has the advantages of high sensitivity, high precision and high accuracy.
Description
Technical field
The present invention relates to field of food detection.More specifically, a kind of detection method of phosphorus in food acyl serine content is related to.
Background technology
Phosphatidylserine (being called for short ps) is a kind of phospholipid substance, has vital role to the brain neuroblastoma system health of people.At present, ps can be added in food as raw-food material and take, or take as health food.When ps takes as health food, because purity is high, content is high, general high performance liquid chromatography is used to detect, do not need complicated pretreatment technology, and when ps adds in food as bread and cheese raw material, its addition is generally less, interference by other raw materials in food not easily detects, especially based in the food of the materials such as protein, fat, starch, because the materials such as protein, fat, starch can play certain bury function to ps, make ps be not easy to be separated from these materials, thus affect the detection of ps.
Because effect of ps is extensively approved by people, in increasing food, with the addition of ps, explore and set up the new method that effectively detects phosphorus in food acyl serine content, for the monitoring of raw-food material, there is more importantly meaning.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of detection method of phosphorus in food acyl serine content.The method utilizes special separation and extraction technology that phosphatidylserine almost can all be extracted from the interfering material of raw-food material; the recovery of method is high, favorable reproducibility; simple to operate, provide technical support for the scale of phosphatidylserine in food uses.
For solving the problems of the technologies described above, the present invention adopts following technical proposals:
A detection method for phosphorus in food acyl serine content, the method comprises the following steps:
(1) take food to be measured, be mixed with sample aqueous solution, extract with the mixed solution of methenyl choloride and methyl alcohol, then filter, by filtrate evaporate to dryness;
(2) with the mixed solution of methenyl choloride, first alcohol and water, the evaporate to dryness material that step (1) obtains is extracted, then filter, filtrate stratification;
(3) take off layer solution and carry out high performance liquid chromatography detection.
In said method, described food comprises solid-state product and liquid product.Because the addition difference of phosphatidylserine in different food products is comparatively large, during preparation sample aqueous solution, in order to easy to detect, preferably in Quality control aqueous solution, the concentration of phosphatidylserine is 0.1mg/mL-5mg/mL, is more preferably 0.1mg/mL-1.5mg/mL.
Further, in step (1), in the mixed solution of described methenyl choloride and methyl alcohol, the volume ratio of methenyl choloride and methyl alcohol is 1-10, is preferably 2.5-5.When extracting sample aqueous solution with the mixed solution of methenyl choloride and methyl alcohol, the mixed solution of described methenyl choloride and methyl alcohol and the volume ratio of sample aqueous solution are at least greater than 10.In addition, the time of extraction and temperature also have impact for ps percentage extraction, usually under 15 DEG C of-70 DEG C of conditions, extract 15min-5h, preferably under 35 DEG C of-50 DEG C of conditions, extract 30min-2h.
In one embodiment of the invention, what adopted by filtrate evaporate to dryness in step (1) is rotary evaporation.
Further, in step (2), the compound method of the mixed solution of described methenyl choloride, first alcohol and water is: the proportions being 1-3 according to methenyl choloride and the volume ratio of methyl alcohol becomes the mixed solution of methenyl choloride and methyl alcohol, and the proportions being then 1-3 according to methenyl choloride and the mixed solution of methyl alcohol and the volume ratio of water becomes the mixed solution of methenyl choloride, first alcohol and water.When extracting evaporate to dryness material with the mixed solution of methenyl choloride, first alcohol and water, as long as evaporate to dryness material can fully dissolve by the consumption of the mixed solution of methenyl choloride, first alcohol and water.
