CN104198518A - Method for true and false identification and content determination of sesame oil - Google Patents
Method for true and false identification and content determination of sesame oil Download PDFInfo
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- CN104198518A CN104198518A CN201410495096.3A CN201410495096A CN104198518A CN 104198518 A CN104198518 A CN 104198518A CN 201410495096 A CN201410495096 A CN 201410495096A CN 104198518 A CN104198518 A CN 104198518A
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- oleum sesami
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Abstract
The invention provides a method for true and false identification and content determination of sesame oil. The method utilizes a low-field nuclear magnetic resonance technique to identify and determine the content of the sesame oil. The method mainly comprises the operation steps that 1, a mixed oil sample is prepared; 2, a detection sample is prepared; 3, relaxation signals of pure sesame oil, pure soybean oil and mixed oil are quickly determined by the low-field nuclear magnetic resonance technique; and 4, signal data is analyzed and processed. The method is easy and simple to operate and good in effect, can achieve quick detection of the content of the sesame oil in the sesame oil and soybean oil mixed sample, is applicable to the field of quality control of the pure sesame oil, and lays a foundation for quality detection work of the sesame oil.
Description
Technical field
The invention belongs to Oleum Sesami Quality Detection field, relate to a kind of method of utilizing low-field nuclear magnetic resonance technology to realize the discriminating of the Oleum Sesami true and false and assay.
Background technology
Present food security has become the topic that the common people are concerned about most.Because Oleum Sesami has higher economic worth, therefore, Oleum Sesami is mixed pseudo-phenomenon and detected is exactly the problem that society pays close attention to all the time.It is generally that non-oil substances or low price edible oil inferior are mixed in high-quality edible oil therefrom to make a profit that grease is mixed puppet.Research about Oleum Sesami detection of adulterations constantly has new progress.Although these methods can judge the quality of Oleum Sesami to a certain extent, the very difficult while to equipment and instrument operation requirements with to jointly taking into account aspect senior adulterated two targetedly, has certain limitation technician.Therefore, detect the method for Oleum Sesami quality in the urgent need to a kind of quick nondestructive.
In recent years, nuclear magnetic resonance has been widely used in each field as a kind of important modern analysis means.According to nuclear magnetic resonance principle, adopt specific pulse train to excite the atomic nucleus in sample with fixed magnetic moment, produce relaxation signals, this relaxation signals intensity is directly proportional to contained nuclear spin number in sample, and the constituent structure of signal attenuation process and measured matter is closely related.By mathematical method, relaxation signals is carried out to back analysis, can obtain various compositions and micromechanism information that other means are difficult to obtain, thereby reach testing goal.But up to now, there are no the report that utilizes low-field nuclear magnetic resonance technology to the adulterated assay of Oleum Sesami.
Compared with differentiating Oleum Sesami quality method with tradition, nuclear magnetic resonance technique can keep the integrality of sample; Method of operating is simple and quick, and measurement result is accurate; Measurement result is not subject to the impact of sample of material size and appearance luster.Therefore, nuclear magnetic resonance technique is a kind of new technology of very potential Oleum Sesami quality fast detecting.
The present invention fully recognizes the importance that Oleum Sesami quality is differentiated, and recognize the advantage of NMR (Nuclear Magnetic Resonance) relaxation time series analysis in Oleum Sesami Quality Detection, adopt low-field nuclear magnetic resonance technology for detection Oleum Sesami quality can not only greatly improve detection speed and accuracy, may realize real-time online simultaneously and detect.
Summary of the invention
The object of the invention is to for prior art above shortcomings, the method for the amount of a kind of quick discriminating and the adulterated soybean oil of detection Oleum Sesami is provided.
Following technical proposals of the present invention is for reaching above-mentioned technical purpose:
A method for the discriminating of the Oleum Sesami true and false and assay, comprises the steps:
1) make miscella sample: pure Oleum Sesami and pure soy bean are pressed to different proportion mixing, make multiple miscella samples, the volume percent content by soybean oil in Oleum Sesami is uniformly distributed from 0-100%, to ensure the representativeness of sample.
2) make and detect sample: draw oil sample respectively 3ml in 5ml centrifuge tube.
3) adopt low-field nuclear magnetic resonance technology to measure the relaxation spectrogram of pure Oleum Sesami, pure soy bean and miscella.
