CN104458739A - Method for detecting acid value of vegetable oil containing oryzanol - Google Patents
Method for detecting acid value of vegetable oil containing oryzanol Download PDFInfo
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- CN104458739A CN104458739A CN201410846858.XA CN201410846858A CN104458739A CN 104458739 A CN104458739 A CN 104458739A CN 201410846858 A CN201410846858 A CN 201410846858A CN 104458739 A CN104458739 A CN 104458739A
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Abstract
The invention discloses a method for detecting the acid value of vegetable oil containing oryzanol. The method comprises the steps that the following mixed dissolved solutions are used for dissolving a vegetable oil sample containing the oryzanol, wherein diethyl ether and ethyl alcohol with the concentration being 95% are mixed according to the volume ratio of 1:1, before using, 0.1mL of alkali blue-ethyl alcohol indicating liquid is added in every 100 mL of the above mixed solvent of the diethyl ether and the ethyl alcohol, and a KOH standard solution is used for accurately neutralizing the solution to be in the slight red color; 1-2 drops of alkali blue-ethyl alcohol are used as the indicating liquid, a potassium hydroxide- ethyl alcohol standard solution is used as a titrating solution, and a titrimetric method is used for detecting the acid value of the vegetable oil containing the oryzanol. The method solves the problem that the determination of titration end-point is influenced due to the color disturbance of the oryzanol in the vegetable oil with high oryzanol content. According to the method, the titration end points are observed and cleaned accurately, and the accuracy of the acid value detecting is improved. The method can be widely applied to acid value detecting of the vegetable oil with the high oryzanol content.
Description
Technical field
The invention belongs to vegetable oil detection technique field, be specifically related to a kind of detection method of the acid value of plant oil containing oryzanol.
Background technology
The milligram number of potassium hydroxide required for free fatty acid during acid value of lipids refers to and in 1g grease.Acid value is the important indicator of edible oil quality evaluation, product safety restriction, is also the foundation that oil alkali refining depickling calculates the change of alkali charge, oil and fat refining degree and storage quality.Therefore, acid value of lipids is determined in real work very important effect.
The size of acid value of lipids with produce the raw material of grease, grease produces with the method for storage and transportation of the technique of processing, grease and storing condition etc. relevant.Such as: the acid value that the more immature or seed that mildews of just germinateing of ripe oilseed produces grease is little.Triglyceride liquefaction process be heated or lipolytic enzyme effect and decompose generation free fatty acid, thus to make in oil acid value increase.Grease is at duration of storage, and due to the effect of the factors such as moisture, temperature, light, lipase, be broken down into free fatty acid makes acid value increase in oil, and storage-stable reduces.
The method of current mensuration acid value is a lot: wherein colourimetry is by organic solvent (isooctane), surfactant [two one (2 one ethylhexyl) sodium sulfo-succinate] and a small amount of water are mixed to form optically transparent stable Reverse Micelle System with certain proportion, are dissolved in phenol red in the aqueous phase of reverse micelle pH=9.It is phenol red when pKl equals 7.8, aobvious red in alkaline medium, its aqueous solution has absorption maximum in 558nm place, free fatty acid content is calculated by typical curve, this method is highly sensitive, finding speed fast, is applicable to the occasion measuring the low sample of content of fatty acid and needs Fast Measurement gross sample; First chromatography utilizes the free fatty acid in ethanol equal solvent analysis grease, because the general polarity of fatty acid is stronger, volatility is low, poor heat stability, so generally first convert it into corresponding derivant fatty acid methyl ester with KOH/ methyl alcohol, thus reduces its polarity, increase its thermal stability, then analyze with Agilent4890D gas chromatograph, use fid detector, its recovery is at 89%-109%.This method reagent dosage is few, is suitable for large batch of sample determination, but vapor-phase chromatography needs standard items to compare, and this method is more suitable for the content and the fatty acid component that measure single fatty acid in sample; Potentiometric titration is a kind of analytical approach of classics, has that equipment is simple, easy and simple to handle, degree of accuracy advantages of higher.Since the sixties in 20th century, developing rapidly as potentiometric titration provides a collection of good indicator electrode of ion-selective electrode, improves sensitivity and selectivity.The accuracy of potentiometric determination acidity or acid value is higher than general titrimetry, to colored solutions, turbid solution or do not have suitable indicators to judge the titrimetry of terminal is comparatively suitable.Its measuring principle indicator electrode (glass electrode) and contrast electrode (mercurous chloride electrode) or combination electrode is inserted in oil sample solution to form a primary element, and its electromotive force size is relevant with the pH size of solution.When measuring acid value, in the process with standard base (SB) drop stand oil sample solution, the mV value (or pH value) of solution is constantly measured with pH acidometer, along with adding of titrant, owing to there is neutralization reaction, FFA concentrations constantly reduces, thus indicator electrode current potential respective change, by the time time near titration end-point, indicator electrode potential break, the mV(recorded or pH value) produce hop change, so, the volume of alkali lye is consumed by the mV value (or pH value) recorded and titration, make titration curve, just can find out the alkali lye volume that titration end-point is corresponding, calculate acid value value.
