CN108982570A - A kind of edible oil quality discrimination method based on nuclear magnetic resonance technique - Google Patents
A kind of edible oil quality discrimination method based on nuclear magnetic resonance technique Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
Abstract
The invention discloses a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique: 1) standard plant edible oil sample and exceeded edible oil sample are collected；2) magnetic resonance detection is carried out to each sample, collects high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum；3) whether contrast standard edible oil and exceeded edible oil spectrogram find difference between the two, then identified according to difference substance exceeded；4) high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum is pre-processed to obtain two-dimensional integration data, establishes standard edible oil component and quality database；5) two-dimensional integration data is handled directly using standard edible oil component and quality database unified standard setting ingredient and quality indicator threshold, design MATLAB program to identify the quality or type of edible oil.Above-mentioned method can quickly, expeditiously identify variety classes edible oil and adulterated or underproof edible oil.
Description
Technical field
The invention belongs to analysis technical fields, and in particular to the edible oil quality discrimination method based on nuclear magnetic resonance technique.
Background technique
In mankind's daily life, edible oil is closely bound up daily necessities of living with people.Edible oil can provide
The nutriment beneficial to human health such as sitosterol, unsaturated fatty acid, oryzanol.It is most popular in China market at present
Edible oil mainly includes soybean oil, peanut oil, rapeseed oil, sunflower oil, sesame oil, corn oil, olive oil.Different types of food
It is quite similar with oily main component, but its price and the content difference of its ingredient and related with nutritive value, therefore price difference
Different very big, this also causes some illegal retailers to mix using exceeded or cheap edible oil with expensive edible oil, disguises oneself as
High price edible oil obtains higher interests, seriously compromises the interests of consumer, compromises the health of the mankind.Mixing edible oil be by
Edible oil made of two or more pure edible oil is mixed in a certain ratio.Mixing edible oil is by pure edible oil
Mix the gutter oil and frying oil that exceeded edible oil includes high risk.Gutter oil and frying oil are long term high temperature heating
Edible oil, this process can generate various harmful substances.Even across filtering and purifying, a variety of in exceeded edible oil toxic have
Evil substance is also difficult to remove.But this edible oil is relatively difficult by appearance or smell identification, it is very big to human health damage.
Additional mixing edible oil further includes the high price edible oil mixed with cheap edible oil, the olive oil such as mixed with soybean oil.It is this to mix
Vacation is not only our focus of attention and the most common method for reducing cost of illegal transaction person.But it is this adulterated more private
It is close, the health of consumer will not be endangered, therefore often ignored by ordinary consumer.So carrying out identification pair to the quality of edible oil
Consumer and the manager in Food circulation field have important meaning, and can establish for corresponding system and provide reference price
Value, provides feasible method for the quality control evaluation of edible oil.
Current technological means is that we provide multiple eating oil discrimination methods.However, traditional chemical method often needs
Want various chemical apparatuses and reagent and professional operation laboratory apparatus.The detection of mass parameter takes a long time, it is impossible to be used in
Quickly screening.Therefore, develop a kind of method that edible oil is quickly analyzed to the quality monitoring for improving edible oil enterprise, ensure edible
The equity of oily consumption market and consumer are of great significance.
Summary of the invention
The main technical problem to be solved by the present invention is to provide a kind of, and the edible oil quality based on nuclear magnetic resonance technique reflects
Other method can quickly, expeditiously identify variety classes edible oil, adulterated or underproof edible using the method for the present invention
Oil, it is economical and practical, it is convenient and efficient, can effectively improve supervision department's efficiency, guarantee purchase edible oil consumer equity and
Health, convenient for promoting the use of.
In order to solve the above technical problems, the present invention provides a kind of, and the edible oil quality based on nuclear magnetic resonance technique reflects
Other method, including the following steps:
1) standard plant edible oil sample and exceeded edible oil sample are collected；
2) magnetic resonance detection is carried out to each sample, collects high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum；And
After switch to step 3 or step 4；
3) design MATLAB program comparison conventional edible oils and exceeded edible oil spectrogram, find difference between the two, then
Whether exceeded identified according to difference substance；
4) high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum is pre-processed to obtain two-dimensional integration data, carries out statistical number
The ownership of edible oil component small molecule characteristic peak is obtained according to analysis, calculates variety classes edible oil component and quality using characteristic peak
Index, to establish standard edible oil component and quality database；
5) standard edible oil component and quality database unified standard setting ingredient and quality indicator threshold, design are utilized
MATLAB program handles two-dimensional integration data directly to identify the quality or type of edible oil.