4) adopt chemometrics method treatment step 3) in the CPMG data that obtain, set up based on low-field nuclear magnetic resonance data, and for predicting the regression equation of adulterated ratio of sesame-soybean miscella, realize the fast detecting of Oleum Sesami.
As described in method, the wherein CPMG spectrogram parameter of the described working sample of step (3): 90 degree pulsewidth P
1: 4 μ s, 180 degree pulsewidth P
2: 8 μ s, repeated sampling stand-by period Tw:3500ms, analog gain RG1:[-3.0 to 40, is integer], digital gain DRG1:[0 to 7, be integer], pre-amp gain PRG:[0 to 3], repeated sampling times N S:4,8,16, echo number NECH:3500, receiver bandwidth SW:100,200,300KHz, the control parameters R FD:0.002-0.05ms in beginning sampling time, time delay D L1:0.1-0.5ms carries out NMR signal collection.
As described in method, wherein the described chemometrics method of step (4) adopts principal component analysis (PCA) and partial least-square regression method.
More specifically, technical scheme operation steps of the present invention is as follows:
1) make miscella sample: pure Oleum Sesami and pure soy bean are pressed to different proportion mixing, make multiple miscella samples, the volume percent content by soybean oil in Oleum Sesami is uniformly distributed from 0-100%, to ensure the representativeness of sample.
2) make and detect sample: draw oil sample respectively 3ml in 5ml centrifuge tube with liquid-transfering gun.
3) adopt low-field nuclear magnetic resonance technology to measure the CPMG spectrogram of pure Oleum Sesami, pure soy bean and miscella; The parameter of relaxation spectrum: 90 degree pulsewidth P
1: 4 μ s, 180 degree pulsewidth P
2: 8 μ s, repeated sampling stand-by period Tw:3500ms, analog gain RG1:[-3.0 to 40, is integer], digital gain DRG1:[0 to 7, be integer], pre-amp gain PRG:[0 to 3], repeated sampling times N S:4,8,16, echo number NECH:3500, receiver bandwidth SW:100,200,300KHz, the control parameters R FD:0.002-0.05ms in beginning sampling time, time delay D L1:0.1-0.5ms carries out NMR signal collection.
4) data analysis and processing.Adopt Chemical Measurement as principal component analysis (PCA) and partial least-square regression method treatment step 3) the middle CPMG data that obtain, set up based on low-field nuclear magnetic resonance data, and for predicting the regression equation of adulterated ratio of sesame-soybean miscella, realize the fast detecting of Oleum Sesami.
Compared with prior art, excellent benefit of the present invention is: method of the present invention does not have complicated sample pretreatment process, can within a few minutes, realize fast detecting and the analysis of the content of Oleum Sesami in sesame-soybean miscella, thereby the quality to Oleum Sesami is identified fast, for consumer provides quality assurance.Compared with traditional method, the inventive method has not only improved detection speed, and the accuracy detecting also improves greatly.
Brief description of the drawings
Fig. 1 is the CPMG die-away curve spectrogram of oil sample;
Fig. 2 is the T that LF-NMR detects oil samples
2data spectrogram;
Fig. 3 is T
2with the variation broken line graph of blending ratio;
Fig. 4 is the major component scatter diagram of all oil samples;
Fig. 5 is the histogram of the remaining deviation of the calibrating patterns of all oil samples;
Fig. 6 is that practical measurement value and predicted value must return spectrogram;
Fig. 7 is the standard deviation spectrogram of the offset minimum binary of calibration sample.
Embodiment
Below in conjunction with accompanying drawing, further illustrate essence of the present invention with embodiments of the invention, but be not limitation of the present invention.
Embodiment 1:
1) make miscella sample: the pure Oleum Sesami that supermarket is bought and pure soy bean are pressed different proportion and mixed, and make 7 miscella samples, and the volume percent content of its soybean oil in Oleum Sesami is respectively 0,10,20,40,60,80,100%.
2) make and detect sample: adopt liquid-transfering gun to get respectively and mix oil sample 3ml in 5ml centrifuge tube separately.
