CN103983605B - A kind of method of Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate - Google Patents
A kind of method of Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate Download PDFInfo
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Abstract
The invention provides a kind of method of Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate.The method comprises the steps: to adopt near infrared spectrometer to gather the near infrared spectrum data of sample to be tested; Multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of described sample to be tested; Choose 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, adopt the sporoderm-broken rate forecast model set up according to partial least-squares regression method to detect the sporoderm-broken rate of described sample to be tested.The advantage that the present invention has fast, accurate, harmless, cost is low, is beneficial to and popularizes, effectively can solve the problem of ganoderma spove powder sporoderm-broken rate quality monitoring.
Description
Technical field
The present invention relates to a kind of detection method of fungal spore sporoderm-broken rate, specifically a kind of method of Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate.
Background technology
Lucidum spore powder be glossy ganoderma in the growth and maturity phase, to be hit by a bullet the extremely small avette reproduction cell shot out from glossy ganoderma lamella, i.e. the seed of glossy ganoderma.It has condensed the elite of glossy ganoderma, has whole inhereditary material and the health-care effect of glossy ganoderma.The shell of lucidum spore powder comprises the two-layer sporoderm be made up of very hard chitin fiber element; Sporoderm quality is hard, and have the character such as acidproof alkali resistant, withstand voltage heat resistanceheat resistant, the anti-digestion of resistance to enzyme, therefore, the existence of sporoderm makes the active principle in lucidum spore powder be difficult to be absorbed by the body.By artificial machinery, physico-chemical process or biologic enzymolysis method, after the fragmentation of the sporoderm of lucidum spore powder or eliminating, the effective constituent wrapped tightly by sporoderm could farthest directly be absorbed by human body stomach.Have data to show, the lucidum spore powder after broken wall is conducive to the stripping of the compositions such as triterpene, Thick many candies, crude fat, and wherein Thick many candies content exceeds 70% than non-ganoderma spove powder.If the directly lucidum spore powder of edible non-broken wall, human body only can utilize the effective constituent of about 12%, and takes the lucidum spore powder after broken wall, and utilization rate of active components can reach more than 95%.Therefore, can the size of the sporoderm-broken rate of ganoderma spove powder be exactly the key point that utilize effective component of ganoderma lucidum spore powder to the full extent.For ganoderma spove powders numerous on market, sporoderm-broken rate is often by the important indicator as this product quality of measurement.
At present, the sporoderm-broken rate of ganoderma spove powder measures Primary Reference Ministry of Agriculture standard " mensuration of NY/T1677-2008 ganoderma spove powder sporoderm-broken rate " and national standard " GB/T29344-2012 lucidum spore powder is gathered and process technology specification " appendix A " assay method of ganoderma spove powder sporoderm-broken rate ".In these two standards, sporoderm-broken rate measuring principle is all counted by the spore of blood counting chamber to non-broken wall, calculate the quantity of intact spore in the quantity of intact spore in the non-ganoderma spove powder of unit mass and unit mass ganoderma spove powder respectively, thus obtain the sporoderm-broken rate of ganoderma spove powder.The operating process of this analytical approach is complicated, and minute is longer, and sample preparation and the counting process of blood counting chamber easily produce error, and the skill level for operator requires higher.
Except blood counting chamber method, the assay method of the sporoderm-broken rate of open report also has water load in conjunction with microtechnic detection method, suspension method in conjunction with physics technology detecting method and chemical fingerprint detection method etc. at present.Wherein, chemical fingerprint detection method breaches the restriction of artificial counting, redefines from composition to the detection mode of ganoderma spove powder sporoderm-broken rate.Due to the development of current chromatographic technique, measure sporoderm-broken rate by the analytical approach of component content and be not a problem, and its accuracy rate can be fully guaranteed; But the detecting step of component analyzing method is complicated, instrument is expensive, and sample is destroyed, and testing cost is higher.
Summary of the invention
Object of the present invention is just to provide a kind of method of Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate, to solve the problem that existing detection method step is complicated, cost is high and easily make sample be destroyed.
