CN102901744A - Method for detecting authenticity of peanut oil - Google Patents
Method for detecting authenticity of peanut oil Download PDFInfo
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- CN102901744A CN102901744A CN2012104442971A CN201210444297A CN102901744A CN 102901744 A CN102901744 A CN 102901744A CN 2012104442971 A CN2012104442971 A CN 2012104442971A CN 201210444297 A CN201210444297 A CN 201210444297A CN 102901744 A CN102901744 A CN 102901744A
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Abstract
The invention discloses a method for detecting authenticity of peanut oil, and relates to a method for detecting vegetable oil. The method comprises the following steps of: measuring a liquid oil sample to be detected; dissolving the sample by using a deuterated solvent, and transferring the solution to a nuclear magnetic tube for later detection; acquiring data of 1H hydrogen spectrum and 13C carbon spectrum of the sample through a nuclear magnetic resonance spectrometer; and analyzing the data, namely carrying out integral analysis on the data through nuclear magnetic spectrogram fingerprint peak comparison analysis of the peanut oil by virtue of R software, calculating the relative content of components of each main fatty acid in the sample to obtain the proportion of oxidative products and free fatty acids when the content of the total fatty acid is 100 percent, and obtaining an identification result according to multiple indexes. The method is easy to operate, accurate in measurement and high in repeatability; through nondestructive detection of the sample, the same sample can be used for repeated measurement or other analysis and test, and the measurement result is not influenced by skills and judgment of operators; and the method is suitable for quick detection of the peanut oil.
Description
Technical field
The present invention relates to the detection method of a vegetable oil, especially relate to a kind of discrimination method of the peanut oil true and false.
Background technology
Peanut oil is the third-largest edible oil of China, and its use amount is only second to rapeseed oil and soybean oil, and peanut oil is celebrated with nutritious, belongs to one of the highest edible oil of price in market.Peanut oil can make cholesterol in human body be decomposed into bile acid and excrete, thereby reduces the content of cholesterol in the blood plasma.In addition, also contain wheat germ phenol, phosphatide, vitamin E, choline etc. in the peanut oil to human body beneficial's material.Often edible peanut oil can prevent that chapped skin is aging, and the protection vascular wall prevents thrombosis, helps prevention of arterial sclerosis and coronary heart disease.Choline in the peanut oil also can improve the memory of human brain, delays brain function decline.
According to national standard, must not add any essence and spices in the peanut oil, must not be mixed with other edible oils and unedible oil; Product should mark the production name of the country of quality grade and raw material; Squeezing finished product peanut oil, leaching finished product peanut oil will mark respectively " squeezing " and " leaching " printed words in Product labelling.
Peanut oil is our current consumption product, in recent years because the continuous rising of price, indivedual illegal businessmans are subjected to the driving of interests, so played the idea of mingling in the peanut oil production run, the numerous peanut oil of brand on the market, quality is uneven, and for consumers, light is difficult to judge exactly to be pure peanut oil from outward appearance.
The peanut oil of marking identical manufacturing process and quality grade equally, but the price of different brands differ near half.Does this allow a lot of citizen not understand, and is expensive price virtual height, or cheap quality has problem? recently, various low price peanut oil are sold fiery in market, and these low price peanut oil not only appear on the market of farm produce, but also have appeared on the sales counter of large supermarket.Some at a low price peanut oil inferior be not peanut oil, be the mixed oil of palm oil and rapeseed oil in fact, the model oil of bottle cap is actually and has added essence, sends of short duration peanut fragrance temptation client.Peanut oil at a low price unlike label declare belong to ' special fragrant flower oil generation ', but the formulated oil that may more or less mix other cheap vegetable oil, peanut oil inferior has been blent let off fireworks what of oil generation of basis that salad oil produces with a small amount of peanut oil, and the peanut oil of OEM fraud also divides different class.
Country is after having carried out a series of cleaning up to the peanut oil true and false, and the peanut oil true and false is at leisure away from our dining table.But by reporter's investigation discovery, fake and forged peanut oil still is flooded with the market of rural area and remote districts.Believe and only have the source, fake and forged peanut oil is hit in multidisciplinary associating, could purify edible oil market, and then allows the harm of common people away from poor oil.
