CN105950285A - Extraction method for fat in dairy product and determination method for peroxide value of fat - Google Patents
Extraction method for fat in dairy product and determination method for peroxide value of fat Download PDFInfo
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- CN105950285A CN105950285A CN201610252265.XA CN201610252265A CN105950285A CN 105950285 A CN105950285 A CN 105950285A CN 201610252265 A CN201610252265 A CN 201610252265A CN 105950285 A CN105950285 A CN 105950285A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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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
- G01N1/34—Purifying; Cleaning
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
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Abstract
The invention discloses an extraction method for fat in a dairy product, a determination method for the peroxide value of the fat in the dairy product, a determination method for the peroxide value of fat in a viscous dairy product, and a determination method for the peroxide value of fat in milk powder. The extraction method for the fat in the dairy product comprises the following steps: subjecting the dairy product and ethanol to primary mixing so as to obtain first mixed liquor; subjecting the first mixed liquor and water to secondary mixing so as to obtain second mixed liquor; subjecting the second mixed liquor and petroleum ether to tertiary mixing and carrying out standing so as to obtain third mixed liquor; and carrying out filtering and rotary evaporation on the third mixed liquor so as to obtain fat. With the extraction method provided by the invention, fat in the dairy product can be thoroughly extracted.
Description
Technical field
The present invention relates to field of food.In particular it relates to extracting method fatty in milk product and fatty peroxide value
Assay method.More particularly it relates to peroxide fatty in the extracting method of fat, mensuration milk product in milk product
The side of the peroxide value of fat in the method for change value, the method measuring the peroxide value of fat in thickness milk product and mensuration milk powder
Method.
Background technology
Fat is one of main component in milk product, by extracting fat and detecting it, as measured acid value or peroxide
Change value, to weigh quality of dairy products.
But, in current milk product, the extracting method of fat still haves much room for improvement.
Summary of the invention
It is contemplated that at least solve one of technical problem present in prior art.To this end, it is an object of the present invention to
The extracting method of fat in milk product is provided, measures in the method for the peroxide value of fat in milk product, mensuration thickness milk product
The method of the peroxide value of fat in the method for the peroxide value of fat and mensuration milk powder.Utilize fat in the milk product of the present invention
Extracting method can fully extract fat, and measure the peroxide value of fat in milk product further with the present invention
Method measures the peroxide value of fat in milk product exactly.
It should be noted that the present invention is following discovery based on inventor and completes:
Owing to containing protein and/or the additive such as stabilizer, thickening agent in milk product, significant quantities of fat is embedded by it.If it is straight
Connect and utilize petroleum ether to soak milk product, be difficult to by fat-extraction out.
In view of this, the present inventor finds through great many of experiments, is mixed with ethanol by milk product in advance, it is possible to
Make protein and/or additive precipitation, thus discharge fat, and then petroleum ether can be made full use of by fat-extraction out.
To this end, in a first aspect of the present invention, the present invention proposes the extracting method of fat in a kind of milk product.According to this
Bright embodiment, described method includes: milk product and ethanol are carried out the first mixed processing, obtains the first mixed liquor;By institute
State the first mixed liquor and carry out the second mixed processing with water, obtain the second mixed liquor;Described second mixed liquor is carried out with petroleum ether
3rd mixing and standing process, and obtain the 3rd mixed liquor;And carry out filtering and revolve steaming process by described 3rd mixed liquor, with
Just fat is obtained.Inventor is it was unexpectedly observed that mix milk product with ethanol in advance, it is possible to make protein or additive
Etc. species precipitate, and fat can't be with species precipitate such as protein such that it is able to be effectively prevented protein and/or additive
Petroleum ether extraction fat is interfered.Thus, the extracting method energy of fat in milk product according to embodiments of the present invention is utilized
Enough fully extract fat.