The present invention extracts the interfering material that effectively removes in food by two steps, composed the content detection of the phosphatidylserine that can complete in food by the high-efficient liquid phase color of routine.In order to make those skilled in the art implement the present invention better, provide a kind of preferred high-efficiency liquid chromatography method for detecting at this, specific as follows:
The testing conditions of high performance liquid chromatography is: adopt LiChrosphere100diol chromatographic column, mobile phase is by A phase and B phase composition, carry out gradient elution, flow velocity 1.5mL/min, column temperature 25 DEG C-30 DEG C, detects by evaporative light-scattering detector, wherein, described A phase is n-normal hexane: 2-propyl alcohol: acetic acid: the volume ratio of triethylamine is 820:170:10:0.8, B phase is 2-propyl alcohol: pure water: acetic acid: the volume ratio of triethylamine is 850:140:10:0.8.
Preferred condition of gradient elution is: 0-23min, and in mobile phase, the volumetric concentration of A phase rises to 40% from the volumetric concentration that 95% is down to 60%, B phase from 5%; 23-28min, in mobile phase, the volumetric concentration of A phase rises to 100% from the volumetric concentration that 60% is down to 0, B phase from 40%; 28-39min, in mobile phase, the volumetric concentration of A phase is down to 5% from the volumetric concentration that 0 rises to 95%, B phase from 100%; 39-50min, in mobile phase, the volumetric concentration of A phase is the volumetric concentration of 95%, B phase is 5%.
According to above-mentioned testing conditions, to the sample after pre-treatment, the lower floor's solution namely obtained in step (2), detects.Generalized case, also will use methenyl choloride or methanol constant volume before detection, obtains the peak area of phosphatidylserine in high performance liquid chromatography, is calculated the concentration of phosphatidylserine by typical curve correction equation.
According to detection method of the present invention, from protecting instrument and reducing the angle disturbed in test process, preferably this sample solution was filtered before the solution of described sample is detected, thus remove the insolubles in this sample solution.Described filtration can be various method well known to those skilled in the art, preferably adopts the solution of miillpore filter to described sample to filter.The aperture of described miillpore filter can be 0.1-0.45 μm, is preferably 0.2 μm.
Beneficial effect of the present invention is as follows:
Based on detection method of the present invention, the concentration of phosphatidylserine is good in 1.08-127.9 μ g/ μ L scope internal linear, can the content of stability analysis ps.And the method range of linearity is wider, be suitable for the analysis of the food of different ps addition; Method detects and is limited to 0.54 μ g/ μ L, and method is quantitatively limited to 1.8 μ g/ μ L.Method detection limit of the present invention is low, highly sensitive, can detect the food that with the addition of micro-ps; Method average recovery rate is between 97.0%-101.0%, and method accuracy is high.
Accompanying drawing explanation
The high-efficient liquid phase chromatogram of Fig. 1 phosphatidylserine standard items.
The high-efficient liquid phase chromatogram of sample detection in Fig. 2 embodiment 2.
Embodiment
In order to be illustrated more clearly in the present invention, below in conjunction with preferred embodiment, the present invention is described further.It will be appreciated by those skilled in the art that specifically described content is illustrative and nonrestrictive, should not limit the scope of the invention with this below.
Embodiment 1
Ps standard items being mixed with concentration is 50mg/100mL, i.e. 0.5 μ g/ μ L, according to chromatographic test strip part respectively sample introduction 10 μ L(ps content 5 μ g), 30 μ L(ps content 15 μ g), 50 μ L(ps content 25 μ g), 80 μ L(ps content 40 μ g), with ps content for horizontal ordinate, peak area is ordinate, the linear regression equation of trying to achieve is typical curve, and regression equation is y=4132.3x-2956.2, R2=0.9919.