Somebody proposes a kind of technology utilizing indirect titration to measure edible oil acid value in water and ethanol medium, and the degree of accuracy of this technology and accuracy are suitable for the monitoring of edible oil quality, and without the need to the neutralisation treatment in advance of acid.L.Lykken etc. have studied free acidity in potentiometric determination edible oil and lubricating oil and in conjunction with acidity.Potentiometric titration is generally considered to one of alternative method of traditional alkali titration, but this method needs duplicate measurements and comparatively strict process, also needs loaded down with trivial details titration and calibration procedure, the oil sample that this method needs relative quantity larger.
GB/T mono-5530-2005 defines the method measuring animal and plant fat acidity and comprises hot ethanol determination method, cold solvent determination method and potentiometric titration, wherein hot ethanol determination method is normative reference method, cold solvent method is only applicable to light grease, potentiometric titration utilizes pH meter to judge titration end-point, then needed for titration, the gauge of potassium hydroxide calculates acid value of oil and fat, the essence of the method is titrimetry, take potassium hydroxide solution as titrant, and phenolphthalein is indicator.The milligram number of potassium hydroxide required for the free fatty acid in the change calculations of titration end-point color and in 1g grease, thus draw the acid value of grease.
But oryzanol be forulic acid and plant sterol in conjunction with fat, when grease forms mixed phase by diethylether-ethanol dissolution with solvents, in oil, contained oryzanol is also dissolved in mixing oil phase simultaneously.Can react owing to also meeting titration alkali lye containing acid value in oryzanol, and oryzanol content is higher, acid value is also higher, when with phenolphthalein as indicator time, oryzanol and phenolphthalein react, and titration end-point is postponed, and cause result bigger than normal.
When selecting alkali indigo plant as indicator, oryzanol therewith indicator does not react, and after adding indicator, titration system becomes blueness, is titration end-point when titration system blueness disappears and becomes blush, and terminal change obviously.
Summary of the invention
The object of the present invention is to provide a kind of acid value of plant oil detection method containing oryzanol, overcome and contain in the high acid value of plant oil titration process of oryzanol at present, the interference of the oryzanol color contained in grease and be difficult to observe the variable color of indicator, is namely difficult to the problem judging titration end-point.To solve at present containing the technical matters that the acid value of plant oil that oryzanol is high detects.
The present invention is achieved by the following technical solutions:
Containing an acid value of plant oil detection method for oryzanol, said method comprising the steps of:
(1) accurately take the vegetable oil sample m gram containing oryzanol, be placed in 250mL conical flask;
(2) preparation of mixed solution: the ethanol being 95% by ether and concentration mixes according to the volume ratio of 1:1, face in the mixed solvent of every above-mentioned diethylether-ethanol of 100mL before using and add 0.1mL alkali indigo plant-ethanol indicator solution, be accurately neutralized to blush with KOH standard solution;
(3), in the mixed liquor sample dissolution after taking obtained in (2) that 80mL neutralized in advance, fully shake up, oil sample is dissolved completely, add 1-2 afterwards and drip alkali indigo plant-ethanol indicator solution, shake well, is titrated to blush with potassium hydroxide-ethanol standard solution, till 15s is colour-fast;
(4) acid value=(56.1 × V × C)/m.
Containing an acid value of plant oil detection method for oryzanol, accurately containing quality accurately to 0.01 gram of the vegetable oil sample of oryzanol described in step (1).
Containing an acid value of plant oil detection method for oryzanol, the concentration of the KOH standard solution described in step (2) is 0.1mol/L.