According to embodiments of the invention, in above-mentioned milk product, the extracting method of fat can also have a following additional technical feature:
According to embodiments of the invention, described milk product is milk powder, and based on 1 gram of described milk powder, the volume of described ethanol is 3~6
ML, preferably 5mL, the volume of described water is 0.5~3mL, preferably 1mL, and the volume of described petroleum ether is 3~7mL,
Preferably 5mL.Thus, the extracting method of fat in milk product according to embodiments of the present invention is utilized can fully to extract fat.
According to embodiments of the invention, described milk product is thickness milk product, based on 1 gram of described thickness milk product, described second
The volume of alcohol is 0.5~2mL, preferably 0.5mL, and the volume of described water is 0.1~1mL, preferably 0.1mL, described petroleum ether
Volume be 2~6mL, preferably 2mL.Thus, the extracting method of fat in milk product according to embodiments of the present invention is utilized
Can fully extract fat.
According to embodiments of the invention, described thickness milk product is Yoghourt.
According to embodiments of the invention, the time of described first mixed processing is 1~5 minute, preferably 1 minute.Thus, profit
Fat can be fully extracted with the extracting method of fat in milk product according to embodiments of the present invention.
According to embodiments of the invention, the time of described second mixed processing is 0.5~2 minute, preferably 0.5 minute.Thus,
The extracting method of fat in milk product according to embodiments of the present invention is utilized can fully to extract fat.
According to embodiments of the invention, the time of described 3rd mixed processing is 1~5 minute, preferably 1 minute.Thus, profit
Fat can be fully extracted with the extracting method of fat in milk product according to embodiments of the present invention.
According to embodiments of the invention, the time that described standing processes is 8~18 hours, preferably 12 hours.Thus, utilize
In milk product according to embodiments of the present invention, the extracting method of fat can fully extract fat.
In a second aspect of the present invention, the present invention proposes a kind of method measuring peroxide value fatty in milk product.According to
Embodiments of the invention, described method includes: extract fat according to the extracting method of fat in milk product described above;
And use known method to measure the peroxide value of described fat.Thus, mensuration milk product according to embodiments of the present invention is utilized
The method of the peroxide value of middle fat can measure the peroxide value of fat in milk product exactly.
It will be appreciated to those of skill in the art that above for the feature and excellent described by the extracting method of fat in milk product
Point, the method being equally applicable in this mensuration milk product the peroxide value of fat, do not repeat them here.
In a third aspect of the present invention, the present invention proposes a kind of method measuring peroxide value fatty in thickness milk product.
According to embodiments of the invention, described method includes: thickness milk product described in 200g is poured in container by (1), adds 100mL
Ethanol solution, stirs 1 minute with Glass rod;(2) mixed liquor obtained by step (1) is poured in separatory funnel, add
20mL water, lid lid rocks 0.5 minute, adds petroleum ether 400mL, and lid lid rocks 1 minute, after standing 12 hours,
Ether layer is released to be covered with the funnel of filter paper and gauze from separatory funnel end opening, and in collection filtrate to rotary evaporation bottle, rotation is steamed
Evaporate solvent, obtain fat;(3) weigh described in 2-5g fatty in iodine flask, add 50mL isobutyltrimethylmethane .-glacial acetic acid and mix
Closing liquid (2:3 mixing), shaking flask makes lipid solubilization, adds 1mL saturated solution of potassium iodide and (is added 10mL by 14g potassium iodide
Ionized water is mixed to get), close the lid, shake up, dark place reaction 5min (period shakes once again), take out iodine flask and add 100mL
Deionized water, adds starch indicator (1g/100mL), titrates with sodium thiosulfate standard solution (0.002mol/L), with
Time do blank assay;(4) peroxide value of fat is calculated in described thickness milk product according to the following formula:
X2=X1× 78.8,
In formula: (1) X1: fatty peroxide value in sample, unit is gram every hectogram (g/100g);(2)X2: fat in sample
Peroxide value, unit is milliequivalent every kilogram (meq/kg);(3)V1: sample consumes sodium thiosulfate standard titration solution
Volume, unit is milliliter (mL);(4)V2: blank assay consumes the volume of sodium thiosulfate standard titration solution, unit
For milliliter (mL);(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;(6) M: sample mass,
Unit is gram (g);(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.Thus, the peroxide value of fat in mensuration thickness milk product according to embodiments of the present invention is utilized
Method can measure the peroxide value of fat in milk product exactly.
