CN107247051A - A kind of method of quick detection phospholipid in lipid - Google Patents
A kind of method of quick detection phospholipid in lipid Download PDFInfo
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- CN107247051A CN107247051A CN201710693081.1A CN201710693081A CN107247051A CN 107247051 A CN107247051 A CN 107247051A CN 201710693081 A CN201710693081 A CN 201710693081A CN 107247051 A CN107247051 A CN 107247051A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention discloses a kind of method of quick detection phospholipid in lipid, a, the preparation of color standards series：The grease of known different content of phospholipid is subjected to 280 DEG C of heating chromogenic reactions, color standards series is obtained；B, colorimetric detection：Oil sample containing phosphatide is subjected to 280 DEG C of heating chromogenic reactions, the color of solution is compared with color standards series, the concentration or concentration range of phosphatide in oil sample are determined using optical colorimetry sxemiquantitative.The present invention is a kind of method of quick detection phospholipid in lipid, and accurate judgement is quickly carried out to grease phosphorus content, determines oil product content of phospholipid height, reaches the purpose of Instructing manufacture technique adjustment, more effectively can carry out process control to the finished product oil quality produced；Also ensure that different quality oil products carry out a point tank storage；High phospholipid oil product can be directed to simultaneously, and the technique for using aquation after first adding citric acid solution instead reduces the content of phospholipid in lipid.
Description
Technical field
The invention belongs to phosphatide detection technique field, specifically, it is related to a kind of method of quick detection phospholipid in lipid.
Background technology
Because the different phospholipid in lipid contents of vegetable seed raw material have bigger difference, there is considerable influence to direct aquation dephosphorization technique.
Conventional (national standard) phosphatide detection method time is oversize, about 5 hours, it is impossible to actual production process is provided timely, instruct
The technical parameter of property.And because the freezing dewaxing technique of oil product is batch (-type), and phosphatide detection time is long, original inspection
Survey process, 1 order of classes or grades at school can only be detected to 1 pot of dewaxed oil, and 1 order of classes or grades at school has 3 pots of aquation oil to come out, it is impossible to every pot of oil
The phosphatide of product is detected that entering tank to product oil has hidden danger of quality.
The content of the invention
To solve above technical problem, it is an object of the invention to provide a kind of method of quick detection phospholipid in lipid,
The content of phospholipid in lipid is more rapidly and effectively determined, and can adapt to the oil product freezing dewaxing technique of batch (-type).
What the object of the invention was realized in：A kind of method of quick detection phospholipid in lipid, it is characterised in that：
A, color standards series preparation：The grease of known different content of phospholipid is subjected to 280 DEG C of heating chromogenic reactions,
Obtain color standards series；
B, colorimetric detection：Oil sample containing phosphatide is subjected to 280 DEG C of heating chromogenic reactions, by the color and colorimetric of solution
Standard series is compared, and the concentration or concentration range of phosphatide in oil sample are determined using optical colorimetry sxemiquantitative.
Further, the grease of different content of phospholipid carries out Accurate Determining phosphatide by molybdenum blue colorimetric method in above-mentioned steps a
Content.
Further, above-mentioned molybdenum blue colorimetric method is specially：By the grease containing phosphatide, the calcination together with zinc oxide, makes phosphorus
Organic compound is transformed into inorganic compound, is stayed in the form of phosphate (mainly trbasic zinc phosphate) in ash content, then acid adding dissolving,
Phosphate anion is acted on generation sodium phosphomolybdate with sodium molybdate, meet the complex compound molybdenum blue that sulphuric acid leaching is reduced into blueness, produce
The depth of blueness is directly proportional to the content of phosphorus, by test solution and standard liquid colorimetric assay under the same conditions, you can measure phosphorus
Content, so as to calculate the content for obtaining phosphatide.
Further, 280 DEG C of heating chromogenic reactions are specially in above-mentioned steps a and b：Uniform heating, and 16~
Grease temperature is set to rise to 280 DEG C, chromogenic reaction in 18min.
Beneficial effect：
The present invention is a kind of method of quick detection phospholipid in lipid, wherein 280 DEG C of heat run methods are in itself simply to oil
Content of phospholipid carries out qualitative analysis in fat, and this method by national standard detect and obtains accurate to different content of phospholipid oil products first
After numerical value, then correspond oil product 280 DEG C of heat runs of progress of different content of phospholipid, observation color and luster (high phospholipid and low-phosphorous fat
Color and luster is had any different after oil product heat run), the color standards for making different content of phospholipid is serial (colorimetric cylinder sample).Thus can
Quickly judge phospholipid in lipid content in which scope by 280 DEG C of heat runs in process of production.