HPLC analysis condition:
Phosphatidylserine (ps) standard model: sigma company, name of product: L-A-PHOSPHATIDYL-SERINE FROM SOYBEAN
Instrument: Shimatzu HPLC10VP series
Column type number: LiChrosphere100diol(Merck): 4mm(internal diameter) × 125mm(column length) (Merck), particle diameter: 5 μm
Pre-column: LiChrosphere diol pre cartridge
Column temperature: 35 DEG C
Detector parameters: ELSD2000, ALLTECH, U.S.A
Drift tube100℃
Nebulizer gas flow rate:2.0SLPM
Flow velocity: 1.5mL/min
Condition of gradient elution:
| Time | A mobile phase | B mobile phase |
| 0min | 95% | 5% |
| 23min | 60% | 40% |
| 28min | 0 | 100% |
| 39min | 95% | 5% |
| 50min | 95% | 5% |
Eluent A(2.5L):
N-normal hexane/2-propyl alcohol/acetic acid/triethylamine=820/170/10/0.8 (volume ratio)
Eluent B(2.5L):
2-propyl alcohol/pure water/acetic acid/triethylamine=850/140/10/0.8 (volume ratio)
Embodiment 2
Take 20g milk powder, dissolve with 40mL pure water, in solution, add the methenyl choloride of 950mL and the mixed solution of methyl alcohol, CHCl in this mixed solution
3: MeOH=1(volume ratio), under the condition of temperature 15 DEG C, extract 5h, complete soln is with after the membrane filtration of 0.2 μm, and rotary evaporated to dryness is dry.Then, with methenyl choloride, the mixed solution of methyl alcohol and pure water extracts (methenyl choloride to evaporate to dryness material, the preparation of methyl alcohol and pure water mixed solution: the ratio being 1 according to the volume ratio of methenyl choloride and methyl alcohol is made into the mixed solution of methenyl choloride and methyl alcohol, the pure water mixing of then getting this mixed solution 30mL and 30mL is made into methenyl choloride, the mixed solution of methyl alcohol and pure water), complete soln uses the membrane filtration of 0.2 μm again, filtrate stratification, be divided into upper and lower two layers of solution, with three filter methane or methanol solution by lower floor's solution constant volume to 50mL, for the detection analysis of HPLC.The actual addition of the phosphatidylserine in this milk powder is 150mg/100g, detects 142.5mg/100g.
HPLC analysis condition embodiment 1.
Embodiment 3
Take 20g bread, dissolve with 40mL pure water, in solution, add methenyl choloride and the methanol solution of 950mL, CHCl
3: MeOH=10(volume ratio), under the condition of temperature 70 C, extract 15min, complete soln is with after the membrane filtration of 0.2 μm, and rotary evaporated to dryness is dry.Then, with methenyl choloride, methyl alcohol, the mixed solution of pure water extracts (methenyl choloride to evaporate to dryness material, the preparation of methyl alcohol and pure water mixed solution: the ratio being 3 according to the volume ratio of methenyl choloride and methyl alcohol is made into the mixed solution of methenyl choloride and methyl alcohol, the pure water mixing of then getting this mixed solution 30mL and 10mL is made into methenyl choloride, the mixed solution of methyl alcohol and pure water), the complete soln membrane filtration of 0.2 μm, filtrate stratification, be divided into upper and lower two layers of solution, with three filter methane or methanol solution by lower floor's solution constant volume to 50mL, for the detection analysis of HPLC.The actual addition of the phosphatidylserine in this bread is 100mg/100g, detects 98.8mg/100g.
HPLC analysis condition is with embodiment 1.
Embodiment 4
Take 20g Yoghourt, dissolve with 40mL pure water, in solution, add methenyl choloride and the methanol solution of 950mL, CHCl
3: MeOH=5(volume ratio), under the condition of temperature 50 C, extract 1h, complete soln is with after the membrane filtration of 0.2 μm, and rotary evaporated to dryness is dry.Then, with methenyl choloride, the mixed solution of methyl alcohol and pure water extracts (methenyl choloride to evaporate to dryness material, the preparation of methyl alcohol and pure water mixed solution: the ratio being 2 according to the volume ratio of methenyl choloride and methyl alcohol is made into the mixed solution of methenyl choloride and methyl alcohol, the pure water mixing of then getting this mixed solution 40mL and 20mL is made into methenyl choloride, the mixed solution of methyl alcohol and pure water), the complete soln membrane filtration of 0.2 μm, filtrate stratification, be divided into upper and lower two layers of solution, with three filter methane or methanol solution by lower floor's solution constant volume to 50mL, for the detection analysis of HPLC.The actual addition of the phosphatidylserine in this milk powder is 120mg/100g, detects 119.3mg/100g.