In a preferred embodiment: the standard plant edible oil sample refers to buying in supermarket or scientific research institution purchases
It buys, meet the vegetable edible oil that country uses standard；The exceeded edible oil sample is that street pedlar uses repeatedly or not on street
The edible oil of bright approach.
In a preferred embodiment: in step 2, magnetic resonance detection is complete on the nuclear magnetic resonance spectrometer of Brooker 600MHz
At: pulse train: zg30, scanning stacking fold: 32 times, relaxation delay: 1 second, single acquisition time: 4.95 seconds, acquisition points:
32K, spectrum width: 6613.8Hz, experimental situation are controlled by spectrometer in 298K.
In a preferred embodiment: in step 4, the high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum collected is used
MestReNova software is pre-processed, and obtain after full spectrum normalization every behavioural analysis sample, every to treated spectrogram
It is classified as the two-dimensional matrix of edible oil component small molecule information, finally the characteristic peak of edible oil component small molecule is belonged to.
In a preferred embodiment: in step 5, the integral of integrating range where superposition edible oil component small molecule characteristic peak
Value calculates variety classes edible oil component and quality index by formula, so obtain the standard setting of each edible oil at
Point and quality indicator threshold.
In a preferred embodiment: the identification logic of MATLAB program are as follows:
1) exceed standard material characteristic peak that may be present is first detected, if there is exceed standard material, is then directly determined as exceeded food
With oil；
2) edible with each if it is not detected that exceed standard material, then calculate the value of main component and relevant parameter
Standard setting ingredient and the quality indicator threshold comparison of oil, provide judging result if the parameter for meeting a certain edible oil；If
It is unsatisfactory for carrying out linear analysis to ingredient into mixing edible oil decision logic with regard to recurrence, obtains the composition result of composition sample.
Compared to the prior art, technical solution of the present invention have it is following the utility model has the advantages that
The present invention provides a kind of edible oil quality discrimination methods, are reflected using the edible oil quality based on nuclear magnetic resonance technique
Other method provides technical support to design program software according to edible oil parameter database to identify for edible oil quality.This hair
The bright food group method based on NMR spectrum technology detects different types of conventional edible oils and exceeded edible oil
To corresponding original figure spectrum, conventional edible oils and exceeded edible oil spectrogram are compared, finds out both exceed standard material peak verifyings interstitial
Difference, and the characteristic peak by map being further analyzed edible oil component are measured, to calculate the mark of each edible oil
Quasi- setting ingredient and quality indicator threshold, can be effectively quasi- using the data of designed program software and these threshold values before
It really distinguishes different types of edible oil and edible oil is adulterated.Detection food samples can be obtained using the method for the present invention
To a large amount of, multidimensional the information abundant in relation to food macromolecular or small molecule.Using based on NMR spectrum technology
It is adulterated that food group detects edible oil, can be adulterated and quality provides brand-new, convenient and fast technology for supervision department's supervision edible oil
Method has important economic and social benefit.
Detailed description of the invention
Fig. 1 is that u fatty acid molecule signal is composed in (0.5-5.5ppm) in soybean oil (SO) and the one-dimensional hydrogen of sesame oil (SE)
Ownership, the region of 3.0-5.5ppm is by 4 times of vertical magnification.
Fig. 2 is variety classes standard edible oil principal component analysis shot chart.
Fig. 3 is that exceeded edible oil (gutter oil, frying oil) and the nmr spectrum of standard edible oil compare.
Fig. 4 is the expert system operating result page；
Fig. 5 is mixing edible oil principal component analysis shot chart (rapeseed oil, soybean oil, peanut oil and olive oil).
Specific embodiment
Below with reference to specific implementation example, the present invention is further illustrated:
A kind of edible oil quality discrimination method based on nuclear magnetic resonance technique, including the following steps:
1) standard plant edible oil sample and exceeded edible oil sample are collected；
2) magnetic resonance detection is carried out to each sample, collects high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum；And
After switch to step 3 or 4；
3) design MATLAB program comparison conventional edible oils and exceeded edible oil spectrogram, find difference between the two, then
Whether exceeded identified according to difference substance；
4) high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum is pre-processed to obtain two-dimensional integration data, carries out statistical number
The ownership of edible oil component small molecule characteristic peak is obtained according to analysis, calculates variety classes edible oil component and quality using characteristic peak
Index, to establish standard edible oil component and quality database；
5) standard edible oil component and quality database unified standard setting ingredient and quality indicator threshold, design are utilized
MATLAB program handles two-dimensional integration data directly to identify the quality or type of edible oil.