And the use of quick phosphatide detection method, accurate to the progress of grease phosphorus content in 30 minutes it can sentence
It is fixed, oil product content of phospholipid height is determined, the purpose of Instructing manufacture technique adjustment is reached, finished product oil product that more can effectively to producing
Matter carries out process control, moreover it is possible to ensures that different quality (high phospholipid and low-phosphorous fatty oil product) oil products carry out a point tank storage, both rationally had
The oil product to different qualities of effect makes full use of, and in turn ensures that oil quality.High phospholipid oil product can be directed to simultaneously, used instead
The technique of aquation after first adding citric acid solution, reduces the content of phospholipid in lipid.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1：
First, molybdenum blue colorimetric method determines phospholipid in lipid content：
1.1 instruments and apparatus
Porcelain crucible；Ultra-violet and visible spectrophotometer (721 or UV2401PC)；50ml colorimetric cylinders with plug；Pipette (5,
10m1)；Electric furnace；High temperature furnace；Volumetric flask (100,500,1000m1)；Surface plate；Beaker；Graduated cylinder；Thermostat water bath；Funnel；Earthenware
Crucible is clamped；Reagent bottle etc..
1.2 reagent
50% potassium hydroxide solution, hydrochloric acid, sulfuric acid, zinc oxide, filter paper；
0.015% sulphuric acid leaching solution：1. 0.15g sulphuric acid leachings solution is weighed in 250ml flasks, plus distilled water
200ml, is allowed to dissolve with glass bar；2. go in 1000ml volumetric flasks, capacity is all gone to 3 contents of distilled water flushing
Shaken up at bottle 3/4；3. constant volume graduation mark shakes up, and goes to standby in narrow-mouthed bottle；
2.5% sodium molybdate dilution heat of sulfuric acid：Measure in 140ml sulfuric acid injection 300ml water, shake up, be cooled to room temperature, add
500m1 is added water to after 12.5g sodium molybdates, dissolving, is shaken up, 24h is stood standby.
Phosphorus standard liquid：Anhydrous potassium dihydrogen phosphate 0.4391g is weighed to be dissolved in 1000m1 water, it is (phosphorous as l liquid
0.1mg/ml), No. 1 liquid lOml is drawn, lOOml, phosphorous 0.01mg/ m1 is diluted with water to, as No. 2 liquid, colorimetric is used.
1.3 operating method
1.3.1 standard curve is drawn：6 50m1 colorimetric cylinders are taken, 0,1,2,4,6,8 five number is weaved into, according to number order
It is injected separately into No. 2 liquid 0,1,2,4,6,8m1 of phosphorus standard, then adds water 10,9,8,6,4,2m1 respectively in order.Then it is interior by all means to 6
Respectively plus 0.015% sulphuric acid leaching solution 8.0ml；Respectively plus sodium molybdate dilution heat of sulfuric acid 2.Oml, jump a queue, shake up.Plug is removed, by 6 by all means
10min is heated in the water-bath for being placed in boiling, taking-up is cooled to room temperature, is diluted with water to 50m1, fully shakes up, through 10min
Afterwards, 1cm liquid baths are used under wavelength 650nm with UV2401PC (or 721) spectrophotometers, zero point is adjusted with water, determined disappear respectively
Change value.Using digestion value as ordinate, with phosphorus amount (0.00,0.01,0.02,0.04,0.06,0.08mg) for abscissa draw mark
Directrix curve.
1.3.2 test solution is prepared：Sample about 10g (accurately to 0.00lg), plus zinc oxide 0.5g are weighed with crucible, first in electricity
Charing is heated on stove, calcination in 550~600 DEG C of high temperature furnace is then fed into and is extremely ashed (white), calcination time about 2h takes out earthenware
Crucible is cooled to room temperature, with hot hydrochloric acid (1：1) 10m1 dissolves ash content, and heats micro-boiling 5min, and lysate filtering injection 100ml is held
In measuring bottle, with hot water injection's crucible and filter paper, after filtrate is cooled to room temperature, appearance is neutralized to 50% potassium hydroxide solution muddy
Turbid, hydrochloric acid, which is slowly added dropwise, to be made after zinc oxide precipitate whole dissolving, then drips 2 drops, is finally diluted with water to scale, is shaken up.
1.3.3 colorimetric：With in pipette, extract test solution 10ml injection 50ml colorimetric cylinders, 0.015% sulphuric acid leaching is added
8.Oml, plus 2.Oml sodium molybdate dilution heat of sulfuric acid, jump a queue, shake up.Plug is removed, colorimetric cylinder is placed in the water-bath of boiling and heated
LOmin, taking-up is cooled to room temperature, is diluted with water to 50ml, fully shakes up, after lOmin, with UV2401PC (or 721) light splitting
Photometer uses 1cm liquid baths under wavelength 650nm, and zero point is adjusted with water, determines extinction value.