In a fourth aspect of the present invention, the present invention proposes a kind of method measuring peroxide value fatty in milk powder, its feature
It is, including: (1) adds milk powder described in 30g and ethanol solution (95%) 150mL in container, shakes 1 minute,
Add water 30mL, shake 0.5 minute;(2) mixed liquor obtained by step (1) is poured in separatory funnel, add stone
Oil ether 150mL, shakes 1 minute, then stands 12 hours, ether layer is released to be covered with the leakage of filter paper from separatory funnel end opening
In bucket, in collection filtrate to rotary evaporation bottle, rotation steaming evaporates solvent, obtains fat;(3) weigh described in 2-5g fat in
In iodine flask, adding 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor (2:3 mixing), shaking flask makes lipid solubilization, adds 1mL saturated
Liquor kalii iodide (is added 10mL deionized water by 14g potassium iodide to be mixed to get), closes the lid, shakes up, dark place reaction 5min
(period shakes once again), takes out iodine flask and adds 100mL deionized water, add starch indicator (1g/100mL), use sulfur
Sodium thiosulfate standard solution (0.002mol/L) titrates, and does blank assay simultaneously;(4) described thickness is calculated according to the following formula
The peroxide value of fat in milk product:
X2=X1× 78.8,
In formula: (1) X1: the peroxide value of fat in sample, unit is gram every hectogram (g/100g);(2)X2: fat in sample
Peroxide value, unit is milliequivalent every kilogram (meq/kg);(3)V1: sample consumes sodium thiosulfate standard titration solution
Volume, unit is milliliter (mL);(4)V2: blank assay consumes the volume of sodium thiosulfate standard titration solution, single
Position is milliliter (mL);(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;(6) M: sample mass,
Unit is gram (g);(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.Thus, in utilization mensuration milk powder according to embodiments of the present invention, the method for fatty peroxide value can
Measure the peroxide value of fat in milk product exactly.
The additional aspect of the present invention and advantage will part be given in the following description, and part will become bright from the following description
Aobvious, or recognized by the practice of the present invention.
Detailed description of the invention
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining the present invention,
And be not considered as limiting the invention.
It should be noted that term " first ", " second " are only used for describing purpose, and it is not intended that instruction or hint relatively
Importance or the implicit quantity indicating indicated technical characteristic.Thus, define " first ", " second " feature permissible
Express or implicitly include one or more this feature.Further, in describing the invention, unless otherwise saying
Bright, " multiple " are meant that two or more.
The present invention proposes the extracting method of fat in milk product and measures the method for fatty peroxide value in milk product, below will
It is described in greater detail respectively.
The extracting method of fat in milk product
In a first aspect of the present invention, the present invention proposes the extracting method of fat in a kind of milk product.Reality according to the present invention
Executing example, the method includes: milk product and ethanol are carried out the first mixed processing, obtains the first mixed liquor;Mix described first
Close liquid and carry out the second mixed processing with water, obtain the second mixed liquor;With petroleum ether, described second mixed liquor is carried out the 3rd mix
And standing processes, obtain the 3rd mixed liquor;And carry out filtering and revolve steaming process by described 3rd mixed liquor, in order to obtain fat
Fat.Inventor is it was unexpectedly observed that mix milk product with ethanol in advance, it is possible to make protein and/or additive precipitation,
And fat can't be with species precipitate such as protein such that it is able to be effectively prevented the materials such as protein to Petroleum ether extraction fat
Interfere.Thus, the extracting method of fat in milk product according to embodiments of the present invention is utilized can fully to extract fat.