The present invention is achieved in that a kind of method of Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate, comprises the steps:
A, employing near infrared spectrometer gather the near infrared spectrum data of sample to be tested;
B, multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of described sample to be tested;
C, choose 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, adopt the sporoderm-broken rate forecast model set up according to partial least-squares regression method to detect the sporoderm-broken rate of described sample to be tested.
Described sporoderm-broken rate forecast model in described step c is:
Y＝A
0+A
1×X
1+A
2×X
2+A
3×X
3+A
4×X
4+A
5×X
5+A
6×X
6+A
7×X
7+A
8×X
8+A
9×X
9+A
10×X
10
In formula: Y is sporoderm-broken rate, A
0, A
1..., A
10be constant, X
1for spectroscopic data factor I score after principal component analysis (PCA) dimensionality reduction, X
2for spectroscopic data factor Ⅱ score after principal component analysis (PCA) dimensionality reduction, X
3for spectroscopic data factor III score after principal component analysis (PCA) dimensionality reduction, X
4for spectroscopic data CA++ score after principal component analysis (PCA) dimensionality reduction, X
5for spectroscopic data accelerator factor score after principal component analysis (PCA) dimensionality reduction, X
6for spectroscopic data factor Va score after principal component analysis (PCA) dimensionality reduction, X
7for spectroscopic data factor VII score after principal component analysis (PCA) dimensionality reduction, X
8for spectroscopic data Factor VIII score after principal component analysis (PCA) dimensionality reduction, X
9for spectroscopic data factor IX score after principal component analysis (PCA) dimensionality reduction, X
10for spectroscopic data factor X score after principal component analysis (PCA) dimensionality reduction; Described spectroscopic data is near infrared spectrum data 9411.6-5446.4cm after pretreatment
-1and 4613.2-4243cm
-1the data of two spectrum ranges.
Described sporoderm-broken rate forecast model in described step c is:
Y＝0.06866×X
1+0.046809×X
2+0.019892×X
3+0.125289×X
4+0.06593×X
5+0.019621×X
6+0.053336×X
7+0.018258×X
8+0.094993×X
9+0.079206×X
10
In formula: Y is sporoderm-broken rate, X
1for spectroscopic data factor I score after principal component analysis (PCA) dimensionality reduction, X
2for spectroscopic data factor Ⅱ score after principal component analysis (PCA) dimensionality reduction, X
3for spectroscopic data factor III score after principal component analysis (PCA) dimensionality reduction, X
4for spectroscopic data CA++ score after principal component analysis (PCA) dimensionality reduction, X
5for spectroscopic data accelerator factor score after principal component analysis (PCA) dimensionality reduction, X
6for spectroscopic data factor Va score after principal component analysis (PCA) dimensionality reduction, X
7for spectroscopic data factor VII score after principal component analysis (PCA) dimensionality reduction, X
8for spectroscopic data Factor VIII score after principal component analysis (PCA) dimensionality reduction, X
9for spectroscopic data factor IX score after principal component analysis (PCA) dimensionality reduction, X
10for spectroscopic data factor X score after principal component analysis (PCA) dimensionality reduction; Described spectroscopic data is near infrared spectrum data 9411.6-5446.4cm after pretreatment
-1and 4613.2-4243cm
-1the data of two spectrum ranges.
Described step a specifically comprises the steps:
A1, described sample to be tested to be dried 48 hours at 30 DEG C, then load in sample cup;
A2, employing Fourier transform near infrared instrument scan sample to be tested with diffuse reflectance mode, obtain sample to be tested at 12500-4000cm
-1spectroscopic data in scope; The scanning resolution of described Fourier transform near infrared instrument is 8cm
-1;
Average after a3, scanning testing sample 32 times.
The concrete construction method of sporoderm-broken rate forecast model described in described step c is as follows:
C1, choose some ganoderma spove powders with different sporoderm-broken rate as the training sample set up needed for sporoderm-broken rate forecast model;
C2, employing near infrared spectrometer gather the near infrared spectrum data of described training sample;
C3, blood counting chamber method is adopted to detect the sporoderm-broken rate of described training sample, using as the training sample sporoderm-broken rate reference value set up needed for sporoderm-broken rate forecast model;
C4, multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of described training sample, choose 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, in conjunction with described training sample sporoderm-broken rate reference value, adopt partial least-squares regression method to set up sporoderm-broken rate forecast model.