1.4 results are calculated:
1.4.1 according to the extinction value of test solution, phosphorus amount (P) is checked in from standard curve.
It is calculated as follows phosphorous in oil：Phosphorous (ppm)=P ÷ W × 104
In formula：The phosphorus content that P----- standard curves are checked in, mg；
W----- sample weights, g.
1.4.2 content of phospholipid is calculated as follows：
Phosphatide (%)=(P × V2/V1)×26.31×100/(W×1000)
In formula：The phosphorus amount that P----- standard curves are checked in, mg；
V2--- the volume diluted after sample ashing, ml；
V1--- the test solution volume taken during colorimetric, ml；
26.31 --- milligram number of the every milligram of phosphorus equivalent to phosphatide；
W --- sample weight, g.
Double result of the test tolerances are no more than 0.04%, ask its average, as measurement result.Measurement result takes decimal point
Second afterwards.
2nd, the preparation of color standards series：The grease for the known different content of phospholipid that said determination is gone out is heated,
Grease temperature is set to rise to 280 DEG C in 16~18min, chromogenic reaction obtains color standards series；
3rd, colorimetric detection：Oil sample containing phosphatide is heated, grease temperature is risen to 280 in 16~18min
DEG C, the color of solution is compared by chromogenic reaction with color standards series, and grease sample is determined using optical colorimetry sxemiquantitative
The concentration or concentration range of phosphatide in product.
Finally it should be noted that foregoing description is only the preferred embodiments of the present invention, the ordinary skill people of this area
Member on the premise of without prejudice to present inventive concept and claim, can make table as multiple types under the enlightenment of the present invention
Show, such conversion is each fallen within protection scope of the present invention.
Claims (4)
1. a kind of method of quick detection phospholipid in lipid, it is characterised in that：
A, color standards series preparation：The grease of known different content of phospholipid is subjected to 280 DEG C of heating chromogenic reactions, obtained
Color standards series；
B, colorimetric detection：Oil sample containing phosphatide is subjected to 280 DEG C of heating chromogenic reactions, by the color and color standards of solution
Series is compared, and the concentration or concentration range of phosphatide in oil sample are determined using optical colorimetry sxemiquantitative.
2. a kind of method of quick detection phospholipid in lipid according to claim 1, it is characterised in that：In the step a
The grease of different content of phospholipid passes through molybdenum blue colorimetric method Accurate Determining content of phospholipid.
3. a kind of method of quick detection phospholipid in lipid according to claim 2, it is characterised in that the molybdenum blue colorimetric
Method is specially：The calcination together with zinc oxide by the grease containing phosphatide, then acid adding dissolving, meet sulphuric acid leaching and are reduced into blueness
Complex compound molybdenum blue, the depth for producing blueness is directly proportional to the content of phosphorus, by test solution and standard liquid colorimetric under the same conditions
It is quantitative, you can the content of phosphorus to be measured, so as to calculate the content for obtaining phosphatide.
4. a kind of method of quick detection phospholipid in lipid according to claim 1, it is characterised in that the step a and b
In 280 DEG C heating chromogenic reactions be specially：Uniform heating, and grease temperature is risen to 280 DEG C in 16~18min, colour developing is anti-
Should.
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| CN201710693081.1A CN107247051A (en) | 2017-08-14 | 2017-08-14 | A kind of method of quick detection phospholipid in lipid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181143A (en) * | 2017-12-12 | 2018-06-19 | 山东金胜粮油集团有限公司 | A kind of method of quick detection grease phosphorus content |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175672A (en) * | 2011-01-06 | 2011-09-07 | 西北大学 | Method for measuring phospholipid in lipid |
| CN103969248A (en) * | 2013-01-30 | 2014-08-06 | 中国石油天然气股份有限公司 | Microwave digestion method for the determination of phosphorus / phosphatide content in oil |
-
2017
- 2017-08-14 CN CN201710693081.1A patent/CN107247051A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175672A (en) * | 2011-01-06 | 2011-09-07 | 西北大学 | Method for measuring phospholipid in lipid |
| CN103969248A (en) * | 2013-01-30 | 2014-08-06 | 中国石油天然气股份有限公司 | Microwave digestion method for the determination of phosphorus / phosphatide content in oil |
Non-Patent Citations (2)
| Title |
|---|
| 王肇慈: "《粮油食品品质分析》", 30 April 2000, 中国轻工业出版社 * |
| 邵秀芝等: "《食品化学实验》", 31 December 2013, 郑州大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181143A (en) * | 2017-12-12 | 2018-06-19 | 山东金胜粮油集团有限公司 | A kind of method of quick detection grease phosphorus content |
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Application publication date: 20171013 |