3) adopt low-field nuclear magnetic resonance technology to measure the relaxation spectrogram of pure Oleum Sesami, pure soy bean and miscella; The parameter of relaxation spectrum: 90 degree pulsewidth P
1: 4 μ s, 180 degree pulsewidth P
2: 8 μ s, repeated sampling stand-by period Tw:3500ms, analog gain RG1:[-3.0 to 40, is integer], digital gain DRG1:[0 to 7, be integer], pre-amp gain PRG:[0 to 3], repeated sampling times N S:4,8,16, echo number NECH:3500, receiver bandwidth SW:100,200,300KHz, the control parameters R FD:0.002-0.05ms in beginning sampling time, time delay D L1:0.1-0.5ms.
4) relaxation spectrum data analysis and process.Adopt principal component analysis (PCA) and partial least-square regression method treatment step 3 in Chemical Measurement) the middle relaxation spectrum data that obtain, set up the data based on low-field nuclear magnetic resonance, and for predicting the regression equation of adulterated ratio of sesame-soybean miscella, realize the fast detecting of Oleum Sesami.
Below for adopting said method to carry out the concrete test example of Oleum Sesami Quality Detection:
One, the object of this test
1. detect the relaxation signals of the nuclear magnetic resonance of certified products Oleum Sesami and adulterated Oleum Sesami;
2. detect the parameter of certified products Oleum Sesami and adulterated Oleum Sesami;
3. set up the detection model of relaxation signals and the Oleum Sesami quality of nuclear magnetic resonance.
Two, test material
Oleum Sesami, soybean oil.
Three, test apparatus
NM12 magnetic nuclear resonance analyzer (Shanghai knob steps electronics technology).
Four, process of the test
Adopt NM12 magnetic nuclear resonance analyzer to carry out test analysis to sample, specifically first adopt cpmg sequence row to measure after the T2 of certified products Oleum Sesami and adulterated Oleum Sesami and soybean oil, adopt again the anti-Laplce's algorithm of one dimension as T2 inversion algorithm, draw the relaxation time collection of illustrative plates of each sample, the relaxation data of certified products Oleum Sesami and adulterated Oleum Sesami and soybean oil is analyzed in conjunction with principal component analysis (PCA), obtain major component scatter diagram, then, carry out data processing by partial least-squares regressive analysis, and then set up regretional analysis curve, thereby set up Oleum Sesami attribute test database.Finally utilize the database of setting up to carry out Quality Detection to unknown Oleum Sesami sample, from test data and test result, the method that low-field nuclear magnetic resonance detects Oleum Sesami quality is one simple method of testing very fast, for Oleum Sesami attributional analysis provides a kind of detection method of quick nondestructive.
The relaxation time T of table 1 oil sample signal single component inverting
2relaxation time T with polycomponent inverting
21, T
22
A, b, c, d, e, f, g: different letter representation significant differences (p<0.01) in table
The data of the partial least squares regression that table 2 is analyzed based on raw data
Claims (3)
1. a method for the discriminating of the Oleum Sesami true and false and assay, is characterized in that the method comprises the steps:
1) make miscella sample: pure Oleum Sesami and pure soy bean are pressed to different proportion mixing, make multiple miscella samples, the volume percent content by soybean oil in Oleum Sesami is uniformly distributed from 0-100%, to ensure the representativeness of sample;
2) make and detect sample: draw oil sample respectively 3ml in 5ml centrifuge tube;
3) adopt low-field nuclear magnetic resonance technology to measure the CPMG spectrogram of pure Oleum Sesami, pure soy bean and miscella;
4) adopt chemometrics method treatment step 3) in the CPMG data that obtain, set up based on low-field nuclear magnetic resonance data, and for predicting the regression equation of adulterated ratio of sesame-soybean miscella, realize the fast detecting of Oleum Sesami.
2. the method for claim 1, is characterized in that the CPMG spectrogram parameter of the described working sample of step (3): 90 degree pulsewidth P
1: 4 μ s, 180 degree pulsewidth P
2: 8 μ s, repeated sampling stand-by period Tw:3500ms, analog gain RG1:[-3.0 to 40, is integer], digital gain DRG1:[0 to 7, be integer], pre-amp gain PRG:[0 to 3], repeated sampling times N S:4,8,16, echo number NECH:3500, receiver bandwidth SW:100,200,300KHz, the control parameters R FD:0.002-0.05ms in beginning sampling time, time delay D L1:0.1-0.5ms carries out NMR signal collection.
3. the method for claim 1, is characterized in that the described chemometrics method of step (4) adopts principal component analysis (PCA) and partial least-square regression method.