At present, the technological means of domestic detection peanut oil has that thin-layer chromatography, fluorescence spectrum, gas chromatography coupling mass spectrum (GC-MS), electricity are led, gas chromatography (GC), atomic absorption spectrum and plasma be coupled mass spectrum (ICP-MS).In the existing state compulsory standard " edible vegetable oil hygienic standard " (2716-2005), the physics and chemistry of edible oil detects index and comprises the indexs such as acid value, peroxide value, leaching oil solvent are residual, free phenol (cottonseed oil), total arsenic, lead, aflatoxin.
Nuclear magnetic resonance (NMR) technology is to study on the whole the technology of complex material system, is applied in the food evaluation.Nuclear magnetic resoance spectrum can be realized Non-Destructive Testing, nuclear-magnetism
1H hydrogen spectrum and
13C carbon spectrum reflection molecular structures feature can be identified exactly to fatty acid compositions all in the laboratory sample, can obtain various fatty acid quick nondestructive and form.Nuclear magnetic spectrogram is a kind of dactylogram, can carry out the Rapid identification of vegetable oil by independently developed software, and these class methods do not destroy the composition of sample, does not need determination, does not have complicated sample preparation process.Nuclear magnetic spectrogram can be realized the discriminating of structure of matter composition and relative content, therefore has a wide range of applications in fields such as quality monitoring, safety inspections.
Chinese patent CN102221533A discloses a kind of peanut oil based on ultraviolet and mixes pseudo-quantitative detecting method, and the method utilizes ultraviolet spectrophotometer as testing tool.Utilize the different of the oily ultraviolet spectrum characteristic of peanut oil and other peak during mensuration, mensuration characteristic wave strong point light absorption value and known peanut oil are mixed pseudo-amount and are set up model, mix pseudo-amount with model prediction again.
Chinese patent CN101482494A discloses a kind of detector for adulterated peanut oil and adulterated peanut oil detection method.The method is used the voluntarily detector of development, and the cuvette that testing sample is housed is put into 40 ℃ of constant temperature 10min of pre-processing module, then takes out the cuvette that testing sample is housed and puts into 3～4 ℃ of modules of constant temperature oven and detect; Detect 25min, detection signal generates detection curve by microprocessor between detection period, bit processor is arranged with detection curve and Standard Curve Database Plays curve comparison, output detections result.
Summary of the invention
The object of the present invention is to provide a kind of detection method of the peanut oil true and false.
The present invention includes following steps:
1) measures the testing liquid oil samples;
2) with the deuterated solvent dissolution sample, and transfer in the nuclear magnetic tube to be measured;
3) by the nuclear magnetic resonance analyser collected specimens
1H hydrogen spectrum and
13C carbon spectrum data;
4) data analysis, by peanut oil nuclear magnetic spectrogram fingerprint peaks compare of analysis, in conjunction with R software data are carried out holistic approach, calculate various main fatty acid composition relative contents in the sample, obtain the ratio that oxidation product and free fatty acid account for when total fatty acid content is a hundred per cent, judges by many index to obtain qualification result.
In step 1), the amount of described testing liquid oil samples can be 5～500 μ L.
In step 2) in, described deuterated solvent can be selected from deuterated methanol, a kind of in benzene etc. of deuterochloroform, deuterium.
In step 3), described high-field nuclear magnetic resonance instrument can adopt 300MHz and above high-field nuclear magnetic resonance instrument.
In step 4), described data analysis is concrete composition, acidity, the oxidizability of automatically calculating sample by spectral data being imported R software; Described many index judgement refers to following index:
(1) nuclear magnetic resonance characteristic fingerprint hydrogen spectrum, the comparison of characteristic fingerprint carbon spectrum;
(2) the normal contained linolenic amount of peanut oil is below 1%, and normal peanut oil contains arachidic acid;
(3) characteristic fatty acid of normal peanut oil forms: peanut oil contains unsaturated fatty acid more than 78%, oleic acid 38% ~ 44%, and linoleic acid 35% ~ 37% also contains palmitic acid, the saturated fatty acids such as stearic acid and arachidic acid 20% ~ 25% in addition;
Whether be peanut oil from above 3 indexs to sample, perhaps whether adulterated peanut oil, even there is one defectively to judge that namely product is non-pure peanut oil if judging.
