CN106525556A - Method for detecting acid value and peroxidation value in canned sardines - Google Patents
Method for detecting acid value and peroxidation value in canned sardines Download PDFInfo
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- CN106525556A CN106525556A CN201610926829.3A CN201610926829A CN106525556A CN 106525556 A CN106525556 A CN 106525556A CN 201610926829 A CN201610926829 A CN 201610926829A CN 106525556 A CN106525556 A CN 106525556A
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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
- G01N1/4055—Concentrating samples by solubility techniques
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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
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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Abstract
The invention discloses a method for detecting an acid value and a peroxidation value in canned sardines. The method includes the steps of firstly, extracting sardine grease, to be more specific, drying and performing ultrafine crushing and supercritical carbon dioxide extraction; secondly, using a potassium hydroxide standard solution titration method to determine the acid value; thirdly, determining the peroxidation value, to be more specific, using excessive ferrocene solution to have oxidation and complexation reaction with cumene hydroperoxide in the sardine grease to generate ferrocene cumene ether, and using a spectrophotometric method to detect complex concentration. The method has the advantages that the canned sardines are dried first and crushed in ultrafine manner to obtain sardine micro-powder, supercritical carbon dioxide extraction is performed on the sardine micro-powder to obtain the sardine grease, the extraction rate of the sardine grease is high, the extraction quality of the sardine grease is good, and the determining result accuracy of the acid value and the peroxidation value in the canned sardines is increased greatly.
Description
Technical field
The present invention relates to technical field of food detection, the detection of acid value and peroxide value in specifically a kind of canned sardines
Method.
Background technology
Acid value refers to the content of free fatty in vegetable oil, with the milligram number of every gram of coil neutralization potassium hydroxide（Mg hydrogen-oxygens
Change potassium/g）Represent.Detection acid value can reflect the degree that whether grease is sour and becomes sour.If eaten during the grease for becoming sour can cause
Toxication shape.Peroxide value raise be early stage index spoiled by rancid oil or fat, when it is spoiled by rancid oil or fat to a certain extent when, peroxide can be formed
Aldehyde and copper, hereafter peroxide value can reduce again（Acid value is raised）.The World Health Organization（WHO）Peroxide value is recommended to be not to be exceeded
10mmol/kg, can occur the poisoning symptom such as headache, dizzy, stomachache, diarrhoea, vomiting after otherwise eating.For water in national standard
Producing dried product, cake, quick-frozen conditioning product etc. has corresponding product standard, which specify the index of acid value and peroxide value
Limit value, but it is as some food are low oil contents therefore bad using traditional mode oil extracting rate, and take reagent and time.
Sardine is rich in surprising nutritive value, is OMEGA-3 aliphatic acid, protein and calcium rich in phosphatide.According to the U.S.
The web site contents of cardiovascular association show that this special fatty acid can reduce the generation of triglyceride（That causes thrombus has
Evil aliphatic acid）, and have the magical effect for being gradually lowered blood pressure and slowing down atherosclerotic speed.Pregnant woman should eat in the gestational period more
Fish, such as sardine, because sardine is rich in phosphatide.Phosphatide in sardine promotes for the brain development of fetus has simultaneously
Advantageous effect.Except phosphatide, sardine also containing a large amount of calcareous, especially in fish-bone.
Canned sardines is a kind of canned food made with sardine meat and catsup, because its shelf-life is longer, is subject to
The pursuing of numerous gourmands.Because of fat of the sardine containing about 1.1%, also there is risk spoiled by rancid oil or fat in sardine, therefore, need
Work out the detection method of acid value and peroxide value in a kind of suitable canned sardines.
The content of the invention
It is an object of the invention to provide in a kind of canned sardines acid value and peroxide value detection method, by extract
Yield is high, the sardine grease that quality is excellent, improves the measurement result accuracy of wherein acid value and peroxide value.