According to embodiments of the invention, milk product is milk powder, and based on 1 gram of milk powder, the volume of ethanol is 3~6mL, preferably 5mL,
The volume of water is 0.5~3mL, preferably 1mL, and the volume of petroleum ether is 3~7mL, preferably 5mL.Reality according to the present invention
Executing example, milk product is thickness milk product, and based on 1 gram of thickness milk product, the volume of ethanol is 0.5~2mL, preferably 0.5mL,
The volume of water is 0.1~1mL, preferably 0.1mL, and the volume of petroleum ether is 2~6mL, preferably 2mL.
Owing in milk powder, protein and fat content are higher, and containing the material such as thickening agent, stabilizer in thickness milk product, lead
The addition of ethanol, water and petroleum ether required for causing the fat in extraction milk powder and thickness milk product is different.
Inventor obtains above-mentioned optimum weight percent through great many of experiments optimization.If the addition of ethanol is less, will be unable to make completely
The species precipitate such as protein, are still partially embedded fat, thus cause petroleum ether thoroughly by fat-extraction, and then cannot to make
Obtain extraction ratio on the low side.It is to make water-soluble substances be substantially soluble in water by the purpose that the first mixed liquor mixes with water, to avoid rear
Continuous extraction interferes.If the addition of water is less, it is impossible to be completely dissolved water-soluble substances, it will cause two phase stratification to be failed to understand
Aobvious, if the addition of petroleum ether is very few, it is impossible to extract fat completely, cause extraction ratio on the low side.Thus, utilize according to this
In the milk product of inventive embodiments, the extracting method of fat can fully extract fat.
It will be appreciated to those of skill in the art that " thickness milk product " refers to that viscosity is higher than the milk product of liquid plain chocolate, right
The kind of thickness milk product does not make considered critical.According to a particular embodiment of the invention, thickness milk product is Yoghourt.
According to embodiments of the invention, the time of the first mixed processing is 1~5 minute, preferably 1 minute.First mixed processing
Purpose be to make milk product be sufficiently mixed with ethanol so that species precipitate such as protein, to discharge the fat of its embedding.
If incorporation time is too short, will be unable to the materials such as abundant precipitating proteins, thus cause its fat embedded cannot be carried by petroleum ether
Take out, and then cause extraction ratio to reduce.Thus, the extracting method energy of fat in milk product according to embodiments of the present invention is utilized
Enough fully extract fat.
According to embodiments of the invention, the time of the second mixed processing is 0.5~2 minute, preferably 0.5 minute.At second mixing
The purpose of reason is to make the first mixed liquor be sufficiently mixed with water, so that the water-soluble substances in the first mixed liquor is completely dissolved in water,
To prevent it from disturbing subsequent experimental, cause extraction ratio higher.If incorporation time is shorter, it is impossible to be completely dissolved water-soluble substances,
The extraction ratio that will cause fat is higher.Thus, the extracting method energy of fat in milk product according to embodiments of the present invention is utilized
Enough fully extract fat.
According to embodiments of the invention, the time of the 3rd mixed processing is 1~5 minute, preferably 1 minute.3rd mixed processing
Purpose be to make petroleum ether fully mix with the fat in the second mixed liquor to contact.If incorporation time is too short, it is impossible to extract completely
Go out fat, cause extraction ratio on the low side.Thus, in utilization milk product according to embodiments of the present invention, the extracting method of fat can
Fully extract fat.
According to embodiments of the invention, the time that standing processes is 8~18 hours, preferably 12 hours.The purpose that standing processes
It is to make petroleum ether fully extract fat, and lamination significantly can be realized.Thus, utilize according to embodiments of the present invention
In milk product, the extracting method of fat can fully extract fat.
Measure the method for the peroxide value of fat in milk product
In a second aspect of the present invention, the present invention proposes a kind of method measuring peroxide value fatty in milk product.According to
Embodiments of the invention, described method includes: extract fat according to the extracting method of fat in milk product described above;
And use known method to measure the peroxide value of described fat.Thus, mensuration milk product according to embodiments of the present invention is utilized
The method of the peroxide value of middle fat can measure the peroxide value of fat in milk product exactly.