A kind of acid value of plant oil detection method containing oryzanol, the preparation method of the potassium hydroxide-ethanol standard solution described in step (3) comprises the following steps: the potassium hydroxide taking 7.5-8g, be placed in polyethylene can, add the water-soluble solution of 6-7ml, ethanol with 95% is diluted to 1000m L, airtight placement 24 h, with plastic tube siphon supernatant liquor in another polyethylene can, take the working standard reagent Potassium Hydrogen Phthalate that 0.75g is dried to constant weight in 105-110 DEG C of electric dry oven, being dissolved in 50m L boiled in the distilled water of also cooling, add the instructions phenolphthalein solution of 2 10 g/L, solution pinkiness is titrated to the potassium hydroxide-ethanol solution prepared, do blank test simultaneously, then potassium hydroxide-ethanol standard titration solution concentration (c (KOH)], numerical value represents with mole often liter, for in c (KOH)=m X 1 000/ (V1 mono-V2)/M formula: m is the exact value of the quality of Potassium Hydrogen Phthalate, unit is gram, V1 is the numerical value of the volume of the liquor-saturated solution of potassium hydroxide-second, and unit is milliliter, the numerical value of the volume of V2 blank test potassium hydroxide-ethanol solution, unit is milliliter, M is the numerical value of the molal weight of Potassium Hydrogen Phthalate, and unit is gram every mole.
Containing an acid value of plant oil detection method for oryzanol, the standard solution described in above-mentioned steps is all being demarcated before use.
A kind of acid value of plant oil detection method containing oryzanol, described in above-mentioned steps, the preparation method of alkali indigo plant-ethanol indicator solution comprises the following steps: take the blue 6b 1.00g of alkali, add in 50 milliliters of 95% ethanolic solutions boiled, and reflux 1 hour in a water bath, cooled and filtered, to obtain final product.
Containing an acid value of plant oil detection method for oryzanol, take oil sample 5-10g when acid number is less than 0.3, when acid number is 0.3-1.0, take oil sample 1-2g, when acid number is 1.0-3.0, take oil sample 0.5-1g, when acid number is greater than 3.0, take oil sample 0.1-0.5g.
Containing an acid value of plant oil detection method for oryzanol, be the color change observing mixed system when observing terminal.
Containing an acid value of plant oil detection method for oryzanol, in described acid value=(56.1 × V × C)/m, V is the volume of the potassium hydroxide-ethanol standard solution that titration consumes, and unit is milliliter; C is potassium hydroxide solution N, and m is vegetable oil example weight, and unit is gram.
The major technique of invention solves the problem being difficult to judge titration end-point containing the interference of oryzanol color in the high acid value determination process of oryzanol.
When titrate indicator is phenolphthalein, in titration system, oryzanol chance alkali lye presents yellow, and the yellow that oryzanol presents masks the blush that titration end-point phenolphthalein presents, and titration end-point is postponed, and causes result bigger than normal; And the color change of the blue indicator of alkali avoids the generation of this situation, after titration system adds the blue indicator of alkali, titration system becomes blueness, and in titration process, titration system blueness disappears when becoming blush and is titration end-point, and terminal change obviously
Advantage of the present invention is:
A kind of acid value of plant oil detection method containing oryzanol of the present invention solves the problem affecting titration end-point containing the color interference of oryzanol in the high vegetable oil of oryzanol and judge, the method titration end-point is observed cleaning, accurately, improve the accuracy that acid value detects.The acid value of plant oil that can be widely used in containing oryzanol is high measures.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, so that those skilled in the art more understands the present invention, but does not therefore limit the present invention.
Embodiment 1
Oil sample: not containing oryzanol corn oil (oil sample 1), oryzanol content 1700mg/kg corn oil (oil sample 2), oryzanol content 5000mg/kg corn oil (oil sample 3), oryzanol content 8000mg/kg corn oil (oil sample 4), oryzanol content 10000mg/kg corn oil (oil sample 5), oryzanol content 15000mg/kg corn oil (oil sample 6), oryzanol content 17000mg/kg corn oil (oil sample 7), oryzanol content 19000mg/kg corn oil (oil sample 8), oryzanol content 20000mg/kg corn oil (oil sample 9).