For achieving the above object, the present invention provides following technical scheme：
In a kind of canned sardines, the detection method of acid value and peroxide value, comprises the following steps：
（1）The extraction of sardine grease, comprises the following steps：
11）Drying：Canned sardines is taken, 6～8h at a temperature of being placed in 55～60 DEG C, is toasted, its internal moisture is removed, sand must be done
Fourth fish；
12）Ultramicro grinding：Dry sardine meal is broken to into 20～28 μm using ball mill first, is then crushed to jet mill
1.5～4 μm, obtain sardine micro mist；
13）Supercritical carbon dioxide extracting：Sardine micro mist is placed in extraction kettle, extracting pressure is controlled for 15～18MPa, extraction
Temperature being taken for 62～65 DEG C, extraction time is 4～5h, one-level separating pressure is 8～10MPa, the second-order separation pressure is 3～
4MPa, separation temperature are 50～54 DEG C, repeat extraction three times, collect the grease in separating still, as sardine grease；
（2）The measure of acid value, comprises the following steps：
21）The ethanol that ether and volumetric concentration are 92% is mixed according to equal-volume ratio, then is charged with 0.001 times of its volume
Phenolphthalein indicator, then with the potassium hydroxide solution that concentration is 0.2mol/L be neutralized to phenolphthalein indicator in neutrality, mixed
Close liquid；
22）M gram of sardine grease is accurately weighed, is placed in 250ml conical flasks, add 80ml steps 21）The mixed liquor for obtaining, fills
Divide and shake up, be completely dissolved sardine grease, add 1～2 to drip phenolphthalein indicator afterwards, shake well is 0.1mol/ with concentration
The standard potassium hydroxide solution of L is titrated to blush, till 15 seconds colour-fast；
23）Calculate acid value：Acid value=（56.1×V×C）The unit of/m, wherein acid value is mg/g；V is the hydroxide that titration is consumed
The volume of potassium standard liquid, unit are ml；Concentration of the C for standard potassium hydroxide solution, unit is mol/L；M is sardine grease
Quality, unit for gram.
（3）The measure of peroxide value, comprises the following steps：
31）With isopropanol as solvent, solution of ferrocene of the compound concentration for 28mol/L；
32）M gram of sardine grease is accurately weighed, is placed in 250ml conical flasks, under the conditions of 52～55 DEG C, using excessive two
In luxuriant ferrous solution and sardine grease there is 30～40min of Oxidation and complexation reaction in cumyl hydroperoxide, generate ferrocene isopropyl
Phenylate；
33）Using the concentration of spectrophotometry complex compound；
33）Calculate peroxide value：M=（1000A-255.3）/（0.1101×m）, peroxide values of the wherein M for sardine grease,
Unit is mmol/kg；A is the absorbance that sardine grease is detected at 319nm, and unit is 1；M is sardine grease
Quality, unit for gram.
As further scheme of the invention：The purity of the carbon dioxide used by described supercritical carbon dioxide extracting is not
Less than 99.9%.
As further scheme of the invention：Described step 13）In, extracting pressure is controlled for 16MPa, extraction temperature is
64 DEG C, extraction time is 5h, and one-level separating pressure is 9MPa, and the second-order separation pressure is 4MPa, and separation temperature is 52 DEG C.
As further scheme of the invention：Described step 21）With step 32）In, the quality of sardine grease is accurate
To 0.0002g.
As further scheme of the invention：Described step 32）In, under the conditions of 53 DEG C, there is Oxidation and complexation reaction
35min。
Compared with prior art, the invention has the beneficial effects as follows：
The present invention, is then carried out to sardine micro mist super facing into sardine micro mist first by canned sardines drying, ultramicro grinding
Boundary's carbon dioxide abstraction is extracted and obtains sardine grease, and the recovery rate of the sardine grease is high, and extraction quality is excellent, substantially increases
The wherein measurement result accuracy of acid value and peroxide value.
The present invention replaces water or organic solvent as spe medium, environmental protection, without dirt using the carbon dioxide of nontoxic residue-free
Dye, is worthy of popularization.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, in a kind of canned sardines, the detection method of acid value and peroxide value, comprises the following steps：
（1）The extraction of sardine grease, comprises the following steps：
11）Drying：Canned sardines is taken, at a temperature of being placed in 55 DEG C, 8h is toasted, its internal moisture is removed, is obtained dry sardine；
12）Ultramicro grinding：Dry sardine meal is broken to into 20～28 μm using ball mill first, is then crushed to jet mill
1.5～4 μm, obtain sardine micro mist；
13）Supercritical carbon dioxide extracting：Sardine micro mist is placed in extraction kettle, extracting pressure is controlled for 15MPa, extraction temperature
Spend for 65 DEG C, extraction time is 5h, and one-level separating pressure is 10MPa, and the second-order separation pressure is 4MPa, and separation temperature is 50 DEG C,
Repeat extraction three times, collect the grease in separating still, as sardine grease；
（2）The measure of acid value, comprises the following steps：
21）The ethanol that ether and volumetric concentration are 92% is mixed according to equal-volume ratio, then is charged with 0.001 times of its volume
Phenolphthalein indicator, then with the potassium hydroxide solution that concentration is 0.2mol/L be neutralized to phenolphthalein indicator in neutrality, mixed
Close liquid；
22）M gram of sardine grease is accurately weighed, 0.0002g is accurate to, is placed in 250ml conical flasks, add 80ml steps 21）
The mixed liquor for obtaining, fully shakes up, and is completely dissolved sardine grease, 1～2 drop phenolphthalein indicator of addition afterwards, shake well,
Blush is titrated to the standard potassium hydroxide solution that concentration is 0.1mol/L, till 15 seconds colour-fast；
23）Calculate acid value：Acid value=（56.1×V×C）The unit of/m, wherein acid value is mg/g；V is the hydroxide that titration is consumed
The volume of potassium standard liquid, unit are ml；Concentration of the C for standard potassium hydroxide solution, unit is mol/L；M is sardine grease
Quality, unit for gram.
