CN102759515A - Method for rapidly determining oil contents of agricultural products by using mid-infrared spectrometer based on horizontal attenuated total reflection (ATR) - Google Patents
Method for rapidly determining oil contents of agricultural products by using mid-infrared spectrometer based on horizontal attenuated total reflection (ATR) Download PDFInfo
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Abstract
The invention discloses a method for rapidly determining oil contents of agricultural products by using a mid-infrared spectrometer based on horizontal attenuated total reflection (ATR), and relates to the field of rapid detection of the oil contents of the agricultural (food) products. A dry agricultural (food) product is ground, dissolved by using a certain amount of Alpha-bromonaphthalene and filtered; a filtrate is placed on a horizontal ATR crystal; an ATR infrared spectrum of the filtrate is collected; and the oil content of the filtrate is pre-determined by using a well-established model. The method disclosed by the invention has the advantages that the oil contents of the agricultural (food) products can be analyzed rapidly, simply, conveniently and quantitatively only by simply preprocessing samples, the detection linear range is wide and an accurate and reliable result is obtained.
Description
Technical field
The present invention relates to agricultural production (food) article oil content fast detecting field; Refer in particular to a kind of method based on infrared fast measuring agricultural production (food) article oil content in horizontal ATR (Attenuated Total Reflection is abbreviated as ATR, the means attenuated total reflection) annex.
Background technology
The height of oil content can have influence on the height of this product hierarchy in the agricultural product, and especially grease processing enterprise hopes can measure fast the oil content of these agricultural product, thereby provides reasonable prices.Food enterprise such as instant noodles, French fries needs in time to understand the variation of product oil content, so that feed back to the adjusting that production division instructs production technology early.
The soybean of the especially high fat content of present popular agricultural product, sesame, vegetable seed etc., and the oil content of fried food such as food such as instant noodles, French fries normally adopts ether as solvent, measures through Suo Shi grease extractor.Traditional Suo Shi extraction process (GB/ T14488. 1) has very high requirement to personnel's technical merit, at same sample, when different personnel operate, can produce certain personal error; Carry out oleaginousness by the Suo Shi extraction process simultaneously and measure, two tests do not allow to exceed certain error, will take a sample again and reform if exceed error; Suo Shi extraction process time that need reach more than 8 hours that makes an experiment just can obtain the result; Sometimes a collection of raw material machines the back test findings and just comes out; Minute is oversize, can increase the cost of purchase enterprise, feeds back too late; Can not satisfy and not have the effect of instructing and regulating and control to produce in the needs of modern enterprise, particularly modern food and the grease processing enterprise; The ether that use in the laboratory is volatile as solvent, and long-term suction meeting works the mischief to human body; And ether belongs to inflammable and explosive chemicals, has potential safety hazard.Therefore these departments and need the Fast Detection Technique of grease.
Various spectrum detection techniques have been widely used in the fast detecting research of agricultural production (food) article, but mostly are used for the harmless fast detecting of agricultural production (food) article.Like near-infrared spectrum analysis (NIR) is one of high-new analytical technology with the fastest developing speed over past ten years; Its amount of samples is few and do not destroy sample, need not sample is carried out chemical treatment, and can carry out quantitative test simultaneously to the multiple composition in the sample in the short time at 1-2 minute the utmost point; It is low to have cost; Speed is fast, and is pollution-free, is convenient in real time, advantages such as on-line analysis and control.Nuclear magnetic resonance method only needs 30 seconds to sample measurement at every turn, meets the standard of modern food and oils industry fully, and grease enterprise each link from purchase the former Residual oil of expecting grouts is carried out fast detecting, obtains test result fast.The effect that this can play timely guidance production and reduce cost modern food manufacturing enterprise.But Non-Destructive Testing also has certain limitation, because the constituent at each position of agricultural production (food) article is different, it gathers different at different position and different often, averages through statistical principle, so certain defective is arranged on the precision.
Some scholars were applied to spectrum detection technique in the detection of agricultural production (food) quality both at home and abroad in recent years.But do not see the method for utilization based on infrared fast measuring agricultural production (food) article oil content among the horizontal ATR.
Summary of the invention
The present invention utilizes the oil content of mid-infrared light spectrometer fast measuring agricultural production (food) article that have horizontal ATR annex in order to overcome above-mentioned deficiency of the prior art.
The present invention is based on the method for mid-infrared light spectrum quick test agricultural production (food) the article oil content of horizontal ATR, carry out according to following step:
(1) gets a certain amount of dry sample of need measuring, pulverize and mix, adopt the extracting of Suo Shi extraction process to go out crude fat and be used for the standard specimen preparation;
(2) carry out the standard specimen preparation by certain gradient;
(3) middle infrared spectrum collection;
(4) spectrum pre-service;
(5) modelling;
(6) sample prediction;
(7) model tuning;
(8) utilize above-mentioned model to detect the oil content of agricultural product or food.