Specifically, the standard plant edible oil sample refers to buying in supermarket or scientific research institution buys, meets
Country uses the vegetable edible oil of standard；The exceeded edible oil sample is that street pedlar uses multiple or unknown approach on street
Edible oil.
In step 2, magnetic resonance detection is completed on the nuclear magnetic resonance spectrometer of Brooker 600MHz: pulse train: zg30,
Scan stacking fold: 32 times, relaxation delay: 1 second, single acquisition time: 4.95 seconds, acquisition points: 32K, spectrum width:
6613.8Hz, experimental situation are controlled by spectrometer in 298K.
In step 3, the high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum collected is carried out pre- using MestReNova software
Processing carries out obtaining every behavioural analysis sample after full spectrum normalization, is often classified as edible oil component small molecule to treated spectrogram
The two-dimensional matrix of information finally belongs to the characteristic peak of edible oil component small molecule.
In step 4, the integrated value of integrating range, is calculated not by formula where superposition edible oil component small molecule characteristic peak
With type edible oil component and quality index, and then obtain the standard setting ingredient and quality indicator threshold of each edible oil.
In step 4, the identification logic of MATLAB program are as follows:
1) exceed standard material characteristic peak that may be present is first detected, if there is exceed standard material, is then directly determined as exceeded food
With oil；
2) edible with each if it is not detected that exceed standard material, then calculate the value of main component and relevant parameter
Standard setting ingredient and the quality indicator threshold comparison of oil, provide judging result if the parameter for meeting a certain edible oil；If
It is unsatisfactory for carrying out linear analysis to ingredient into mixing edible oil decision logic with regard to recurrence, obtains the composition result of composition sample.
Hereafter it is illustrated by the experiment embodiment of distance:
1. research object
The present embodiment collects 7 types and adds up to 49 regular edible oil samples, wherein 6 sunflower oil samples (SS), 6
Vegetable seed oil samples (RA), 6 soybean oil samples (SO), 6 peanut oil samples (PE), 6 corn oil samples (CO), 4 olives
Oil samples (OL) and 15 sesame oil samples (SE).Having 5 in 49 samples is the mark from Institute of Science and Technology, National Food Bureau
Quasi- edible oil sample (including soybean oil, peanut oil, sunflower oil, corn oil and sesame oil) is remaining to purchase in large supermarket
It buys.In addition, collecting exceeded edible oil used in 7 kinds of street pedlars, including gutter oil and frying oil sample.7 kinds of exceeded oil sample sheets,
Two of them are gutter oil (No. 1 and No. 2 exceeded oil), and one is the oil with common edible (No. 3 exceeded oil) for mixing 20% gutter oil,
One is high erucic acid edible oil (No. 4 exceeded oil), there are two be respectively the oil with common edible (No. 5 exceeded oil) stored for a long time and
The edible oil (No. 6 exceeded oil) of emulsion deterioration, the last one is the frying oil (No. 7 exceeded oil) independently refined.Final gained
Sample is 56 edible oil samples.
2. reagent and instrument and equipment
Experiment reagent includes deuterated chloroform (tetramethylsilane containing 0.03%), deuterated dimethyl sulfoxide.
Testing consumptive material includes 5mm nuclear magnetic tube, 50mL EP pipe, marking pen, emgloves, mask.
Experimental facilities includes 100 μ L, 200 μ L, 500 μ L microsyringes, oscillator, Brooker 600MHz nuclear magnetic resoance spectrum
Instrument.
3. the collection and pretreatment of sample
Packing moves into 50mL EP pipe behind edible oil packing Kaifeng, is put into 277K refrigerator until sample.It, will when sample
50 μ L edible oil samples are dissolved in the organic solvent CDCl containing 0.03%TMS (tetramethylsilane, for calibrating) of 300 μ L3(deuterium
For chloroform, deuterated rate 99.8%) in, while the DMSO-d of 250 μ L of additional addition6(deuterated dimethyl sulfoxide).Solution is shaken
5mm nuclear magnetic tube is moved into the uniformly rear 500 μ L that take out, sealing is put into 277K refrigerator, stands the experiment of waiting in 12 hours.
4. nuclear magnetic resonance spectroscopy
Nuclear magnetic resonance experiment is completed on the nuclear magnetic resonance spectrometer of the Brooker 600MHz equipped with CryoProbeTM, is tested
Temperature setting is 298K, and the resonant frequency of hydrogen is 600.13MHz.Edible oil sample selection zg30 sequence is detected, and acquisition is just
Advise the high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum of edible oil and exceeded edible oil sample.Sampling parameter is as follows: scanning times: 32
It is secondary；Relaxation delay: 1s；Sampling time: 4.95s；Sampling number: 32K；Spectrum width: 6613.8Hz.