HPLC analysis condition is with embodiment 1.
Embodiment 5
The milk powder product of testing the two kinds of commercially available ps of with the addition of selected carries out precision test.Process by the inventive method, each sample parallel operates 6 times, measures precision.The results are shown in Table 1.
Table 1 Precision test result
As can be seen from measurement result, RSD% < 2, the precision of illustration method is higher, and between different batches, testing result difference is very little.
Embodiment 6
Get the milk powder product that is not added ps raw material, respectively to wherein adding ps raw material, make the milk powder product that ps content is 50mg/100g, 60mg/100g, 80mg/100g, 100mg/100g, by the inventive method processing sample, often group is done 6 and is parallelly carried out recovery test, the results are shown in Table 2.
Table 2 recovery test result
Note: the milk powder product ps content background values of not adding ps raw material is 0mg/100g.
Can find from result, recovery RSD% < 2, illustrate that the inventive method recovery is high, show that ps does not almost lose in method processing procedure, method pre-treating technology is stablized.
Comparative example 1
Testing sample is 150mg/100g with the actual addition of the phosphatidylserine in this milk powder of embodiment 2(), the pre-treating method of sample only has extraction temperature different with extraction time (actual conditions is see table 3), by HPLC(analysis condition with embodiment 1) detect the addition analyzing ps in sample, result is as shown in table 3.
Table 3:
Comparative example 2
Testing sample is 120mg/100g with the actual addition of the phosphatidylserine in this milk powder of embodiment 4(), only methenyl choloride different with the volume ratio of methyl alcohol (actual conditions is see table 4) in the pre-treating method of sample, by HPLC(analysis condition with embodiment 1) detect the addition analyzing ps in sample, result is as shown in table 4.
Table 4:
Comparative example 3
The pre-treating method of testing sample and sample is different with the condition of embodiment 2, HPLC, and measurement result is: the actual addition of the phosphatidylserine in this milk powder is 150mg/100g, detects 130.5mg/100g.
HPLC analysis condition:
Standard model: sigma company, name of product: L-A-PHOSPHATIDYL-SERINE FROM SOYBEAN
Instrument: Shimatzu HPLC10VP series
Column type number: LiChrosphere100diol(Merck): 4 μm × 125mm(Merck)
Pre-column: LiChrosphere diol pre cartridge
Column temperature: 35 DEG C
Detector parameters: ELSD2000, ALLTECH, U.S.A
Drift tube100℃
Nebulizer gas flow rate:2.0SLPM
Flow velocity: 1.5mL/min
Condition of gradient elution:
| TIME | A mobile phase | B mobile phase |
| 0min | 95% | 5% |
| 23min | 40% | 60% |
| 28min | 0 | 100% |
| 39min | 95% | 5% |
| 50min | 95% | 5% |
Eluent A(2.5L):
N-normal hexane/2-propyl alcohol/acetic acid/triethylamine=820/170/10/0.8 (volume ratio)
Eluent B(2.5L):
2-propyl alcohol/pure water/acetic acid/triethylamine=850/140/10/0.8 (volume ratio)
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (3)
1. a detection method for phosphorus in food acyl serine content, is characterized in that, the method comprises the following steps:
(1) take food to be measured, be mixed with sample aqueous solution, extract with the mixed solution of methenyl choloride and methyl alcohol, then filter, by filtrate evaporate to dryness; Wherein, in the mixed solution of described methenyl choloride and methyl alcohol, the volume ratio of methenyl choloride and methyl alcohol is 1-10; The mixed solution of described methenyl choloride and methyl alcohol and the volume ratio of sample aqueous solution are greater than 10; Described extraction extracts 15min-5h under 15 DEG C of-70 DEG C of conditions;