Wherein the described dry sample of step (1) is meant the sample that is lower than equilibrium moisture content under the normal temperature.
Wherein the described standard specimen of step (2) is meant the configuration sample of concentration range when content range is wanted to cover sample detection.
Wherein the described middle infrared spectrum collection of step (3) is meant the middle infrared spectrum collection of utilization based on horizontal ATR.
The wherein described spectrum pre-service of step (4); Be meant according to the spectrum needs of gathering; Can adopt various preprocessing procedures such as spectrum is level and smooth, first order derivative, second derivative, normalization to carry out pre-service,, also can directly adopt original spectrum if the spectrum of gathering is more stable.
Wherein the described modelling of step (5) is meant that employing progressively returns, PLS various chemometrics methods such as (PLS) are set up the oil content forecast model.
The wherein described sample prediction of step (6) is meant accurately to take by weighing a certain amount of sample, is dissolved in the not volatile organic solvent of a certain amount of easy dissolved fat; Concussion shakes up; Left standstill and filtered clear liquid, carried out spectra collection, and utilized above-mentioned model to detect agricultural production (food) article oil content.
The wherein described model tuning of step (7) is meant and gets the somewhat sample of above-mentioned different oil contents, adopts Suo Shi extraction process (GB/ T14488. 1) to measure, and predicting the outcome according to testing result and spectrometer compares analysis, then model is proofreaied and correct.
Wherein step (8) utilizes above-mentioned model to detect the oil content of agricultural product or food; Be meant and accurately take by weighing a certain amount of sample; Be dissolved in the not volatile organic solvent of a certain amount of easy dissolved fat, concussion shakes up, and leaves standstill to filter clear liquid; Carry out spectra collection, utilize and proofread and correct the oil content that the back model detects agricultural product or food.
Beneficial effect of the present invention:Utilization can be taken into account the inside and outside overall permanence of sample based on the method for infrared fast measuring agricultural production (food) article oil content among the horizontal ATR, to improve rapidity, security and the reliability that detects.With instant noodles is sample; Adopt middle infrared spectrum acquisition system image data; Utilize the Chemical Measurement software of establishment voluntarily to set up model through stepwise regression method; As measurement index, set up progressively regression model, the predicted value of model and the related coefficient of measured value with related coefficient and relative error based on optimal characteristics
RBe 0.998, average relative error is 2.43%, and precision is higher, can satisfy production run control average relative error and be not more than the requirement in 5%.
The present invention compares with the conventional sense method, fast, the easy and simple to handle convenience of detection speed; Compare with near-infrared spectrum technique, nuclear magnetic resonance technique, the information that obtains is more comprehensive, and the accuracy and the stability of testing result all increase.
In food and grease processing enterprise now, production scale is increasing, if also carrying out with traditional detection method, the manpower of consumption, charges for water and electricity and chemical reagent take just bigger.Method based on infrared fast measuring agricultural production (food) article oil content among the horizontal ATR provided by the invention can realize the fast detecting of agricultural production (food) article oil content, well solves the consumption manpower, charges for water and electricity and the chemical reagent that exist aborning and takes problem.This invention provides reference for science detects agricultural production (food) article oil content, to improving enterprise intelligent management level and product quality direct meaning is arranged all.Simultaneously, its characteristics of fast, accurately measuring oleaginousness also are well suited for departments' uses such as commodity inspection department, grain and oil purchase and processing and foreign trade.
Embodiment
Be example with instant noodles below, the present invention is explained in further detail.