5. after the high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum for obtaining regular edible oil and exceeded edible oil sample, so that it may
Conventional edible oils and exceeded edible oil spectrogram are compared by design MATLAB program, difference between the two is found, then according to difference
Whether foreign substances identify exceeded.
For exceeded edible oil, we compare the spectrogram with normal edible oil, and Fig. 3 has found exceeded edible oil some
Region will appear apparent variation (such as 9.50ppm aldehyde material increases sharply or the decline of the double bond methine peak 5.30ppm), utilize
The judgement of these exceed standard materials can directly give the judgement of unqualified edible oil.
If 6. also need to distinguish the type of edible oil, need to compose high-resolution one-dimensional nuclear magnetic resonance hydrogen into
Row pretreatment.
Using MestReNova, v.9.0.1 software carries out in Fu the high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum collected
The pretreatments such as leaf transformation, phasing, baseline correction, spectral peak calibration, remaining water peak removal, to treated, spectrogram is integrated
Every behavioural analysis sample is obtained with after full spectrum normalization, is often classified as the two-dimensional matrix of edible oil component small molecule information, edible oil
The documents and materials that the ownership of ingredient small molecule feature spectral peak refers to the database of KEGG, HMDB and delivered, have belonged to spy out
Sign peak information is shown in Fig. 1 and table 1.
The NMR Assignments of main component in the one-dimensional hydrogen spectrum of 1. edible oil of table
Spectral peak multiplicity: s, singlet；D, doublet；T, triplet；Dd, doublet of doublets；M, multiplet；Br, broad peak
UFA, unsaturated fatty acid；TG, triglycerides；DG, diglyceride
7. multivariable and univariate statistics analysis
Two-dimensional matrix is imported into 14.0 software of SIMCA and carries out multivariate statistical analysis, mainly includes principal component analysis
(PCA), the data Standard graduation conversion mode that principal component analysis uses centralization to convert.It can be seen that me from the PCA shot chart of Fig. 2
It can be seen that edible oil component of the same race is similar to flock together well, and the edible oil that ingredient has differences can be
It is well distinguished out on two principal component directions.Component difference is bigger, and sample, which is just got, more to be opened, and it is edible to imply variety classes
Oil can be distinguished by component substances.
8. calculating and the edible oil judging standard of edible oil component and mass parameter.
According to formula (1)-(6), can calculate linolenic acid, linoleic acid, oleic acid and saturated fatty acid percentage composition,
The iodine number and acid value of edible oil.
[linolenic acid]=B/ (A+B) (1)
[linoleic acid]=(3E-4B)/[2 (A+B)] (2)
[4 (A+B)]-[linolenic acid]-[linoleic acid] (3) [oleic acid]=3D/
[saturated fatty acid]=A/ (A+B)-[linoleic acid]-[oleic acid] (4)
[iodine number]=(I/2-H/4)/[(A+B)/3] × 86 (5)
[acid value]=(C/2-3G/4-H/2-F/2)/(C/2) × 100% × [average molecular weight]/56 (6)
Calculate the ingredient and quality parameter thresholds judgment criteria such as table 2 of all edible oil.
The single edible oil judgment threshold of table 2.
Annotation: C18A, a degree of unsaturation content of fatty acid percentage；C18B, two degree of unsaturation content of fatty acid hundred
Divide ratio；C18C, three degree of unsaturation content of fatty acid percentages；C18O, saturated fatty acid content percentage.
For single edible oil, we, which determine, can directly give the information such as type, ingredient, iodine number, Fig. 4.Then I
Edible oil PCA shot chart according to the observation, Fig. 5, it is found that mixing edible oil exists relative to the purebred edible oil for participating in mixing
Score value in shot chart illustrates that mixed component content and mixed proportion have certain pass there are apparent linear dependence
Connection.We further calculate the edible oil ratio that component content discovery all main components of sample after mixing are equal and participation is mixed
Example is positively correlated.Our expert system takes the mode of changeable metric, can automatically remove the biggish unstable ginseng of fluctuation
Number retains relatively stable data, automatically analyzes mixed nature and calculate most accurate mixing ratio, finally combines error analysis,
A possibility that providing confidence level highest.