The present invention adopts the magnetic resonance differential method, and is simple to operate, measures accurately, repeatability is high, so that same sample can take multiple measurements or be used for other analytical test, measurement result is not subjected to operator's technology and judges that institute affects, and is suitable for the fast detecting of peanut oil to the Non-Destructive Testing of sample.
The fingerprint pattern technology that the present invention is based on NMR adopts advanced analytical technology, and by mathematical statistics and computer simulation, can carry out quality control and Quality Detection to peanut oil, estimates food quality from system and whole angle.Measure content of fatty acid in the peanut oil by NMR, can analyze the distribution situation of measured content of fatty acid, identify the peanut oil quality, differentiate and mingle oil or miscella.Nuclear magnetic resoance spectrum can also reflect the molecular structures feature, can accurately identify fatty acid compositions all in the laboratory sample, with quick nondestructive obtain various fatty acid and form.In addition, can carry out to the NMR data Rapid identification of oil product, and have other many advantages, such as the composition that does not destroy sample, do not need determination, do not have complicated sample preparation process etc., have a wide range of applications in fields such as food quality monitoring, safety inspections.
The characteristics of the detection method of a kind of peanut oil true and false of the present invention are:
1. quick, simple and direct, only need 5min the detection time of a sample.
2. sample nondestructive need not to carry out pre-treatment.
3. can be on any nuclear magnetic resonance analyser data acquisition.
4. automatically analyze by data importing software and provide the result.
5. there are not big-difference in whole data acquisition and analysis good stability because of the difference of using instrument.
6. the sample test of a 5min can obtain required multinomial information.(content of each main fatty acid of sample, the relative content of oxide, free fatty acid etc.).
7. this method can be judged the peanut oil of mingling, and also can judge its quality quality by its acidity, oxidizability and degree of unsaturation to the peanut oil of not mingling.
Description of drawings
Fig. 1 is normal peanut oil
1H hydrogen spectrum; In Fig. 1, horizontal ordinate is chemical shift (ppm); The peak in chemical shift 0.5～5.5ppm interval is the characteristic fingerprint peak.
Fig. 2 is normal peanut oil
13C carbon spectrum; In Fig. 2, horizontal ordinate is chemical shift (ppm); The peak in chemical shift 10.0～175.0ppm interval is the characteristic fingerprint peak.
Embodiment
Embodiment 1～6
Measure 300 μ L peanut oil in nuclear magnetic tube, add deuterated solvent, obtain testing sample.Gather with high-field nuclear magnetic resonance spectrometer
1H hydrogen spectrum as Fig. 1 with
13C carbon spectrum obtains at first relatively existing such as Fig. 1 behind the spectrogram such as Fig. 2
1The characteristic fingerprint peak in H hydrogen spectrum chemical shift 0.0～6.0ppm interval; Relatively exist such as Fig. 2
13The characteristic fingerprint peak in C spectrum chemical shift 0.0～190.0ppm interval.
Table 1
Derive simultaneously raw data, carry out computing with R software, obtain the concrete composition of fatty acid and saturation degree, relative acidity and relative oxidizability, obtain the result as shown in table 1.
Claims (6)
1. the detection method of a peanut oil true and false is characterized in that may further comprise the steps:
1) measures the testing liquid oil samples;
2) with the deuterated solvent dissolution sample, and transfer in the nuclear magnetic tube to be measured;
3) by the nuclear magnetic resonance analyser collected specimens
1H hydrogen spectrum and
13C carbon spectrum data;
4) data analysis, by peanut oil nuclear magnetic spectrogram fingerprint peaks compare of analysis, in conjunction with R software data are carried out holistic approach, calculate various main fatty acid composition relative contents in the sample, obtain the ratio that oxidation product and free fatty acid account for when total fatty acid content is a hundred per cent, judges by many index to obtain qualification result.
2. the detection method of a kind of peanut oil true and false as claimed in claim 1 is characterized in that in step 1), and the amount of described testing liquid oil samples is 5～500 μ L.
3. the detection method of a kind of peanut oil true and false as claimed in claim 1 is characterized in that in step 2) in, described deuterated solvent is selected from deuterated methanol, a kind of in the benzene of deuterochloroform, deuterium.