According to a particular embodiment of the invention, the concrete operations of " known method " are as follows:
Weigh 2-5g extract fat in iodine flask, add 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor (2:3 mixing), cover
Cap flasks makes lipid solubilization, adds 1mL saturated solution of potassium iodide (being added 10mL deionized water by 14g potassium iodide to prepare),
Close the lid, shake up, dark place reaction 3-5min (the example reaction time keeps consistent), it is subsequently adding 100mL deionization
Water, adds starch indicator (1g/100mL), titrates with sodium thiosulfate standard solution (0.002mol/L), does sky simultaneously
White test.Result of calculation:
X2=X1× 78.8,
In formula:
(1)X1: the peroxide value of fat in sample, unit is gram every hectogram (g/100g);(2)X2: the peroxide of fat in sample
Change value, unit is milliequivalent every kilogram (meq/kg);(3)V1: sample consumes the volume of sodium thiosulfate standard titration solution,
Unit is milliliter (mL);(4)V2: consuming the volume of sodium thiosulfate standard titration solution in blank assay, unit is milliliter
(mL);(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;(6) M: sample mass, unit is
Gram (g);(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;(8) 78.8:
Conversion factor.
It will be appreciated to those of skill in the art that above for the feature and excellent described by the extracting method of fat in milk product
Point, the method being equally applicable in this mensuration milk product the peroxide value of fat, do not repeat them here.
It addition, the present invention proposes a kind of method measuring peroxide value fatty in thickness milk product.Reality according to the present invention
Executing example, described method includes: thickness milk product described in 200g is poured in container by (1), adds 100mL ethanol solution,
Stir 1 minute with Glass rod;(2) mixed liquor obtained by step (1) is poured in separatory funnel, adds 20mL water,
Lid lid rocks 0.5 minute, adds petroleum ether 400mL, and lid lid rocks 1 minute, after standing 12 hours, ether layer from dividing
Liquid funnel end opening is released to be covered with in the funnel of filter paper and gauze, and in collection filtrate to rotary evaporation bottle, rotation steaming evaporates solvent,
Obtain fat;(3) weighing described in 2-5g fatty in iodine flask, (2:3 mixes to add 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor
Close), shaking flask makes lipid solubilization, adds 1mL saturated solution of potassium iodide and (is added the mixing of 10mL deionized water by 14g potassium iodide
Obtain), close the lid, shake up, dark place reaction 5min (period shakes once again), take out iodine flask and add 100mL deionization
Water, adds starch indicator (1g/100mL), titrates with sodium thiosulfate standard solution (0.002mol/L), does sky simultaneously
White test;(4) peroxide value of fat is calculated in described thickness milk product according to the following formula:
X2=X1× 78.8,
In formula: (1) X1: the peroxide value of fat in sample, unit is gram every hectogram (g/100g);(2)X2: fat in sample
Peroxide value, unit is milliequivalent every kilogram (meq/kg);(3)V1: sample consumes sodium thiosulfate standard titration solution
Volume, unit is milliliter (mL);(4)V2: blank assay consumes the volume of sodium thiosulfate standard titration solution, single
Position is milliliter (mL);(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;(6) M: sample mass,
Unit is gram (g);(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.Thus, the peroxide value of fat in mensuration thickness milk product according to embodiments of the present invention is utilized
Method can measure the peroxide value of fat in milk product exactly.
