CN106370619A - Comprehensive determination method for gross cottonseed quality indexes - Google Patents
Comprehensive determination method for gross cottonseed quality indexes Download PDFInfo
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- CN106370619A CN106370619A CN201610772617.4A CN201610772617A CN106370619A CN 106370619 A CN106370619 A CN 106370619A CN 201610772617 A CN201610772617 A CN 201610772617A CN 106370619 A CN106370619 A CN 106370619A
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- 235000012343 cottonseed oil Nutrition 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000001228 spectrum Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 11
- 235000019198 oils Nutrition 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000002329 infrared spectrum Methods 0.000 claims description 17
- 210000000582 semen Anatomy 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 238000003786 synthesis reaction Methods 0.000 claims description 12
- 241000628997 Flos Species 0.000 claims description 6
- 238000012937 correction Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 4
- 238000009499 grossing Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000007781 pre-processing Methods 0.000 abstract description 3
- 238000012216 screening Methods 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 45
- 240000000902 Diospyros discolor Species 0.000 description 3
- 235000003115 Diospyros discolor Nutrition 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 235000007474 pcego de ndia Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003041 laboratory chemical Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a comprehensive determination method for gross cottonseed quality indexes. The method comprises the steps that screening and tabletting pretreating are conducted on gross cottonseeds, near-infrared spectrogram is scanned, spectral information is processed according to an optimal preprocessing method, and then the water content, the protein content, the oil content, the acid value, the kernel yield and the lint containing rate of the gross cottonseeds are quickly determined. According to the method, by conducting screening and extrusion pretreating on the gross cottonseeds, influences of impurities on the spectrum stability are reduced, obstruction of gross cottonseed lint on application of a near-infrared technology is overcome, therefore, modeling can be conducted on the gross cottonseeds by combining near-infrared scanning with a chemometrics multi-variate calibration method, and then the method through which various quality indexes of the gross cottonseeds can be determined is built. The method has the advantages of being high in speed, low in cost and free of chemical harm; meanwhile, multiple indexes can be detected, the defect problems of conventional chemical detection can be effectively solved, and compared with manual value detection in a laboratory, the outstanding advantages of being quick, accurate, green and environmentally friendly are achieved.
Description
Technical field
The present invention relates to a kind of detection method, especially a kind of gross cottonseed quality index synthesis measuring method.
Background technology
Gross cottonseed is of paramount importance side-product in cotton processing, moisture in Semen Gossypii, protein content, contains
Oil mass, acid number, kernel percent and rate containing floss are to pass judgment on the important indicator of Semen Gossypii quality and economic benefit.The mensure of gross cottonseed index is led to
Often based on conventional chemical method, the such as soxhlet extraction of oil content detection, the Oven Method of water content detection, protein content inspection
The Kjeldahl's method of survey, pure manual inspection of kernel percent etc..These traditional analysis methods are homogeneous in sensitivity and degree of accuracy
To higher, but all exist that sample treatment is loaded down with trivial details, the problems such as length analysis time, high cost and reagent consume big.
At present the research of Semen Gossypii quality determination aspect is concentrated mainly on and gross cottonseed is carried out with light cotton after lint pretreatment
The mensure of seed, and often can only measure one or two index it is impossible to Quality evaluation is carried out to gross cottonseed.Actually in Semen Gossypii
In intensive processing enterprise, due to shelling floss complex operation, time-consuming and there is the non-repeated of subjective judgment, leads to detection error
Very greatly it would be desirable to be able to carry out quick, accurate detection for gross cottonseed.How to provide one kind can detect velvet apple by quick, accurate, full item
The method of seed aggregative indicator, is rarely reported both at home and abroad, and the method is real, important for instructing buying, producing and selling all to have
Meaning.
Content of the invention
The technical problem to be solved in the present invention is to provide one kind fast and accurately gross cottonseed quality index synthesis measuring side
Method.
