CN103592198A - Determination method for polar components in edible oil - Google Patents
Determination method for polar components in edible oil Download PDFInfo
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- CN103592198A CN103592198A CN201310625381.8A CN201310625381A CN103592198A CN 103592198 A CN103592198 A CN 103592198A CN 201310625381 A CN201310625381 A CN 201310625381A CN 103592198 A CN103592198 A CN 103592198A
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Abstract
The invention provides a determination method for polar components in edible oil, which relates to determination methods for edible oil. The method comprises the following steps: dissolving a semisolid or solid sample, carrying out filtering, then dissolving an oil sample in a mixed solution of petroleum ether and ether and allowing a volume to be fixed at 10 mL; drying silica gel, cooling the silica gel to room temperature, adding water, transferring the silica gel to the syringe of an injector, compacting the silica gel, adding sea sand or quartz sand and then adding the mixed solution of petroleum ether and ether along the wall of the syringe so as to wet the silica gel; when the surface of the mixed solution of petroleum ether and ether and the surface of sea sand or quartz sand are parallel and level, dissolving the oil sample in a chromatography column, adding the mixed solution of petroleum ether and ether for elution of nonpolar components, collecting eluate to a flask or beaker and carrying out drying by distillation and then weighing; studying separation effects of the nonpolar components; and carrying out calculation.
Description
Technical field
The present invention relates to the assay method of edible oil and fat, especially relate to a kind of assay method of edible oil and fat Semi-polarity composition.
Background technology
Polar component is that edible oil and fat occur after series of chemical under the service conditions such as frying, some the larger compositions of the normal grease molecule of ratio (triglyceride) polarity that produce are general names of triglyceride oxidation product, polymerizate, oxidative polymerization product and hydrolysate.These reaction product all can exert an adverse impact to the quality of grease, local flavor and nutritive value, and what have is even harmful to the health of human body.The total content of the polar component in grease can be used as a good standard of measure oil quality, and many countries delimits 25%～30% polar component content (m/m) in grease as method, over the oil product of this value, must forcibly discard.
The general method of measuring grease Semi-polarity composition is column chromatography, the standard method (GB/T5009.202-2003) of standard method ，Ye Shi China of the mensuration grease Semi-polarity composition of Gai Fashi IUPAC (IUPAC) and chemurgy scholar association of official (AOAC) approval.Concrete measuring principle is: edible oil and fat sample is by the chromatographic column of the silica gel of the certain moisture of absorption is housed, and under the wash-out of the mixtures of eluents forming at sherwood oil and ether, first nonpolarity element triglyceride is flowed out chromatographic column by wash-out.Be adsorbed on polar component on silica gel can be subsequently by ether as eluant, eluent wash-out, eluant, eluent is removed in volatilization, weighs, and calculates, and can obtain the content of grease Semi-polarity composition.
Because these standard methods exist length consuming time, need to use the shortcomings such as a large amount of organic solvents, so some researchers improve these standard methods.(Sebedio, the J.L. such as Sebedio J.L.; Septier, C.; Grandgirard, A..Fraction of commercial frying oil samples using SEP-PAK cartridges.Journal of the american oil chemists society, 1986,63:1541-1543) use Sep-Pak solid-phase extraction column to replace chromatographic column to carry out separation determination to the polar component in used edible oil, but because commercially available extraction column cannot regulate the fixing moisture of phase, fixedly the polarity of phase is uncontrollable, and Sep-Pak extraction column is expensive, and cost of determination is high; Have, there is memory effect in commercially available solid-phase extraction column in Reusability process again, makes measured value higher.Schulte E.(Schulte, E..Micromethod for the gravimetric determination of polar components in frying fats with ready for use columns.European Journal of lipid science and technology, 2000,102:574-579) use the fixedly Solid-Phase Extraction method of phase of making by oneself to measure the polar component in grease, the shortcoming of this method is: (1) sample size is little, and weighing error is large.(2) device is complicated, comprises the parts such as solvent bottle and nitrogen dry up, heating evaporation, poor practicability.