Additionally, the invention allows for a kind of method measuring peroxide value fatty in milk powder.According to embodiments of the invention,
Described method includes: (1) adds milk powder described in 30g and ethanol solution (95%) 150mL in container, shakes 1 minute,
Add water 30mL, shake 0.5 minute;(2) mixed liquor obtained by step (1) is poured in separatory funnel, adds stone
Oil ether 150mL, shakes 1 minute, then stands 12 hours, ether layer is released to be covered with the leakage of filter paper from separatory funnel end opening
In bucket, in collection filtrate to rotary evaporation bottle, rotation steaming evaporates solvent, obtains fat;(3) weigh described in 2-5g fat in
In iodine flask, adding 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor (2:3 mixing), shaking flask makes lipid solubilization, adds 1mL saturated
Liquor kalii iodide (is added 10mL deionized water by 14g potassium iodide to be mixed to get), closes the lid, shakes up, dark place reaction 5min
(period shakes once again), takes out iodine flask and adds 100mL deionized water, add starch indicator (1g/100mL), use sulfur
Sodium thiosulfate standard solution (0.002mol/L) titrates, and does blank assay simultaneously;(4) described thickness is calculated according to the following formula
The peroxide value of fat in milk product:
X2=X1× 78.8,
In formula: (1) X1: the peroxide value of fat in sample, unit is gram every hectogram (g/100g);(2)X2: fat in sample
Peroxide value, unit is milliequivalent every kilogram (meq/kg);(3)V1: sample consumes sodium thiosulfate standard titration solution
Volume, unit is milliliter (mL);(4)V2: blank assay consumes the volume of sodium thiosulfate standard titration solution, single
Position is milliliter (mL);(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;(6) M: sample mass,
Unit is gram (g);(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.Thus, the method energy measuring peroxide value fatty in milk powder according to embodiments of the present invention is utilized
The peroxide value of fat in enough milk product of mensuration exactly.
Below in conjunction with embodiment, the solution of the present invention is explained.It will be understood to those of skill in the art that following enforcement
Example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted concrete technology or condition in embodiment,
According to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or instrument are not noted
Bright production firm person, be can by city available from conventional products.
Embodiment 1
In this embodiment, the fat in milk powder is extracted in following manner:
(1) in container, add 30g powdered milk sample and ethanol solution (95%) 150mL, shake 1 minute, add water 30mL,
Shake 0.5 minute;
(2) mixed liquor obtained by step (1) is poured in separatory funnel, adds petroleum ether 150mL, shakes 1 minute,
Then stand 12 hours, ether layer is released to be covered with the funnel of filter paper from separatory funnel end opening, collect filtrate to rotary evaporation
In Ping, rotation steaming evaporates solvent, obtains fat.
Embodiment 2
In this embodiment, the fat in Yoghourt is extracted in following manner:
(1) 200g Yoghourt is poured in container, add 100mL ethanol solution, stir 1 minute with Glass rod;
(2) pouring in separatory funnel by the mixed liquor obtained by step (1), add 20mL water, lid lid rocks 0.5 minute,
Adding petroleum ether 400mL, lid lid rocks 1 minute, after standing 12 hours, ether layer is released to paving from separatory funnel end opening
Having in the funnel of filter paper and gauze, in collection filtrate to rotary evaporation bottle, rotation steaming evaporates solvent, obtains fat.
Comparative example 1
Extracting fat in milk powder according to the method for embodiment 1, difference is, in step (1), directly by milk powder and water
Mix.
Comparative example 2
Extracting fat in Yoghourt according to the method for embodiment 2, difference is, in step (1), directly by Yoghourt and water
Mix.
Comparative example 3
Extracting fat in milk powder according to the method for embodiment 1, difference is, in step (1), the addition of ethanol is
50mL。
Comparative example 4
Extracting fat in milk powder according to the method for embodiment 1, difference is, in step (1), and the addition of petroleum ether
For 50mL.
Table 1 give embodiment 1,2, the quality of fat obtained by comparative example 1~4, it can be seen that compared to comparative example
1~4, can fully extract fat from milk product according to the method for embodiment 1 and 2, obtained fat is more.
Table 1 fat-extraction phenomenon
Embodiment 3
In this embodiment, the peroxide value of fat in milk powder is measured in following manner.