(2) with the mixed solution of methenyl choloride, first alcohol and water, the evaporate to dryness material that step (1) obtains is extracted, then filter, filtrate stratification; Wherein, the compound method of the mixed solution of described methenyl choloride, first alcohol and water is: the proportions being 1-3 according to methenyl choloride and the volume ratio of methyl alcohol becomes the mixed solution of methenyl choloride and methyl alcohol, and the proportions being then 1-3 according to methenyl choloride and the mixed solution of methyl alcohol and the volume ratio of water becomes the mixed solution of methenyl choloride, first alcohol and water;
(3) take off layer solution and carry out high performance liquid chromatography detection; Wherein, the testing conditions of high performance liquid chromatography is: adopt LiChrosphere 100 diol chromatographic column, mobile phase is by A phase and B phase composition, carry out gradient elution, detect by evaporative light-scattering detector, wherein, described A phase is n-normal hexane: 2-propyl alcohol: acetic acid: triethylamine, volume ratio is 820:170:10:0.8, B phase is 2-propyl alcohol: pure water: acetic acid: triethylamine, and volume ratio is 850:140:10:0.8, and the condition of described gradient elution is: 0-23min, in mobile phase, the volumetric concentration of A phase rises to 40% from the volumetric concentration that 95% is down to 60%, B phase from 5%; 23-28min, in mobile phase, the volumetric concentration of A phase rises to 100% from the volumetric concentration that 60% is down to 0, B phase from 40%; 28-39min, in mobile phase, the volumetric concentration of A phase is down to 5% from the volumetric concentration that 0 rises to 95%, B phase from 100%; 39-50min, in mobile phase, the volumetric concentration of A phase is the volumetric concentration of 95%, B phase is 5%.
2. detection method according to claim 1, is characterized in that, in step (1), in the mixed solution of described methenyl choloride and methyl alcohol, the volume ratio of methenyl choloride and methyl alcohol is 2.5-5.
3. detection method according to claim 1, is characterized in that, in step (1), described extraction extracts 30min-2h under 35 DEG C of-50 DEG C of conditions.
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| CN105301144A (en) * | 2015-12-02 | 2016-02-03 | 烟台燕园科玛健康产业有限公司 | High-performance liquid chromatography of phosphatidylserine |
| CN107688073B (en) * | 2017-11-02 | 2020-12-04 | 威海百合生物技术股份有限公司 | Method for detecting content of phosphatidylserine |
| CN111721848A (en) * | 2019-03-21 | 2020-09-29 | 仙乐健康科技股份有限公司 | Method for measuring content of phosphatidylserine |
| CN110514776A (en) * | 2019-09-03 | 2019-11-29 | 中国水产科学研究院黄海水产研究所 | The detection method of phosphatide in a kind of antarctic krill oil |
| CN111855844B (en) * | 2020-07-02 | 2021-04-30 | 武汉迈特维尔生物科技有限公司 | Method for analyzing phosphatidylserine |
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| JP2003319793A (en) * | 2002-02-28 | 2003-11-11 | Nagase Chemtex Corp | Phospholipid base exchange method |
| US20090131368A1 (en) * | 2006-07-19 | 2009-05-21 | Su Chen | Mixtures of and methods of use for polyunsaturated fatty acid-containing phospholipids and alkyl ether phospholipids species |
| CN101319237A (en) * | 2008-07-11 | 2008-12-10 | 天津科技大学 | Method for catalysis synthesis of phosphatidylserine with phosphatidylserine synthetase |
| CN101818179A (en) * | 2010-04-28 | 2010-09-01 | 大连理工大学 | Method for preparing phosphatidylserine abundant in polyunsaturated fatty acid |
| CN102564825B (en) * | 2012-01-05 | 2014-01-08 | 上海海洋大学 | Method for preparing mixed phospholipid standard substance by using aquatic products and developing agent thereof |
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