For solving above-mentioned technical problem, the method and step that the present invention is taken is: (1) chooses representative gross cottonseed
Sample is as gross cottonseed sample；
(2) chemical method is adopted to the moisture in gross cottonseed sample, protein content, oil content, acid number, kernel percent and to contain floss
Rate is measured；
(3) gross cottonseed sample is sieved to go the removal of impurity, then the gross cottonseed sample cake of pie will be squeezed into, using near-infrared
Spectrogrph is scanned to gross cottonseed sample cake gathering, and obtains the near infrared spectrum data of gross cottonseed sample；
(4) near infrared spectrum data is carried out with Pretreated spectra, recycles variable analyses method to carry out variable selection；Then use many
First scatter correction method sets up the near infrared spectrum data of gross cottonseed and step (2) is measured the near infrared spectrum of each constituent content
Calibration model；
(5) Semen Gossypii sample to be measured is processed using step (3) methods described and gathered near infrared spectrum data, according to step
(4) the near infrared spectrum calibration model constructed by, you can obtain each component content results of Semen Gossypii sample to be measured.
In step (2) of the present invention, sieved using 30 eye mesh screens.
It is used diameter cylinder corresponding near infrared spectrometer sweep limitss to hold as extruding in step (3) of the present invention
Device, squeeze pressure is 0.8 ± 0.02mpa, and extrusion time is 5～10min.Each applied sample amount of described extruding is 13～16g, directly
Thickness 1.5～2.5cm to gross cottonseed sample cake.
In step (3) of the present invention, the ambient temperature of scanning is 25 ± 0.5 DEG C, and wavelength is 950～1650nm.Described
Scan mode is continuous wavelength infrared diaphanoscopy.
In step (4) of the present invention, the method for Pretreated spectra is that Method of Seeking Derivative, smoothing method and/or multiplication scatter
Bearing calibration.
Have the beneficial effects that using produced by technique scheme: the present invention is by being sieved to gross cottonseed and extruding
Pretreatment, solves the impact to spectrum stability for the impurity, the obstacle overcoming gross cottonseed short flannel that near infrared technology is applied, makes velvet apple
Seed can combine Chemical Measurement multivariate calibration methodses with infrared diaphanoscopy and model, and set up all kinds of quality that can measure gross cottonseed
Refer to calibration method.The present invention has that speed is fast, the advantage of low cost and no chemical hazard, can detect moisture, albumen simultaneously
The full item index such as matter content, oil content, acid number and kernel percent, can efficiently solve conventional chemical detection drawback problem, compare
Laboratory value detection by hand, has quick, accurate, environmental protection prominent effect, realizes the quick, just of gross cottonseed indices
Prompt and efficient nondestructive analysis, provides reliable data and supports to Semen Gossypii quality index synthesis measuring.
Specific embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
Embodiment: the concrete technology step of this gross cottonseed quality index synthesis measuring method is as described below.
(1) choose the representative gross cottonseed sample of different sources, different times and different cultivars as gross cottonseed
Sample；The present embodiment chooses representative Xinjiang gross cottonseeds in 2014 and 2015, Hebei gross cottonseed, Gansu gross cottonseed and lake
Northern gross cottonseed sample is as experiment sample.
(2) using gb/t 14488.1-2008 national standard method, Semen Gossypii is measured to the detection of gross cottonseed sample each index chemical score
Middle oil content, gb/t 14489.1-2008 national standard method measures moisture in Semen Gossypii, gb/t 14489.2-2008 GB side
Method measures protein content and gb/t 5009.37-2003 method in Semen Gossypii and measures acid number in Semen Gossypii.
(3) in gross cottonseed, the chemical determination of rate containing floss method is: weighs representational sample 10 ± 0.5g gross cottonseed and puts
Enter in surface plate, weigh m0, dry 2h in 130 DEG C of constant temperature ovens, weigh m immediately1.Draw 4ml distilled water in 100ml beaker,
Draw 6ml concentrated sulphuric acid again in beaker, stirred evenly with Glass rod；Then the gross cottonseed of drying is poured in beaker, stirred with Glass rod
Dynamic, till velveteen disappears on the gross cottonseed；Then pour them onto rapidly and be rinsed with water on screen cloth, until neutral；Then
Gross cottonseed after washing is poured in original surface plate, dries 1h in 130 DEG C of constant temperature ovens, weigh m2, obtain twice weight difference with
The ratio of gross cottonseed gross weight contains floss for gross cottonseed.