(1) fat is extracted according to the method for embodiment 1;
(2) weigh 2-5g extract fat in iodine flask, add 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor (2:3 mixing),
Shaking flask makes lipid solubilization, adds 1mL saturated solution of potassium iodide (being added 10mL deionized water by 14g potassium iodide to be mixed to get),
Close the lid, shake up, dark place reaction 5min (period shakes once again), take out iodine flask and add 100mL deionized water, add
Enter starch indicator (1g/100mL), titrate with sodium thiosulfate standard solution (0.002mol/L), do blank assay simultaneously.
Calculate the peroxide value of milk powder according to the following formula:
X2=X1×78.8
In formula:
(1)X1: the peroxide value of sample, unit is gram every hectogram (g/100g);
(2)X2: the peroxide value of sample, unit is milliequivalent every kilogram (meq/kg);
(3)V1: sample consumes the volume of sodium thiosulfate standard titration solution, and unit is milliliter (mL);
(4)V2: consuming the volume of sodium thiosulfate standard titration solution in blank assay, unit is milliliter (mL)
(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;
(6) M: sample mass, unit is gram (g);
(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.
Embodiment 4
In this embodiment, measuring the peroxide value of Yoghourt according to the method for embodiment 3, difference is,
In step (1), extract fat according to the method for embodiment 2.
Table 2 gives the peroxide value recorded according to the method for embodiment 3 and 4.It can be seen that according to the method for the present invention
The peroxide value of fat in milk product can be determined exactly.
Table 2 determination of POV
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " concrete example ",
Or specific features, structure, material or the feature bag that the description of " some examples " etc. means to combine this embodiment or example describes
It is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term necessarily
It is directed to identical embodiment or example.And, the specific features of description, structure, material or feature can be arbitrary
Individual or multiple embodiment or example combine in an appropriate manner.Additionally, in the case of the most conflicting, the skill of this area
The feature of the different embodiments described in this specification or example and different embodiment or example can be combined by art personnel
And combination.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is exemplary,
Being not considered as limiting the invention, those of ordinary skill in the art within the scope of the invention can be to above-described embodiment
It is changed, revises, replaces and modification.
Claims (10)
1. the extracting method of fat in a milk product, it is characterised in that including:
Milk product and ethanol are carried out the first mixed processing, obtains the first mixed liquor;
Described first mixed liquor and water are carried out the second mixed processing, obtains the second mixed liquor;
Described second mixed liquor carries out with petroleum ether the 3rd mix and standing process, obtain the 3rd mixed liquor;And
Described 3rd mixed liquor carries out filter and revolve steaming process, in order to obtain fat.
Method the most according to claim 1, it is characterised in that
Described milk product is milk powder, based on 1 gram of described milk powder,
The volume of described ethanol is 3~6mL, preferably 5mL,
The volume of described water is 0.5~3mL, preferably 1mL,
The volume of described petroleum ether is 3~7mL, preferably 5mL.
Method the most according to claim 1, it is characterised in that
Described milk product is thickness milk product, based on 1 gram of described thickness milk product,
The volume of described ethanol is 0.5~2mL, preferably 0.5mL,
The volume of described water is 0.1~1mL, preferably 0.1mL,
The volume of described petroleum ether is 2~6mL, preferably 2mL,
Optionally, described thickness milk product is Yoghourt.
Method the most according to claim 1, it is characterised in that
The time of described first mixed processing is 1~5 minute, preferably 1 minute.
Method the most according to claim 1, it is characterised in that
The time of described second mixed processing is 0.5~2 minute, preferably 0.5 minute.
Method the most according to claim 1, it is characterised in that
The time of described 3rd mixed processing is 1~5 minute, preferably 1 minute.
Method the most according to claim 1, it is characterised in that
The time that described standing processes is 8~18 hours, preferably 12 hours.
8. one kind measures the method for the peroxide value of fat in milk product, it is characterised in that including:
Fat is extracted according to the extracting method of fat in the milk product described in any one of claim 1~7;And
Known method is used to measure the peroxide value of described fat.