8.MATLAB software specialist's system determines result
We have imported 49 kinds of single edible oils, 10 kinds of actual measurement mixing edible oils, 48 kinds of simulation mixing edible oils and 7 kinds not
The two-dimensional information matrix data of qualified edible oil, final result show that single edible oil accuracy is 95.92%, actual measurement mixing food
It is 94.59% with oily accuracy, simulation mixing edible oil accuracy is 89.6%, and unqualified edible oil accuracy is 100%.
9. conclusion
A kind of edible oil quality identification side based on nuclear magnetic resonance technique of the present invention it can be seen from verifying above
Expert system software designed by method has good identification effect, and poor oil or exceeded oil can directly judge super subject matter
For mass peak to provide as a result, single edible oil can go out classification with Direct Identification, it is highest that mixing edible oil can provide confidence level
Two kinds mixing edible oils, that is, identify whether adulterated suspicion, we survey and simulation data accuracy also reached reason
The effect thought can be used for supervision department identification edible oil type, adulterated and quality, reduce testing cost, improves detection effect
Rate.
Food samples of the invention are conventional edible oils or exceeded edible oil, collect and treatment process is simple and convenient,
It spends low, belongs to Non-invaive examination, effectively increase edible oil and identify adulterated efficiency, reduce supervision department's testing cost,
To the quality monitoring for improving edible oil enterprise, ensures that the equity of edible oil consumption market and consumer are of great significance, have
Important economic and social benefit, it is easy to promote and utilize.
The foregoing is only a preferred embodiment of the present invention, but the design concept of the present invention is not limited to this,
Anyone skilled in the art in the technical scope disclosed by the present invention, using this design carries out the present invention non-
Substantive change belongs to the behavior for invading the scope of the present invention.
Claims (6)
1. a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique, it is characterised in that including the following steps:
1) standard plant edible oil sample and exceeded edible oil sample are collected；
2) magnetic resonance detection is carried out to each sample, collects high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum；Then turn
To execute step 3 or step 4；
3) design MATLAB program comparison conventional edible oils and exceeded edible oil spectrogram, find difference between the two, then basis
Whether difference substance identifies exceeded；
4) high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum is pre-processed to obtain two-dimensional integration data, carries out statistical data point
Analysis obtains the ownership of edible oil component small molecule characteristic peak, and the finger of variety classes edible oil component and quality is calculated using characteristic peak
Mark, to establish standard edible oil component and quality database；
5) standard edible oil component and quality database unified standard setting ingredient and quality indicator threshold, design are utilized
MATLAB program handles two-dimensional integration data directly to identify the quality or type of edible oil.
2. a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique as described in claim 1, it is characterised in that: institute
It states standard plant edible oil sample and refers to the plant food bought in supermarket or scientific research institution buys, meets country using standard
With oil；The exceeded edible oil sample is that street pedlar uses the edible oil of multiple or unknown approach on street.
3. a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique as described in claim 1, it is characterised in that: step
In rapid 2, magnetic resonance detection is completed on the nuclear magnetic resonance spectrometer of Brooker 600MHz: pulse train: zg30, scanning superposition time
Number: 32 times, relaxation delay: 1 second, single acquisition time: 4.95 seconds, acquisition points: 32K, spectrum width: 6613.8Hz, experimental situation
It is controlled by spectrometer in 298K.
4. a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique as described in claim 1, it is characterised in that: step
In rapid 3, the high-resolution one-dimensional nuclear magnetic resonance hydrogen spectrum collected is pre-processed using MestReNova software, to processing
Spectrogram afterwards carries out the Two-Dimensional Moment for obtaining every behavioural analysis sample after full spectrum normalization, being often classified as edible oil component small molecule information
Battle array, finally belongs to the characteristic peak of edible oil component small molecule.
5. a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique as claimed in claim 4, it is characterised in that: step
In rapid 4, it is edible to calculate variety classes by formula for the integrated value of integrating range where superposition edible oil component small molecule characteristic peak
Oil component and quality index, and then obtain the standard setting ingredient and quality indicator threshold of each edible oil.
6. a kind of edible oil quality discrimination method based on nuclear magnetic resonance technique as described in claim 1, it is characterised in that:
The identification logic of MATLAB program are as follows:
1) exceed standard material characteristic peak that may be present is first detected, if there is exceed standard material, is then directly determined as exceeded edible oil；
2) if it is not detected that exceed standard material, then calculate the value of main component and relevant parameter, with each edible oil
Standard setting ingredient and quality indicator threshold comparison, provide judging result if the parameter for meeting a certain edible oil；If discontented
Foot carries out linear analysis to ingredient into mixing edible oil decision logic with regard to recurrence, obtains the composition result of composition sample.
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