Except column chromatography, for the assay method of grease Semi-polarity composition, also have near infrared spectroscopy, nuclear magnetic resonance method, efficient volume exclusion chromatography and sensor determination method etc.In international standard, the definition of grease Semi-polarity composition is the polar material of measuring under given conditions by column chromatography, so the accuracy of the methods such as near infrared spectroscopy, nuclear magnetic resonance method, efficient volume exclusion chromatography and sensor determination method how, also need to contrast with column chromatography, not also International Standards Method, standard determination method that neither China.
Summary of the invention
The object of the invention is to the deficiency existing measuring the column chromatography of the polar component in edible oil and fat for existing, a kind of assay method of edible oil and fat Semi-polarity composition is provided.
One of assay method of edible oil and fat Semi-polarity composition, comprises the following steps:
1) semisolid or solid sample are dissolved, filter, then oil sample is dissolved in sherwood oil and ether mixed solution, and be settled to 10mL;
2) silica gel is dried, then add water after being cooled to room temperature, then be transferred in injector syringe, pier is real, adds sea sand or silica sand, then adds sherwood oil and ether mixed solution along needle cylinder wall, makes silica gel wetting;
3) surperficial when concordant on sherwood oil and ether mixed solution surface and sea sand (or silica sand), oil sample is dissolved in chromatographic column, then adds sherwood oil and ether mixed solution to carry out wash-out to nonpolarity element, it is m that eluent is collected in to quality
1flask or beaker in;
4) by the eluent evaporate to dryness in step 3) flask or beaker, weigh, obtaining proper mass is m
1flask or the evaporate to dryness of beaker after quality be m
3;
5) investigate nonpolarity element separating effect;
6) calculate
The computing formula of polar component content is:
In formula:
X: polar component content (%);
M: determined oil sample quality (g);
M
1: the quality of flask or beaker (g);
M
3: nonpolarity element quality sum (g) in flask or beaker and oil sample.
In step 1), described filtration can adopt Filter paper filtering; The consumption of described oil sample can be 1g, is preferably accurate to 0.001g, and the volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
In step 2) in, described silica gel can adopt 70～320 order silica gel; The condition of described oven dry can be put dry 24h in the baking oven of 160 ℃; The addition of described water can be 5% of silica gel by mass percentage; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
In step 3), the consumption of described oil sample can be 5mL; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1; The addition of described sherwood oil and ether mixed solution can be 60mL; Described wash-out can adopt double-stranded ball pressure method wash-out, and the speed of described wash-out can be 1.5mL/min.
In step 4), described evaporate to dryness can adopt the modes such as steaming instrument evaporate to dryness, heating water bath evaporate to dryness or heating plate heating evaporate to dryness of revolving.
In step 5), described investigation nonpolarity element separating effect can be investigated by thin-layer chromatography.
Two of the assay method of edible oil and fat Semi-polarity composition, comprises the following steps:
1) semisolid or solid sample are dissolved, filter, then oil sample is dissolved in sherwood oil and ether mixed solution, and be settled to 10mL;
2) silica gel is dried, then add water after being cooled to room temperature, then be transferred in injector syringe, pier is real, adds sea sand or silica sand, then adds sherwood oil and ether mixed solution along needle cylinder wall, makes silica gel wetting;
3) surperficial when concordant on sherwood oil and ether mixed solution surface and sea sand (or silica sand), oil sample is dissolved in chromatographic column, then adds sherwood oil and ether mixed solution to carry out wash-out to nonpolarity element, it is m that eluent is collected in to quality
1the 1st flask or the 1st beaker in;
4) after step 3) wash-out nonpolarity element, continue polar component wash-out, it is m that eluent is collected in to quality
2the 2nd flask or the 2nd beaker in;
5) by the eluent evaporate to dryness in step 4) flask or beaker, weigh, obtaining proper mass is m
2flask or the evaporate to dryness of beaker after quality be m
4;
6) investigate nonpolarity element separating effect;
7) calculate
If during wash-out nonpolarity element, the computing formula of polar component content is:
If during wash-out polar component, the computing formula of polar component content is:
In formula:
X: polar component content (%);
M: determined oil sample quality (g);
M
1: the quality (g) of the 1st flask or the 1st beaker;
M
2: the quality (g) of the 2nd flask or the 2nd beaker;
M
3: nonpolarity element quality sum (g) in the 1st flask or the 1st beaker and oil sample;
M
4: the 2nd flask or the 2nd beaker and oil sample Semi-polarity composition quality sum (g).