4. the detection method of a kind of peanut oil true and false as claimed in claim 1 is characterized in that in step 3), and described high-field nuclear magnetic resonance instrument adopts 300MHz and above high-field nuclear magnetic resonance instrument.
5. the detection method of a kind of peanut oil true and false as claimed in claim 1 is characterized in that in step 4), and described data analysis is concrete composition, acidity, the oxidizability of automatically calculating sample by spectral data being imported R software.
6. the detection method of a kind of peanut oil true and false as claimed in claim 1 is characterized in that in step 4), and described many index judgement refers to following index:
(1) nuclear magnetic resonance characteristic fingerprint hydrogen spectrum, the comparison of characteristic fingerprint carbon spectrum;
(2) the normal contained linolenic amount of peanut oil is below 1%, and normal peanut oil contains arachidic acid;
(3) characteristic fatty acid of normal peanut oil forms: peanut oil contains unsaturated fatty acid more than 78%, oleic acid 38% ~ 44%, and linoleic acid 35% ~ 37% also contains palmitic acid, the saturated fatty acids such as stearic acid and arachidic acid 20% ~ 25% in addition;
Whether be peanut oil from above 3 indexs to sample, perhaps whether adulterated peanut oil, even there is one defectively to judge that namely product is non-pure peanut oil if judging.
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| CN2012104442971A CN102901744A (en) | 2012-11-08 | 2012-11-08 | Method for detecting authenticity of peanut oil |
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| CN2012104442971A CN102901744A (en) | 2012-11-08 | 2012-11-08 | Method for detecting authenticity of peanut oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103389318A (en) * | 2013-07-24 | 2013-11-13 | 厦门大学 | Method for identifying true and false beef and mutton |
| CN105092628A (en) * | 2015-07-21 | 2015-11-25 | 中国农业科学院农业质量标准与检测技术研究所 | Method for discriminating milk product quality |
| CN105510372A (en) * | 2016-01-27 | 2016-04-20 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for building model for DPLS-BS-UVE rapid honey identification |
| CN106908509A (en) * | 2017-02-08 | 2017-06-30 | 北京农业质量标准与检测技术研究中心 | The quick and quantitative detecting method of doping paraffin in a kind of lard |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102221533A (en) * | 2011-06-09 | 2011-10-19 | 西北农林科技大学 | Method for quantitatively detecting adulteration of peanut oil based on ultraviolet spectrum |
| CN102269720A (en) * | 2011-04-28 | 2011-12-07 | 王士桥 | Method for identifying edible oil quality through combination of nuclear magnetic resonance and pattern recognition method |
| CN102706915A (en) * | 2012-06-28 | 2012-10-03 | 厦门大学 | Method for detecting illegal cooking oil |
-
2012
- 2012-11-08 CN CN2012104442971A patent/CN102901744A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102269720A (en) * | 2011-04-28 | 2011-12-07 | 王士桥 | Method for identifying edible oil quality through combination of nuclear magnetic resonance and pattern recognition method |
| CN102221533A (en) * | 2011-06-09 | 2011-10-19 | 西北农林科技大学 | Method for quantitatively detecting adulteration of peanut oil based on ultraviolet spectrum |
| CN102706915A (en) * | 2012-06-28 | 2012-10-03 | 厦门大学 | Method for detecting illegal cooking oil |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局: "《中华人民共和国国家标准 花生油 GB 1534 2003》", 11 November 2003, article ""花生油"" * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103389318A (en) * | 2013-07-24 | 2013-11-13 | 厦门大学 | Method for identifying true and false beef and mutton |
| CN103389318B (en) * | 2013-07-24 | 2016-12-28 | 厦门大学 | A kind of method differentiating true and false beef and mutton |
| CN105092628A (en) * | 2015-07-21 | 2015-11-25 | 中国农业科学院农业质量标准与检测技术研究所 | Method for discriminating milk product quality |
| CN105510372A (en) * | 2016-01-27 | 2016-04-20 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for building model for DPLS-BS-UVE rapid honey identification |
| CN106908509A (en) * | 2017-02-08 | 2017-06-30 | 北京农业质量标准与检测技术研究中心 | The quick and quantitative detecting method of doping paraffin in a kind of lard |
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Application publication date: 20130130 |