(4) in gross cottonseed, kernel percent chemical determination method is: weighs representational gross cottonseed sample 30g, uses shears
Cut off and peel off boll hull, boll hull, Cottonseed are distinguished, then weigh weight m of Cottonseed and boll hull respectively1、m2, obtain Cottonseed and velvet apple
The ratio of seed sample gross weight is gross cottonseed kernel percent.
(5) gross cottonseed sample preprocessing: gross cottonseed is sieved with 30 eye mesh screens, removes fine sand, soil etc. tiny miscellaneous
Matter；Use diameter rustless steel cylinder corresponding near infrared spectrometer sweep limitss again as extruding container, squeeze pressure for 0.8 ±
0.02mpa, extrusion time is 5～10min；By the way of the extruding of multiple loading, each applied sample amount is 13～16g, until hair
Thickness 1.5～the 2.5cm of Semen Gossypii sample cake；Infrared diaphanoscopy sample cell is disk, its a diameter of 15cm.
(6) gross cottonseed sample spectra acquisition: pretreated gross cottonseed sample cake is loaded in specimen disc, each sample
Scanning at least four times, takes spectrum mean value as sample original spectrum, and scanning circumstance temperature is 25 ± 0.5 DEG C, and wavelength is 950～
In the near infrared spectral range of 1650nm, scan mode is continuous wavelength infrared diaphanoscopy.
(7) Pretreated spectra is carried out to the gross cottonseed original spectrum of collection in step (6), using Method of Seeking Derivative, smooth side
At least one in method and multiplication scatter correction method；The present embodiment, using asking first derivative, second dervative and smoothing processing, obtains
Go out optimal pretreated spectrum.
(8) variable selection is carried out to the near infrared spectrum data of pretreated gross cottonseed in step (7), then dissipated with polynary
Penetrate bearing calibration (msc) set up each constituent content gross cottonseed near infrared spectrum data and step (2), (3), (4) being detected it
Between multiple near infrared spectrum calibration models.
(9) selection of calibration set and forecast set sample: for near-infrared modeling, calibration set and forecast set sample are necessary
The data distribution situation of original sample can be represented, and the sample content scope of calibration set will comprise forecast set sample content model
Enclose, gross cottonseed sample is divided into calibration set sample and forecast set sample according to the ratio of 3:1,624 parts of samples will be carried out point
Collection, obtains 468 parts of calibration set sample, 156 parts of forecast set sample, sets up described near-infrared model, calibration set and forecast set sample
Distribution is as shown in table 1.
Table 1: calibration set and forecast set sample distribution
As it can be seen from table 1 each component concentration ranges of calibration set sample are wide, comprise each component concentration ranges of forecast set sample, fit
Close the structure of near infrared correction.
(10) model is set up: application multiplicative scatter correction method (msc), sets up the near-infrared of the Calibration of gross cottonseed
Calibration model between spectrum and each constituent content of gross cottonseed.
(11) step (5) and the near infrared spectrum data of (6) methods described collection gross cottonseed sample to be measured are adopted, with above-mentioned
The near infrared spectrum calibration model detection gross cottonseed sample of the optimum constructed by step, obtains its each component content results.
(12) 82 batches of gross cottonseeds to be measured are respectively classified into 2 parts, portion is directly with sabot infrared diaphanoscopy, another basis
The preprocess method of step (5), screening carries out infrared diaphanoscopy after being squeezed into cake again, the results are shown in Table 2.
Table 2: gross cottonseed near-infrared result and laboratory chemical value deviation
As can be seen from Table 2, near-infrared can be scanned out number to six indexs simultaneously, compare manual inspection and substantially increase detection
Efficiency；After increasing preprocessing process, gross cottonseed indices deviation all has reduction, accurate for gross cottonseed near infrared detection simultaneously
Property is significantly improved.