（3）The measure of peroxide value, comprises the following steps：
31）With isopropanol as solvent, solution of ferrocene of the compound concentration for 28mol/L；
32）M gram of sardine grease is accurately weighed, 0.0002g is accurate to, is placed in 250ml conical flasks, under the conditions of 52 DEG C, is made
There is Oxidation and complexation reaction 40min with cumyl hydroperoxide in excessive solution of ferrocene and sardine grease, generate two luxuriant
Iron isopropyl phenylate；
33）Using the concentration of spectrophotometry complex compound；
33）Calculate peroxide value：M=（1000A-255.3）/（0.1101×m）, peroxide values of the wherein M for sardine grease,
Unit is mmol/kg；A is the absorbance that sardine grease is detected at 319nm, and unit is 1；M is sardine grease
Quality, unit for gram.
Embodiment 2
In the embodiment of the present invention, in a kind of canned sardines, the detection method of acid value and peroxide value, comprises the following steps：
（1）The extraction of sardine grease, comprises the following steps：
11）Drying：Canned sardines is taken, at a temperature of being placed in 60 DEG C, 6h is toasted, its internal moisture is removed, is obtained dry sardine；
12）Ultramicro grinding：Dry sardine meal is broken to into 20～28 μm using ball mill first, is then crushed to jet mill
1.5～4 μm, obtain sardine micro mist；
13）Supercritical carbon dioxide extracting：Sardine micro mist is placed in extraction kettle, extracting pressure is controlled for 18MPa, extraction temperature
Spend for 62 DEG C, extraction time is 4h, and one-level separating pressure is 8MPa, and the second-order separation pressure is 3MPa, and separation temperature is 54 DEG C,
Repeat extraction three times, collect the grease in separating still, as sardine grease；
（2）The measure of acid value, comprises the following steps：
21）The ethanol that ether and volumetric concentration are 92% is mixed according to equal-volume ratio, then is charged with 0.001 times of its volume
Phenolphthalein indicator, then with the potassium hydroxide solution that concentration is 0.2mol/L be neutralized to phenolphthalein indicator in neutrality, mixed
Close liquid；
22）M gram of sardine grease is accurately weighed, 0.0002g is accurate to, is placed in 250ml conical flasks, add 80ml steps 21）
The mixed liquor for obtaining, fully shakes up, and is completely dissolved sardine grease, 1～2 drop phenolphthalein indicator of addition afterwards, shake well,
Blush is titrated to the standard potassium hydroxide solution that concentration is 0.1mol/L, till 15 seconds colour-fast；
23）Calculate acid value：Acid value=（56.1×V×C）The unit of/m, wherein acid value is mg/g；V is the hydroxide that titration is consumed
The volume of potassium standard liquid, unit are ml；Concentration of the C for standard potassium hydroxide solution, unit is mol/L；M is sardine grease
Quality, unit for gram.
（3）The measure of peroxide value, comprises the following steps：
31）With isopropanol as solvent, solution of ferrocene of the compound concentration for 28mol/L；
32）M gram of sardine grease is accurately weighed, 0.0002g is accurate to, is placed in 250ml conical flasks, under the conditions of 55 DEG C, is made
There is Oxidation and complexation reaction 30min with cumyl hydroperoxide in excessive solution of ferrocene and sardine grease, generate two luxuriant
Iron isopropyl phenylate；
33）Using the concentration of spectrophotometry complex compound；
33）Calculate peroxide value：M=（1000A-255.3）/（0.1101×m）, peroxide values of the wherein M for sardine grease,
Unit is mmol/kg；A is the absorbance that sardine grease is detected at 319nm, and unit is 1；M is sardine grease
Quality, unit for gram.