9. one kind measures the method for the peroxide value of fat in thickness milk product, it is characterised in that including:
(1) thickness milk product described in 200g is poured in container, add 100mL ethanol solution, stir 1 point with Glass rod
Clock;
(2) pouring in separatory funnel by the mixed liquor obtained by step (1), add 20mL water, lid lid rocks 0.5 minute,
Adding petroleum ether 400mL, lid lid rocks 1 minute, after standing 12 hours, ether layer is released to paving from separatory funnel end opening
Having in the funnel of filter paper and gauze, in collection filtrate to rotary evaporation bottle, rotation steaming evaporates solvent, obtains fat;
(3) weigh described in 2-5g fatty in iodine flask, add 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor (2:3 mixing),
Shaking flask makes lipid solubilization, adds 1mL saturated solution of potassium iodide (being added 10mL deionized water by 14g potassium iodide to be mixed to get),
Close the lid, shake up, dark place reaction 5min (period shakes once again), take out iodine flask and add 100mL deionized water, add
Enter starch indicator (1g/100mL), titrate with sodium thiosulfate standard solution (0.002mol/L), do blank assay simultaneously;
(4) oxidation number of fat is calculated in described thickness milk product according to the following formula:
X2=X1× 78.8,
In formula:
(1)X1: the peroxide value of fat in sample, unit is gram every hectogram (g/100g);
(2)X2: the peroxide value of fat in sample, unit is milliequivalent every kilogram (meq/kg);
(3)V1: sample consumes the volume of sodium thiosulfate standard titration solution, and unit is milliliter (mL);
(4)V2: consuming the volume of sodium thiosulfate standard titration solution in blank assay, unit is milliliter (mL);
(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;
(6) M: sample mass, unit is gram (g);
(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.
10. one kind measures the method for the peroxide value of fat in milk powder, it is characterised in that including:
(1) in container, add milk powder and ethanol solution (95%) 150mL described in 30g, shake 1 minute, add water 30mL,
Shake 0.5 minute;
(2) mixed liquor obtained by step (1) is poured in separatory funnel, adds petroleum ether 150mL, shake 1 minute,
Then stand 12 hours, ether layer is released to be covered with the funnel of filter paper from separatory funnel end opening, collect filtrate to rotary evaporation
In Ping, rotation steaming evaporates solvent, obtains fat;
(3) weigh described in 2-5g fatty in iodine flask, add 50mL isobutyltrimethylmethane .-glacial acetic acid mixed liquor (2:3 mixing),
Shaking flask makes lipid solubilization, adds 1mL saturated solution of potassium iodide (being added 10mL deionized water by 14g potassium iodide to be mixed to get),
Close the lid, shake up, dark place reaction 5min (period shakes once again), take out iodine flask and add 100mL deionized water, add
Enter starch indicator (1g/100mL), titrate with sodium thiosulfate standard solution (0.002mol/L), do blank assay simultaneously;
(4) peroxide value of fat is calculated in described thickness milk product according to the following formula:
X2=X1× 78.8,
In formula:
(1)X1: the peroxide value of fat in sample, unit is gram every hectogram (g/100g);
(2)X2: the peroxide value of fat in sample, unit is milliequivalent every kilogram (meq/kg);
(3)V1: sample consumes the volume of sodium thiosulfate standard titration solution, and unit is milliliter (mL);
(4)V2: consuming the volume of sodium thiosulfate standard titration solution in blank assay, unit is milliliter (mL);
(5) C: the concentration of sodium thiosulfate standard titration solution, unit is mol/L;
(6) M: sample mass, unit is gram (g);
(7) 0.1269: the quality of the iodine suitable with 1.00mL sodium thiosulfate standard titration solution, unit is g;
(8) 78.8: conversion factor.
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CN114703014A (en) * | 2022-02-15 | 2022-07-05 | 华南理工大学 | Method for extracting grease from diglyceride microcapsule |
CN117264692A (en) * | 2023-10-24 | 2023-12-22 | 宁夏回族自治区食品检测研究院 | Method for extracting oil for acid value and peroxide value experiments |
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