The mid-infrared light spectrometer that the middle infrared spectrum acquisition system based on horizontal ATR that is adopted in the specific embodiment of the invention is adopted is the WQF-510A Fourier transformation infrared spectrometer that north, Beijing divides Rayleigh analytical instrument (group) company to produce; The NIRSA data handling system that adopts the near infrared work group of Jiangsu University to work out is voluntarily carried out modelling; Buy Zhenjiang and distinguish the flavor of spareribs with brown sauce face that good garden Food Co., Ltd produces as test sample.Oil content according to (GB/ T14488. 1) employing Suo Shi extraction process working sample is used for following modelling and correction.Concrete mensuration process is following:
(1) takes by weighing the 100g instant noodles and adopt Suo Shi extraction process (GB/ T14488. 1) extracting to go out the about 20g of grease, carry out modeling with this grease and use;
(2) selection is prone to the not volatile organic solvent of dissolved fat, and the present invention selects alpha-bromonaphthalene (281 ℃ of boiling points) as solvent;
(3) standard specimen preparation: oil content is one of quality index of fried instant noodle major control, and oil content is generally in 18%～28% scope, and national standard generally requires below 24%.So the standard specimen of preparation is wanted to cover this scope; Require sampling 1.000g to be dissolved in the 5ml alpha-bromonaphthalene during detection; Suppose that this instant oil rate is 30%; The then oil content of alpha-bromonaphthalene (relative density 1.489g/ml)=
, so the oil content of the standard specimen alpha-bromonaphthalene of preparation can be controlled at below 4% and get final product.By the preparation of certain gradient, the result sees table 1: modeling standard specimen allocation list (because the rifle head has the liquid residue when moving liquid, so it is inaccurate to move liquid, must weigh);
Table 1 modeling standard specimen preparation table
| Numbering | Alpha-bromonaphthalene volume (ml) | Alpha-bromonaphthalene quality (g) | Grease volume (ml) | Oil quality (g) | Oil content (%) |
| 0 | 5 | 7.0135 | 0 | 0 | 0 |
| 1 | 5 | 7.194 | 0.04 | 0.0325 | 0.450 |
| 2 | 5 | 7.3476 | 0.08 | 0.0641 | 0.865 |
| 3 | 5 | 7.6008 | 0.12 | 0.0982 | 1.275 |
| 4 | 5 | 7.0025 | 0.16 | 0.1298 | 2.643 |
| 5 | 5 | 7.1915 | 0.2 | 0.1651 | 2.575 |
| 6 | 5 | 6.9733 | 0.24 | 0.2015 | 2.808 |
| 7 | 5 | 6.8644 | 0.28 | 0.2346 | 3.305 |
| 8 | 5 | 6.6166 | 0.32 | 0.2652 | 3.854 |
| 9 | 5 | 7.3732 | 0.36 | 0.3012 | 2.513 |
| 10 | 5 | 7.2208 | 0.4 | 0.3125 | 4.148 |
(4) middle infrared spectrum collection: (sampling, display resolution all are 4WN to instrument condition; Signal gain 4; Sweep velocity 20ms; Scanning times 32 times; Spectral range 800-2000 wave number) the start preheating is 30 minutes; Carry out spectra collection to being used for the standard specimen of modeling then; Scan with No. 0 standard specimen is background at every turn, and the absorbance spectrum of gathering each sample is then gathered three times for every kind; The absorbance of per twice spectrum about 1740 wave numbers is not more than 0.002, otherwise sample spectra will be gathered again.
(5) spectrum pre-service: because the spectrum of gathering is more stable, so directly adopt original spectrum.
(6) modelling: adopt progressively to return (SWF) forward, introducing variable number is 2, returns and sets up calibration model.
Equation returns declares statistical study as a result:
Related coefficient: 0.9980
Return and declare straight-line equation: Y=0.9980X+0.0036
Return and declare root-mean-square error: 0.0450
(7) sample prediction: accurately take by weighing the 1.0000g instant noodles; Adopt the sample after family-use grinder is pulverized 10s; Be dissolved in the not volatile organic solvent (alpha-bromonaphthalene) of easy dissolved fat of a certain amount of (5ml and weigh with analytical balance), vibrate shook up in 2 minutes, left standstill 15 minutes; It is subsequent use that filter paper filtering gets clear liquid, utilizes easy to detect oil content of above-mentioned model.
(8) model tuning: get the sample of 10 parts of above-mentioned different oil contents, adopt Suo Shi extraction process (GB/ T14488. 1) to measure, predicting the outcome according to testing result and spectrometer compares analysis, then model is proofreaied and correct.
(9) interpretation of result: utilize model after the above-mentioned correction to detect the oil content of this 10 duplicate samples, and No. 5 samples are wherein carried out 6 parallel detections, table 2, table 3 are seen in interpretation of result.
The oil content testing result comparative analysis of 10 portions of instant noodles of table 2
| Sample number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Chemical detection value % | 18.41 | 22.83 | 20.24 | 20.18 | 22.47 | 20.52 | 20.16 | 19.68 | 21.92 | 20 |
| Spectral detection value % | 17.57 | 22.51 | 21.11 | 21.05 | 22.44 | 20.31 | 21.01 | 20.09 | 22.38 | 20.05 |
| Absolute error % | 0.84 | 0.32 | -0.87 | -0.87 | 0.03 | 0.21 | -0.85 | -0.41 | -0.46 | -0.05 |
| Relative error % | 4.56 | 1.41 | -4.27 | -4.33 | 0.14 | 1.01 | -4.21 | -2.09 | -2.08 | -0.24 |
6 oil content testing results comparative analysis of the same instant noodles of table 3
The mid-infrared light spectrometry, less demanding to personnel's technical merit, as long as can just can make an experiment by the basic operation computer; Relative error can be controlled at ± 5% in; The factor that does not have the man's activity accuracy fully, can measure degree of stability (referring to absolute error here) repeatedly to same sample can reach ± 0.25% in, facts have proved that the accuracy of mid-infrared light spectrometry is high; Precision and favorable reproducibility can be used for the process control of enterprise production fully.