Embodiment 3
In the embodiment of the present invention, in a kind of canned sardines, the detection method of acid value and peroxide value, comprises the following steps：
（1）The extraction of sardine grease, comprises the following steps：
11）Drying：Canned sardines is taken, at a temperature of being placed in 58 DEG C, 7h is toasted, its internal moisture is removed, is obtained dry sardine；
12）Ultramicro grinding：Dry sardine meal is broken to into 20～28 μm using ball mill first, is then crushed to jet mill
1.5～4 μm, obtain sardine micro mist；
13）Supercritical carbon dioxide extracting：Sardine micro mist is placed in extraction kettle, extracting pressure is controlled for 16MPa, extraction temperature
Spend for 64 DEG C, extraction time is 5h, and one-level separating pressure is 9MPa, and the second-order separation pressure is 4MPa, and separation temperature is 52 DEG C,
Repeat extraction three times, collect the grease in separating still, as sardine grease；
（2）The measure of acid value, comprises the following steps：
21）The ethanol that ether and volumetric concentration are 92% is mixed according to equal-volume ratio, then is charged with 0.001 times of its volume
Phenolphthalein indicator, then with the potassium hydroxide solution that concentration is 0.2mol/L be neutralized to phenolphthalein indicator in neutrality, mixed
Close liquid；
22）M gram of sardine grease is accurately weighed, 0.0002g is accurate to, is placed in 250ml conical flasks, add 80ml steps 21）
The mixed liquor for obtaining, fully shakes up, and is completely dissolved sardine grease, adds 2 to drip phenolphthalein indicator afterwards, and shake well is used
Concentration is titrated to blush for the standard potassium hydroxide solution of 0.1mol/L, till 15 seconds colour-fast；
23）Calculate acid value：Acid value=（56.1×V×C）The unit of/m, wherein acid value is mg/g；V is the hydroxide that titration is consumed
The volume of potassium standard liquid, unit are ml；Concentration of the C for standard potassium hydroxide solution, unit is mol/L；M is sardine grease
Quality, unit for gram.
（3）The measure of peroxide value, comprises the following steps：
31）With isopropanol as solvent, solution of ferrocene of the compound concentration for 28mol/L；
32）M gram of sardine grease is accurately weighed, 0.0002g is accurate to, is placed in 250ml conical flasks, under the conditions of 53 DEG C, is made
There is Oxidation and complexation reaction 35min with cumyl hydroperoxide in excessive solution of ferrocene and sardine grease, generate two luxuriant
Iron isopropyl phenylate；
33）Using the concentration of spectrophotometry complex compound；
33）Calculate peroxide value：M=（1000A-255.3）/（0.1101×m）, peroxide values of the wherein M for sardine grease,
Unit is mmol/kg；A is the absorbance that sardine grease is detected at 319nm, and unit is 1；M is sardine grease
Quality, unit for gram.
The present invention yield height of extraction sardine grease, quality from canned sardines is excellent, substantially increases wherein acid value
With the measurement result accuracy of peroxide value.The present invention replaces water or organic solvent conduct using the carbon dioxide of nontoxic residue-free
Spe medium, environmental protection is pollution-free, is worthy of popularization.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (6)
1. in a kind of canned sardines acid value and peroxide value detection method, it is characterised in that comprise the following steps：
（1）The extraction of sardine grease, comprises the following steps：
11）Drying：Canned sardines is taken, 6～8h at a temperature of being placed in 55～60 DEG C, is toasted, its internal moisture is removed, sand must be done
Fourth fish；
12）Ultramicro grinding：Dry sardine meal is broken to into 20～28 μm using ball mill first, is then crushed to jet mill
1.5～4 μm, obtain sardine micro mist；
13）Supercritical carbon dioxide extracting：Sardine micro mist is placed in extraction kettle, extracting pressure is controlled for 15～18MPa, extraction
Temperature being taken for 62～65 DEG C, extraction time is 4～5h, one-level separating pressure is 8～10MPa, the second-order separation pressure is 3～
4MPa, separation temperature are 50～54 DEG C, repeat extraction three times, collect the grease in separating still, as sardine grease；
（2）The measure of acid value, comprises the following steps：
21）The ethanol that ether and volumetric concentration are 92% is mixed according to equal-volume ratio, then is charged with 0.001 times of its volume
Phenolphthalein indicator, then with the potassium hydroxide solution that concentration is 0.2mol/L be neutralized to phenolphthalein indicator in neutrality, mixed
Close liquid；
22）M gram of sardine grease is accurately weighed, is placed in 250ml conical flasks, add 80ml steps 21）The mixed liquor for obtaining, fills
Divide and shake up, be completely dissolved sardine grease, add 1～2 to drip phenolphthalein indicator afterwards, shake well is 0.1mol/ with concentration
The standard potassium hydroxide solution of L is titrated to blush, till 15 seconds colour-fast；
23）Calculate acid value：Acid value=（56.1×V×C）The unit of/m, wherein acid value is mg/g；V is the hydroxide that titration is consumed
The volume of potassium standard liquid, unit are ml；Concentration of the C for standard potassium hydroxide solution, unit is mol/L；M is sardine grease
Quality, unit for gram.