Reagent: the preparation method of potassium hydroxide-ethanol standard solution comprises the following steps: the potassium hydroxide taking 7.5-8g, be placed in polyethylene can, add the water-soluble solution of 6-7ml, ethanol with 95% is diluted to 1000m L, airtight placement 24 h, with plastic tube siphon supernatant liquor in another polyethylene can, take the working standard reagent Potassium Hydrogen Phthalate that 0.75g is dried to constant weight in 105-110 DEG C of electric dry oven, being dissolved in 50m L boiled in the distilled water of also cooling, add the instructions phenolphthalein solution of 2 10 g/L, solution pinkiness is titrated to the potassium hydroxide-ethanol solution prepared, do blank test simultaneously, then potassium hydroxide-ethanol standard titration solution concentration (c (KOH)], numerical value represents with mole often liter, for in c (KOH)=m X 1 000/ (V1 mono-V2)/M formula: m is the exact value of the quality of Potassium Hydrogen Phthalate, unit is gram, V1 is the numerical value of the volume of the liquor-saturated solution of potassium hydroxide-second, and unit is milliliter, the numerical value of the volume of V2 blank test potassium hydroxide-ethanol solution, unit is milliliter, M is the numerical value of the molal weight of Potassium Hydrogen Phthalate, and unit is gram every mole.
The preparation method of alkali indigo plant-ethanol indicator solution comprises the following steps: take the blue 6b 1.00g of alkali, add in 50 milliliters of 95% ethanolic solutions boiled, and reflux 1 hour in a water bath, cooled and filtered, to obtain final product.
Sample weighting amount: take oil sample 5-10g when acid number is less than 0.3, takes oil sample 1-2g when acid number is 0.3-1.0, take oil sample 0.5-1g when acid number is 1.0-3.0, takes oil sample 0.1-0.5g when acid number is greater than 3.0.
Take corn oil sample appropriate, accurately weighed, be placed in 250mL conical flask, add the neutral diethylether-ethanol mixed solvent of 80mL, fully shake up, oil sample is dissolved completely.Add the alkali indigo plant-ethanolic solution of 2 ~ 3 1%, shake well.Be titrated to yellow with the 0.1mol/LKOH standard solution demarcated, 15s is colour-fast.Volume (GB/T5530-2005) according to consuming KOH standard solution can calculate acid value.
In acid value=(56.1 × V × C)/m, V is the volume of the potassium hydroxide-ethanol standard solution that titration consumes, and unit is milliliter; C is potassium hydroxide solution N, and m is vegetable oil example weight, and unit is gram.
Testing result is in table 1.
the different indicator of table 1 is on the impact containing oryzanol corn oil acid value
。
As can be seen from Table 1, phenolphthalein give instruction agent time acid value of lipids unstable, the corn oil accuracy of surveying containing oryzanol by the method that alkali indigo plant does titrate indicator is higher, and during color change, blue disappearance becomes blush during this method observation terminal, color change is easy to be observed, improve the accuracy of operator to terminal point determining, and then improve the accuracy of acid value determination.
Claims (9)
1., containing an acid value of plant oil detection method for oryzanol, it is characterized in that said method comprising the steps of:
(1) accurately take the vegetable oil sample m gram containing oryzanol, be placed in 250mL conical flask;
(2) preparation of mixed solution: the ethanol being 95% by ether and concentration mixes according to the volume ratio of 1:1, face in the mixed solvent of every above-mentioned diethylether-ethanol of 100mL before using and add 0.1mL alkali indigo plant-ethanol indicator solution, be accurately neutralized to blush with KOH standard solution;
(3), in the mixed liquor sample dissolution after taking obtained in (2) that 80mL neutralized in advance, fully shake up, oil sample is dissolved completely, add 1-2 afterwards and drip alkali indigo plant-ethanol indicator solution, shake well, is titrated to blush with potassium hydroxide-ethanol standard solution, till 15s is colour-fast;
(4) acid value=(56.1 × V × C)/m.
2. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, is characterized in that described in step (1) accurately containing quality accurately to 0.01 gram of the vegetable oil sample of oryzanol.
3. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, is characterized in that the concentration of the KOH standard solution described in step (2) is 0.1mol/L.
4. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, it is characterized in that the preparation method of the potassium hydroxide-ethanol standard solution described in step (3) comprises the following steps: the potassium hydroxide taking 7.5-8g, be placed in polyethylene can, add the water-soluble solution of 6-7ml, ethanol with 95% is diluted to 1000m L, airtight placement 24 h, with plastic tube siphon supernatant liquor in another polyethylene can, take the working standard reagent Potassium Hydrogen Phthalate that 0.75g is dried to constant weight in 105-110 DEG C of electric dry oven, being dissolved in 50m L boiled in the distilled water of also cooling, add the instructions phenolphthalein solution of 2 10 g/L, solution pinkiness is titrated to the potassium hydroxide-ethanol solution prepared, do blank test simultaneously, then potassium hydroxide-ethanol standard titration solution concentration (c (KOH)], numerical value represents with mole often liter, for in c (KOH)=m X 1 000/ (V1 mono-V2)/M formula: m is the exact value of the quality of Potassium Hydrogen Phthalate, unit is gram, V1 is the numerical value of the volume of the liquor-saturated solution of potassium hydroxide-second, and unit is milliliter, the numerical value of the volume of V2 blank test potassium hydroxide-ethanol solution, unit is milliliter, M is the numerical value of the molal weight of Potassium Hydrogen Phthalate, and unit is gram every mole.
5. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, is characterized in that the standard solution described in above-mentioned steps is all being demarcated before use.
6. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, it is characterized in that the preparation method of alkali indigo plant-ethanol indicator solution described in above-mentioned steps comprises the following steps: take the blue 6b 1.00g of alkali, add in 50 milliliters of 95% ethanolic solutions boiled, and reflux 1 hour in a water bath, cooled and filtered, to obtain final product.
7. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, it is characterized in that acid number takes oil sample 5-10g when being less than 0.3, acid number takes oil sample 1-2g when being 0.3-1.0, acid number takes oil sample 0.5-1g when being 1.0-3.0, takes oil sample 0.1-0.5g when acid number is greater than 3.0.
8. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, is characterized in that it being the color change observing mixed system when observing terminal.
9. a kind of acid value of plant oil detection method containing oryzanol according to claim 1, it is characterized in that in described acid value=(56.1 × V × C)/m, V is the volume of the potassium hydroxide-ethanol standard solution that titration consumes, and unit is milliliter; C is potassium hydroxide solution N, and m is vegetable oil example weight, and unit is gram.
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Cited By (5)
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| CN106353460A (en) * | 2016-09-18 | 2017-01-25 | 国网福建省电力有限公司 | Device and method for intelligently and quickly measuring acid values of main transformer insulation paper |
| CN106525556A (en) * | 2016-10-31 | 2017-03-22 | 百奥森（江苏）食品安全科技有限公司 | Method for detecting acid value and peroxidation value in canned sardines |
| CN109632446A (en) * | 2019-02-25 | 2019-04-16 | 四川精卫食品检测科技有限公司 | The Sample pretreatment method of acid value and the detection method using it in a kind of measurement food |
| CN110243993A (en) * | 2018-03-07 | 2019-09-17 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind of detection method of cream acidity |
| CN112730392A (en) * | 2019-12-10 | 2021-04-30 | 浙江省农业科学院 | Test strip for rapidly detecting acid value of salad dressing, preparation method and test method |
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2014
- 2014-12-31 CN CN201410846858.XA patent/CN104458739A/en active Pending
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106353460A (en) * | 2016-09-18 | 2017-01-25 | 国网福建省电力有限公司 | Device and method for intelligently and quickly measuring acid values of main transformer insulation paper |
| CN106353460B (en) * | 2016-09-18 | 2018-12-11 | 国网福建省电力有限公司 | Acid value intelligence rapid determination device and method in a kind of main change insulated paper |
| CN106525556A (en) * | 2016-10-31 | 2017-03-22 | 百奥森（江苏）食品安全科技有限公司 | Method for detecting acid value and peroxidation value in canned sardines |
| CN110243993A (en) * | 2018-03-07 | 2019-09-17 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind of detection method of cream acidity |
| CN109632446A (en) * | 2019-02-25 | 2019-04-16 | 四川精卫食品检测科技有限公司 | The Sample pretreatment method of acid value and the detection method using it in a kind of measurement food |
| CN112730392A (en) * | 2019-12-10 | 2021-04-30 | 浙江省农业科学院 | Test strip for rapidly detecting acid value of salad dressing, preparation method and test method |
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Application publication date: 20150325 |