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Cited By (13)
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| CN104502389A (en) * | 2015-01-27 | 2015-04-08 | 西南民族大学 | Detection method for coconut milk |
| CN104713895A (en) * | 2015-03-13 | 2015-06-17 | 中国科学院武汉物理与数学研究所 | Method for distinguishing between pure and syrup-adulterated honey based on combination of hydrogen nuclear magnetic resonance and partial least square method |
| CN105372276A (en) * | 2015-11-24 | 2016-03-02 | 大连工业大学 | Texture quality non-destructive testing method in sea cucumber heating process |
| CN105748073A (en) * | 2014-12-15 | 2016-07-13 | 中国科学院大连化学物理研究所 | Cage for mouse in waking state and application of cage |
| CN106018451A (en) * | 2016-04-29 | 2016-10-12 | 大连工业大学 | Method for determination of oil content and water content of soybeans by using low field nuclear magnetic resonance technology |
| CN106018452A (en) * | 2016-04-29 | 2016-10-12 | 大连工业大学 | Peanut variety nondestructive testing method based on nuclear magnetic resonance technology |
| CN106896177A (en) * | 2017-04-21 | 2017-06-27 | 山东省分析测试中心 | Pseudo- vegetable oil kind is mixed in a kind of sesame oil and pseudo- amount discrimination method is mixed |
| CN106950241A (en) * | 2017-02-27 | 2017-07-14 | 南昌大学 | A kind of method of other adulterated oil species and content in prediction tea oil |
| CN107505350A (en) * | 2017-10-20 | 2017-12-22 | 河南工业大学 | A kind of grape-kernel oil based on low field nuclear-magnetism mixes pseudo- method for quick identification |
| CN109902638A (en) * | 2019-03-05 | 2019-06-18 | 上海理工大学 | Edible oil transverse-relaxation signals feature extracting method based on 2D-CNN |
| CN111189868A (en) * | 2020-02-18 | 2020-05-22 | 南京农业大学 | Method for rapidly screening adulterated illegal cooking oil in edible oil by using low-field nuclear magnetic resonance |
| CN112285144A (en) * | 2020-10-15 | 2021-01-29 | 青岛农业大学 | Method for detecting breast myopathy of white feather broiler chicken by using low-field nuclear magnetic resonance |
| WO2021218798A1 (en) * | 2020-04-27 | 2021-11-04 | 华东师范大学 | Fluid type identification and quality inspection method based on nuclear magnetic resonance technology |
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| CN104502389A (en) * | 2015-01-27 | 2015-04-08 | 西南民族大学 | Detection method for coconut milk |
| CN104713895A (en) * | 2015-03-13 | 2015-06-17 | 中国科学院武汉物理与数学研究所 | Method for distinguishing between pure and syrup-adulterated honey based on combination of hydrogen nuclear magnetic resonance and partial least square method |
| CN104713895B (en) * | 2015-03-13 | 2017-01-18 | 中国科学院武汉物理与数学研究所 | Method for distinguishing between pure and syrup-adulterated honey based on combination of hydrogen nuclear magnetic resonance and partial least square method |
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| CN106018451A (en) * | 2016-04-29 | 2016-10-12 | 大连工业大学 | Method for determination of oil content and water content of soybeans by using low field nuclear magnetic resonance technology |
| CN106018452A (en) * | 2016-04-29 | 2016-10-12 | 大连工业大学 | Peanut variety nondestructive testing method based on nuclear magnetic resonance technology |
| CN106950241A (en) * | 2017-02-27 | 2017-07-14 | 南昌大学 | A kind of method of other adulterated oil species and content in prediction tea oil |
| CN106896177A (en) * | 2017-04-21 | 2017-06-27 | 山东省分析测试中心 | Pseudo- vegetable oil kind is mixed in a kind of sesame oil and pseudo- amount discrimination method is mixed |
| CN107505350A (en) * | 2017-10-20 | 2017-12-22 | 河南工业大学 | A kind of grape-kernel oil based on low field nuclear-magnetism mixes pseudo- method for quick identification |
| CN109902638A (en) * | 2019-03-05 | 2019-06-18 | 上海理工大学 | Edible oil transverse-relaxation signals feature extracting method based on 2D-CNN |
| CN109902638B (en) * | 2019-03-05 | 2021-02-23 | 上海理工大学 | Edible oil transverse relaxation signal feature extraction method based on 2D-CNN |
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