In step 1), described filtration can adopt Filter paper filtering; The consumption of described oil sample can be 1g, is preferably accurate to 0.001g, and the volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
In step 2) in, described silica gel can adopt 70～320 order silica gel; The condition of described oven dry can be put dry 24h in the baking oven of 160 ℃; The addition of described water can be 5% of silica gel by mass percentage; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
In step 3), the consumption of described oil sample can be 5mL; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1; The addition of described sherwood oil and ether mixed solution can be 60mL; Described wash-out can adopt double-stranded ball pressure method wash-out, and the speed of described wash-out can be 1.5mL/min.
In step 4), described continuation can be the concrete grammar of polar component wash-out: when substantially concordant with sea sand (or silica sand) surface on sherwood oil and ether mixed solution surface, add eluant, eluent ether and adopt double-stranded ball pressure method to carry out wash-out to polar component, elution speed is 1.5mL/min; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1; The addition of described sherwood oil and ether mixed solution can be 50mL.
In step 5), described evaporate to dryness can adopt the modes such as steaming instrument evaporate to dryness, heating water bath evaporate to dryness or heating plate heating evaporate to dryness of revolving.
In step 6), described investigation nonpolarity element separating effect can be investigated by thin-layer chromatography.
The present invention improves measuring the column chromatography of the polar component in edible oil and fat.The features such as use disposable syringe preparative chromatography post, has the memory effect of avoiding, and reduces systematic error, easy and simple to handle, with low cost.Same national standard method (GB/T5009.202-2003) is compared, and is not changing under separating effect prerequisite, reduces reagent consumption, relatively environmental protection.
First the present invention uses disposable syringe preparative chromatography post, and its benefit has: (1) avoids memory effect, reduces systematic error.Chromatographic column is easy residual grease in use, makes measurement result higher.Chromatographic column prepared by disposable syringe is together abandoned with in-built silica gel after use, does not have memory effect.(2) avoided the troublesome operation of washing, dry chromatographic column.Chromatographic column structure is comparatively complicated, especially more complicated with the chromatographic column structure of sieve plate and cock, gives the cleaning of chromatographic column and is dried and bring very large difficulty." disposable " chromatographic column of being prepared by disposable syringe, can avoid washing and dry troublesome operation completely.(3) experimental expenses is low.Disposable syringe is cheap, can greatly reduce experimental cost.
Secondly, do not increasing under the prerequisite of error at measurment, by reducing sample size, reducing the consumption of eluant, eluent and silica gel.Than GB (GB/T5009.202-2003), assay method provided by the invention can make eluant, eluent consumption reduce by 70%, and silica gel consumption is reduced to 5g by 35g; Than IUPAC International Standards Method (2.507), eluant, eluent consumption reduces by 60%, and silica gel consumption is reduced to 5g by 25g.Therefore method provided by the invention both can greatly reduce the use of organic solvent sherwood oil and ether, reduced the harm to environment and experimental implementation person, can also effectively reduce experimental cost.
Again, adopt dry column-packing.Dry column-packing can simplify the operation, and reduces workload, and separating effect is not had a significant effect.In addition, dry column-packing can also reduce eluant, eluent consumption, reduces the loss of silica gel in transfer process, reduces the impact of harmful gas on experimenter.
Embodiment
1. sample preparation
For semisolid or solid sample, low-grade fever makes to dissolve, and fully shakes up.If any solid impurity, with Filter paper filtering; As moisture content, use hydrophobicity Filter paper filtering.