2.（3）The measure of peroxide value, comprises the following steps：
31）With isopropanol as solvent, solution of ferrocene of the compound concentration for 28mol/L；
32）M gram of sardine grease is accurately weighed, is placed in 250ml conical flasks, under the conditions of 52～55 DEG C, using excessive two
In luxuriant ferrous solution and sardine grease there is 30～40min of Oxidation and complexation reaction in cumyl hydroperoxide, generate ferrocene isopropyl
Phenylate；
33）Using the concentration of spectrophotometry complex compound；
33）Calculate peroxide value：M=（1000A-255.3）/（0.1101×m）, peroxide values of the wherein M for sardine grease,
Unit is mmol/kg；A is the absorbance that sardine grease is detected at 319nm, and unit is 1；M is sardine grease
Quality, unit for gram.
3. in canned sardines according to claim 1 acid value and peroxide value detection method, it is characterised in that it is described
Supercritical carbon dioxide extracting used by carbon dioxide purity be not less than 99.9%.
4. in canned sardines according to claim 1 acid value and peroxide value detection method, it is characterised in that it is described
The step of 13）In, extracting pressure is controlled for 16MPa, extraction temperature is 64 DEG C, and extraction time is 5h, and one-level separating pressure is
9MPa, the second-order separation pressure are 4MPa, and separation temperature is 52 DEG C.
5. in canned sardines according to claim 1 acid value and peroxide value detection method, it is characterised in that it is described
The step of 21）With step 32）In, the quality of sardine grease is accurate to 0.0002g.
6. in canned sardines according to claim 1 acid value and peroxide value detection method, it is characterised in that it is described
The step of 32）In, under the conditions of 53 DEG C, there is Oxidation and complexation reaction 35min.
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| CN103776825A (en) * | 2014-01-11 | 2014-05-07 | 河南工业大学 | Determining method of acid value of deep-color grease |
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| CN104764699A (en) * | 2015-01-22 | 2015-07-08 | 四川大学 | Method for determination of edible oil acid value |
| CN105241832A (en) * | 2015-10-12 | 2016-01-13 | 天津科技大学 | Grease peroxide value detection method |
| CN105424872A (en) * | 2015-12-11 | 2016-03-23 | 谱尼测试集团上海有限公司 | Method for detecting acid value and peroxide value through oil in low-oil food |
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2016
- 2016-10-31 CN CN201610926829.3A patent/CN106525556A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102519957A (en) * | 2011-12-23 | 2012-06-27 | 澳优乳业（中国）有限公司 | Detection method for peroxide value of milk powder |
| CN102706872A (en) * | 2012-06-13 | 2012-10-03 | 安徽省农业科学院农产品加工研究所 | Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof |
| CN103776825A (en) * | 2014-01-11 | 2014-05-07 | 河南工业大学 | Determining method of acid value of deep-color grease |
| CN104458739A (en) * | 2014-12-31 | 2015-03-25 | 山东三星玉米产业科技有限公司 | Method for detecting acid value of vegetable oil containing oryzanol |
| CN104764699A (en) * | 2015-01-22 | 2015-07-08 | 四川大学 | Method for determination of edible oil acid value |
| CN105241832A (en) * | 2015-10-12 | 2016-01-13 | 天津科技大学 | Grease peroxide value detection method |
| CN105424872A (en) * | 2015-12-11 | 2016-03-23 | 谱尼测试集团上海有限公司 | Method for detecting acid value and peroxide value through oil in low-oil food |
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Application publication date: 20170322 |