Claims (7)
1. a kind of gross cottonseed quality index synthesis measuring method is it is characterised in that its method and step is:
(1) choose representative gross cottonseed sample as gross cottonseed sample；
(2) chemical method is adopted to the moisture in gross cottonseed sample, protein content, oil content, acid number, kernel percent and to contain floss
Rate is measured；
(3) gross cottonseed sample is sieved to go the removal of impurity, then the gross cottonseed sample cake of pie will be squeezed into, using near-infrared
Spectrogrph is scanned to gross cottonseed sample cake gathering, and obtains the near infrared spectrum data of gross cottonseed sample；
(4) near infrared spectrum data is carried out with Pretreated spectra, recycles variable analyses method to carry out variable selection；Then use many
First scatter correction method sets up the near infrared spectrum data of gross cottonseed and step (2) is measured the near infrared spectrum of each constituent content
Calibration model；
(5) Semen Gossypii sample to be measured is processed using step (3) methods described and gathered near infrared spectrum data, according to step
(4) the near infrared spectrum calibration model constructed by, you can obtain each component content results of Semen Gossypii sample to be measured.
2. a kind of gross cottonseed quality index synthesis measuring method according to claim 1 it is characterised in that: described step
(2), in, sieved using 30 eye mesh screens.
3. a kind of gross cottonseed quality index synthesis measuring method according to claim 1 it is characterised in that: described step
(3) be used in diameter cylinder corresponding near infrared spectrometer sweep limitss as extruding container, squeeze pressure be 0.8 ±
0.02mpa, extrusion time is 5～10min.
4. a kind of gross cottonseed quality index synthesis measuring method according to claim 3 it is characterised in that: described extruding
Applied sample amount is 13～16g every time, until the thickness 1.5～2.5cm of gross cottonseed sample cake.
5. a kind of gross cottonseed quality index synthesis measuring method according to claim 1 it is characterised in that: described step
(3) in, the ambient temperature of scanning is 25 ± 0.5 DEG C, and wavelength is 950～1650nm.
6. a kind of gross cottonseed quality index synthesis measuring method according to claim 5 it is characterised in that: described scanning side
Formula is continuous wavelength infrared diaphanoscopy.
7. a kind of gross cottonseed quality index synthesis measuring method according to claim 1-6 any one, its feature exists
In: in described step (4), the method for Pretreated spectra is Method of Seeking Derivative, smoothing method and/or multiplication scatter correction method.
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| CN201610772617.4A CN106370619A (en) | 2016-08-31 | 2016-08-31 | Comprehensive determination method for gross cottonseed quality indexes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118032677A (en) * | 2024-04-09 | 2024-05-14 | 甘肃农业大学 | Method and system for testing processing quality of angelica freeze-dried product |
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| CN102279168A (en) * | 2011-07-20 | 2011-12-14 | 浙江大学 | Near-infrared spectroscopic technology-based method for fast and undamaged analysis of nutritional quality of whole cottonseed |
| CN104132905A (en) * | 2014-05-05 | 2014-11-05 | 河南科技大学 | Detection method for adulterated sesame oil |
| CN105486662A (en) * | 2016-01-28 | 2016-04-13 | 浙江大学 | Cottonseed gossypol content non-destructive measurement method based on near-infrared spectrum technology |
-
2016
- 2016-08-31 CN CN201610772617.4A patent/CN106370619A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102279168A (en) * | 2011-07-20 | 2011-12-14 | 浙江大学 | Near-infrared spectroscopic technology-based method for fast and undamaged analysis of nutritional quality of whole cottonseed |
| CN104132905A (en) * | 2014-05-05 | 2014-11-05 | 河南科技大学 | Detection method for adulterated sesame oil |
| CN105486662A (en) * | 2016-01-28 | 2016-04-13 | 浙江大学 | Cottonseed gossypol content non-destructive measurement method based on near-infrared spectrum technology |
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| 张晓芳等: "近红外反射技术开放式检测棉籽中水分和油含量的研究", 《光谱学与光谱分析》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118032677A (en) * | 2024-04-09 | 2024-05-14 | 甘肃农业大学 | Method and system for testing processing quality of angelica freeze-dried product |
| CN118032677B (en) * | 2024-04-09 | 2024-06-07 | 甘肃农业大学 | Method and system for testing processing quality of angelica freeze-dried product |
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