Below just combine a specific embodiment (is example with the instant oil rate); The present invention is further understood in exemplary illustration and help, but the embodiment detail only is in order the present invention to be described, not to represent the present invention to conceive down whole technology implementations examples; Therefore should not be construed as the total technology implementation example of the present invention is limited; Some do not depart from the unsubstantiality of inventive concept and change In the view of the technician, for example simple the change or replacement of technical characterictic to have same or similar technique effect; As change organic solvent, change dissolution equilibrium time, infrared other annex of employing, change modeling method etc., all belong to protection domain of the present invention.
Claims (9)
1. based on the method for the mid-infrared light spectrum quick test agricultural product oil content of horizontal ATR, it is characterized in that carrying out according to following step:
(1) gets a certain amount of dry sample of need measuring, pulverize and mix, adopt the extracting of Suo Shi extraction process to go out crude fat and be used for the standard specimen preparation;
(2) carry out the standard specimen preparation by certain gradient;
(3) middle infrared spectrum collection;
(4) spectrum pre-service;
(5) modelling;
(6) sample prediction;
(7) model tuning;
(8) utilize above-mentioned model to detect the oil content of agricultural product or food.
2. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1 is characterized in that wherein the described dry sample of step (1) is meant the sample that is lower than equilibrium moisture content under the normal temperature.
3. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1 is characterized in that the described standard specimen of step (2) wherein is meant the configuration sample of concentration range when content range is wanted to cover sample detection.
4. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1 is characterized in that wherein the described middle infrared spectrum collection of step (3) is meant the middle infrared spectrum collection of utilization based on horizontal ATR.
5. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1; It is characterized in that the wherein described spectrum pre-service of step (4); Be meant according to the spectrum needs of gathering; Adopt that spectrum is level and smooth, first order derivative, second derivative, the various preprocessing procedures of normalization carry out pre-service, if the spectrum of gathering is more stable, also can directly adopt original spectrum.
6. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1 is characterized in that the wherein described modelling of step (5) is meant that employing progressively returns, the various chemometrics methods of PLS are set up the oil content forecast model.
7. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1; It is characterized in that the wherein described sample prediction of step (6), be meant accurately to take by weighing a certain amount of sample, be dissolved in the not volatile organic solvent of a certain amount of easy dissolved fat; Concussion shakes up; Left standstill and filtered clear liquid, carried out spectra collection, and utilized above-mentioned model to detect the agricultural product oil content.
8. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1; It is characterized in that the wherein described model tuning of step (7); Be meant the sample of getting several parts of above-mentioned different oil contents; Adopt the Suo Shi extraction process to measure, predicting the outcome according to testing result and spectrometer compares analysis, then model is proofreaied and correct.
9. the method for the mid-infrared light spectrum quick test agricultural product oil content based on horizontal ATR according to claim 1; It is characterized in that wherein step (8) utilizes above-mentioned model to detect the oil content of agricultural product or food, be meant accurately to take by weighing a certain amount of sample, be dissolved in the not volatile organic solvent of a certain amount of easy dissolved fat; Concussion shakes up; Left standstill and filtered clear liquid, carried out spectra collection, and utilized and proofread and correct the oil content that the back model detects agricultural product or food.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104406916A (en) * | 2014-11-04 | 2015-03-11 | 百度在线网络技术（北京）有限公司 | Method and apparatus for detecting food |
| WO2017107278A1 (en) * | 2015-12-21 | 2017-06-29 | 江苏大学 | In-situ real-time spectrum based on-line protein enzymatic hydrolysis monitoring method and device |
| CN107255626A (en) * | 2017-07-04 | 2017-10-17 | 江南大学 | The rapid assay methods of fat content in a kind of starch base fried food |
| CN110231302A (en) * | 2019-06-10 | 2019-09-13 | 江南大学 | A kind of method of the odd sub- seed crude fat content of quick measurement |
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| SU420914A1 (en) * | 1972-06-16 | 1974-03-25 | В. Г. Гизатулин, В. П. Муругов И. И. Свентицкий | |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104406916A (en) * | 2014-11-04 | 2015-03-11 | 百度在线网络技术（北京）有限公司 | Method and apparatus for detecting food |
| WO2017107278A1 (en) * | 2015-12-21 | 2017-06-29 | 江苏大学 | In-situ real-time spectrum based on-line protein enzymatic hydrolysis monitoring method and device |
| CN107255626A (en) * | 2017-07-04 | 2017-10-17 | 江南大学 | The rapid assay methods of fat content in a kind of starch base fried food |
| CN110231302A (en) * | 2019-06-10 | 2019-09-13 | 江南大学 | A kind of method of the odd sub- seed crude fat content of quick measurement |
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