Accurately take 1g(and be accurate to 0.001g) oil sample in volumetric flask, with petroleum ether/ethyl ether (v/v=9/1) mixed solution, dissolve, and be settled to 10mL.
2. chromatographic column is prepared
Regulate silica gel polarity: select 70～320 object silica gel, put dry 24h in the baking oven of 160oC, then in exsiccator, be cooled to room temperature.Add 5%(m/m) water, machinery shakes 2h, or rotates and mix 1h revolving to steam on instrument, airtight standby.
Select 30～60mL syringe, remove syringe needle and piston, at the bottom of post, put a small amount of absorbent cotton or glass wool, to prevent that silica gel from spilling.
Take the above-mentioned silica gel of 5g, be transferred in injector syringe, pier is real.Jog syringe, makes Silica Surface smooth, adds a small amount of sea sand or silica sand, Silica Surface disturbance when preventing from adding eluant, eluent.Along post jamb, slowly add 20mL petroleum ether/ethyl ether (v/v=9/1) mixed solution, make silica gel wetting.Can adopt double-stranded ball to pressurize to accelerate the rate of outflow of eluant, eluent.
3. polar component is separated with nonpolarity element
When substantially concordant with sea sand (or silica sand) surface on eluant, eluent surface, accurately pipette 5mL grease sample solution in chromatographic column, note not making silica gel dry.Add again 60mL eluant, eluent petroleum ether/ethyl ether (v/v=9/1) mixed solution to carry out wash-out to nonpolarity element.Can adopt double-stranded ball to pressurize to accelerate the rate of outflow of eluant, eluent, control elution speed is 1.5mL/min.It is m that eluent is collected in quality
1the 1st flask or the 1st beaker in.
4. polar component wash-out
If need, can continue polar component wash-out after wash-out nonpolarity element.Concrete operations are: when substantially concordant with sea sand (or silica sand) surface on eluant, eluent petroleum ether/ethyl ether (v/v=9/1) mixed solution surface, add 50mL eluant, eluent ether to carry out wash-out to polar component, note not making silica gel dry.Can adopt double-stranded ball to pressurize to accelerate the rate of outflow of eluant, eluent, control elution speed is 1.5mL/min.It is m that eluent is collected in quality
2the 2nd flask or the 2nd beaker in.
5. evaporation is weighed
Eluent in above-mentioned the 1st flask and the 2nd flask is steamed to instrument evaporate to dryness through revolving, and temperature is no more than 60 ℃ to prevent grease reaction at high temperature.Or the eluent in above-mentioned the 1st beaker and the 2nd beaker is heated to evaporate to dryness through modes such as heating water bath or heating plates, temperature is no more than 80 ℃ to prevent grease reaction at high temperature.
After the moisture drying of flask or beaker outer wall, weigh.Obtaining quality is m
1the 1st flask or the quality of the 1st beaker be m
3, quality is m
2the 2nd flask or the quality of the 2nd beaker be m
4.
6. thin-layer chromatography
The separating effect of nonpolarity element and polar component can be investigated by thin-layer chromatography.
7. calculate
If during wash-out nonpolarity element, the computing formula of polar component content is:
If during wash-out polar component, the computing formula of polar component content is:
In formula:
X: polar component content (%);
M: determined oil sample quality (g);
M
1: the quality (g) of the 1st flask or the 1st beaker;
M
2: the quality (g) of the 2nd flask or the 2nd beaker;
M
3: nonpolarity element quality sum (g) in the 1st flask or the 1st beaker and oil sample;
M
4: the 2nd flask or the 2nd beaker and oil sample Semi-polarity composition quality sum (g).
The present invention improves measuring the column chromatography of the polar component in edible oil and fat.The features such as use disposable syringe preparative chromatography post, has the memory effect of avoiding, and reduces systematic error, easy and simple to handle, with low cost.Same national standard method (GB/T5009.202-2003) is compared, and is not changing under separating effect prerequisite, reduces reagent consumption, relatively environmental protection.
Claims (10)
1. an assay method for edible oil and fat Semi-polarity composition, is characterized in that comprising the following steps:
1) semisolid or solid sample are dissolved, filter, then oil sample is dissolved in sherwood oil and ether mixed solution, and be settled to 10mL;
2) silica gel is dried, then add water after being cooled to room temperature, then be transferred in injector syringe, pier is real, adds sea sand or silica sand, then adds sherwood oil and ether mixed solution along needle cylinder wall, makes silica gel wetting;
3) when concordant with sea sand or quartz sand surface on sherwood oil and ether mixed solution surface, oil sample be dissolved in chromatographic column, then add sherwood oil and ether mixed solution to carry out wash-out to nonpolarity element, it is m that eluent is collected in to quality
1flask or beaker in;
4) by the eluent evaporate to dryness in step 3) flask or beaker, weigh, obtaining proper mass is m
1flask or the evaporate to dryness of beaker after quality be m
3;
5) investigate nonpolarity element separating effect;
6) calculate
The computing formula of polar component content is:
In formula:
X: polar component content, %;
M: determined oil sample quality, g;
M
1: the quality of flask or beaker, g;
M
3: nonpolarity element quality sum in flask or beaker and oil sample, g.
2. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 1, is characterized in that in step 1), and described filtration adopts Filter paper filtering; The consumption of described oil sample is 1g, is preferably accurate to 0.001g, and the volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
3. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 1, is characterized in that in step 2) in, described silica gel adopts 70～320 order silica gel; The condition of described oven dry can be put dry 24h in the baking oven of 160 ℃; The addition of described water can be 5% of silica gel by mass percentage; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
4. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 1, is characterized in that in step 3), and the consumption of described oil sample is 5mL; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1; The addition of described sherwood oil and ether mixed solution can be 60mL; Described wash-out can adopt double-stranded ball pressure method wash-out, and the speed of described wash-out can be 1.5mL/min.
5. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 1, is characterized in that in step 4), and described evaporate to dryness can adopt to revolve and steam instrument evaporate to dryness, heating water bath evaporate to dryness or heating plate heating evaporate to dryness; In step 5), described investigation nonpolarity element separating effect can be investigated by thin-layer chromatography.
6. an assay method for edible oil and fat Semi-polarity composition, is characterized in that comprising the following steps:
1) semisolid or solid sample are dissolved, filter, then oil sample is dissolved in sherwood oil and ether mixed solution, and be settled to 10mL;
2) silica gel is dried, then add water after being cooled to room temperature, then be transferred in injector syringe, pier is real, adds sea sand or silica sand, then adds sherwood oil and ether mixed solution along needle cylinder wall, makes silica gel wetting;
3) when concordant with sea sand or quartz sand surface on sherwood oil and ether mixed solution surface, oil sample be dissolved in chromatographic column, then add sherwood oil and ether mixed solution to carry out wash-out to nonpolarity element, it is m that eluent is collected in to quality
1the 1st flask or the 1st beaker in;
4) after step 3) wash-out nonpolarity element, continue polar component wash-out, it is m that eluent is collected in to quality
2the 2nd flask or the 2nd beaker in;
5) by the eluent evaporate to dryness in step 4) flask or beaker, weigh, obtaining proper mass is m
2flask or the evaporate to dryness of beaker after quality be m
4;
6) investigate nonpolarity element separating effect;
7) calculate
If during wash-out nonpolarity element, the computing formula of polar component content is:
If during wash-out polar component, the computing formula of polar component content is:
In formula:
X: polar component content, %;
M: determined oil sample quality, g;
M
1: the quality of the 1st flask or the 1st beaker, g;
M
2: the quality of the 2nd flask or the 2nd beaker, g;
M
3: nonpolarity element quality sum in the 1st flask or the 1st beaker and oil sample, g;
M
4: the 2nd flask or the 2nd beaker and oil sample Semi-polarity composition quality sum, g.
7. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 6, is characterized in that in step 1), and described filtration adopts Filter paper filtering; The consumption of described oil sample is 1g, is preferably accurate to 0.001g, and the volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
8. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 6, is characterized in that in step 2) in, described silica gel adopts 70～320 order silica gel; The condition of described oven dry can be put dry 24h in the baking oven of 160 ℃; The addition of described water can be 5% of silica gel by mass percentage; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1.
9. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 6, is characterized in that in step 3), and the consumption of described oil sample is 5mL; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1; The addition of described sherwood oil and ether mixed solution can be 60mL; Described wash-out can adopt double-stranded ball pressure method wash-out, and the speed of described wash-out can be 1.5mL/min.
10. a kind of assay method of edible oil and fat Semi-polarity composition as claimed in claim 6, it is characterized in that in step 4), described continuation by the concrete grammar of polar component wash-out is: at sherwood oil and ether mixed solution surface and sea sand or quartz sand surface when substantially concordant, add eluant, eluent ether and adopt double-stranded ball pressure method to carry out wash-out to polar component, elution speed is 1.5mL/min; The volume ratio of described sherwood oil and ether mixed solution PetroChina Company Limited.'s ether and ether can be 9: 1; The addition of described sherwood oil and ether mixed solution can be 50mL;
In step 5), described evaporate to dryness can adopt to revolve and steam instrument evaporate to dryness, heating water bath evaporate to dryness or heating plate heating evaporate to dryness;
In step 6), described investigation nonpolarity element separating effect can be investigated by thin-layer chromatography.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104459010A (en) * | 2014-12-13 | 2015-03-25 | 广西科技大学 | Method for qualitatively detecting waste cooking oil |
| CN107064109A (en) * | 2017-04-18 | 2017-08-18 | 厦门大学 | A kind of method for detecting Benzene in Beverages formic acid |
| CN111458257A (en) * | 2020-04-03 | 2020-07-28 | 青岛天祥食品集团有限公司 | Method for detecting content of filter aid and phospholipid in pressed peanut oil filter residue |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453064A (en) * | 2002-04-27 | 2003-11-05 | 北京市优力凯生物技术有限责任公司 | Method of screening chromatographic stuffing from pearlite |
| CN101647778A (en) * | 2009-06-26 | 2010-02-17 | 郑州后羿制药有限公司 | Preparation method of tilmicosin liposomes |
-
2013
- 2013-11-28 CN CN201310625381.8A patent/CN103592198A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1453064A (en) * | 2002-04-27 | 2003-11-05 | 北京市优力凯生物技术有限责任公司 | Method of screening chromatographic stuffing from pearlite |
| CN101647778A (en) * | 2009-06-26 | 2010-02-17 | 郑州后羿制药有限公司 | Preparation method of tilmicosin liposomes |
Non-Patent Citations (5)
| Title |
|---|
| 中华人民共和国卫生部 等: "《GB/T 5009.202-2003 》", 11 August 2003 * |
| 卢志兵 等: "关于地沟油极性组分指标的研究", 《食品安全质量检测学报》 * |
| 李德海: "《食品化学分析技术》", 31 July 2012, 东北林业大学出版社 * |
| 赵超敏 等: "快速测定煎炸油中极性组分的方法", 《中国油脂》 * |
| 黄泽元: "《食品分析实验》", 31 January 2013, 郑州大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104459010A (en) * | 2014-12-13 | 2015-03-25 | 广西科技大学 | Method for qualitatively detecting waste cooking oil |
| CN104459010B (en) * | 2014-12-13 | 2016-06-08 | 广西科技大学 | A kind of method of qualitative detection hogwash fat |
| CN107064109A (en) * | 2017-04-18 | 2017-08-18 | 厦门大学 | A kind of method for detecting Benzene in Beverages formic acid |
| CN111458257A (en) * | 2020-04-03 | 2020-07-28 | 青岛天祥食品集团有限公司 | Method for detecting content of filter aid and phospholipid in pressed peanut oil filter residue |
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