9411.6-5446.4cm in described step c4
-1and 4613.2-4243cm
-1two spectrum ranges to choose process specific as follows:
According to the load diagram of first three factor of described near infrared spectrum data principal component analysis (PCA), select several spectrum ranges that load value is larger, draw 9411.6-5446.4cm by optimum choice afterwards
-1and 4613.2-4243cm
-1two spectrum ranges.
Described step c2 specifically comprises the steps:
C21, described training sample to be dried 48 hours at 30 DEG C, then load in sample cup;
C22, employing Fourier transform near infrared instrument scan training sample with diffuse reflectance mode, obtain each training sample at 12500-4000cm
-1spectroscopic data in scope; The scanning resolution of described Fourier transform near infrared instrument is 8cm
-1;
C23, to average to after each training Sample Scan 32 times.
Described step c3 specifically comprises the steps:
C31, take non-ganoderma spove powder 0.01g, 0.02g, 0.03g, 0.04g and 0.05g dry 5h at 60 DEG C after respectively, be then respectively charged in 5 color comparison tubes;
C32, respectively take 5 parts through grinding after again through 100 mesh sieves screening after each 1.25g of sucrose powder, 5 parts of sucrose powder are added respectively in 5 color comparison tubes in described step c31, make the lucidum spore powder in the sucrose powder that adds and corresponding color comparison tube be mixed to color and luster homogeneous;
C33, in each color comparison tube, add distilled water to dissolve sucrose powder in corresponding color comparison tube and lucidum spore powder, backward each color comparison tube in add 0.2mL Tween 80, then with distilled water, each color comparison tube is settled to 25mL;
C34, at room temperature make each color comparison tube ultrasonic vibration 30min, period carries out manually rocking of several times every 10min to each color comparison tube, and the lucidum spore powder in each color comparison tube is fully disperseed;
C35, in each color comparison tube, draw 8.0 μ L lucidum spore powder suspending liquid respectively in the edge of 5 different cover glasses, utilize and inhale rainbow phenomenon and makes in the blood counting chamber grid below corresponding lid slide, to be full of corresponding lucidum spore powder suspending liquid;
C36, to leave standstill after 30s, adopt the optical microscope of 400 times of enlargement factors to add up the number containing complete lucidum spore powder in 4 drift angles and central authorities on each blood counting chamber totally 5 middle lattice respectively, average after statistics 5 times is observed to each blood counting chamber;
C37, with the quality of take in described step c1 5 parts of non-ganoderma spove powders for horizontal ordinate, to contain the number of complete lucidum spore powder in 5 middle lattice on each blood counting chamber added up in described step c36 for ordinate, make the typical curve of non-ganoderma spove powder quality and number;
C38, respectively take each at 60 DEG C, dry 5h after training sample 0.04g, put into different color comparison tubes; The number containing complete lucidum spore powder in 5 middle lattice on blood counting chamber corresponding to each training sample is added up respectively according to described step c32 ~ c36;
The number N of the complete lucidum spore powder of search quality corresponding to the non-ganoderma spove powder of 0.04g in c39, the typical curve drawn from described step c37
a, according to formula
Calculate the sporoderm-broken rate of each training sample; In formula: X is the sporoderm-broken rate of training sample, N
bfor the number containing complete lucidum spore powder in 5 middle lattice on the blood counting chamber that the training sample added up in described step c38 is corresponding.
When adopting the present invention to detect the sporoderm-broken rate of ganoderma spove powder, the time gathering spectroscopic data due near infrared spectrometer is very short, pre-service is carried out to spectroscopic data and adopts partial least-squares regression method to carry out time of calculation process also very short, therefore the sporoderm-broken rate of sample to be tested can easily, promptly be detected, and sample to be tested can not be made to be destroyed, to solve in current ganoderma spove powder sporoderm-broken rate testing process that existing operating process is complicated, the problem of easy more, the poor repeatability of destroyed, artificial labile factor etc. of sample.
Sample to be tested after detecting utilizing the present invention, the method recycling traditional blood counting chamber carries out the detection of sporoderm-broken rate, both testing results are compared, result shows, the sporoderm-broken rate of two kinds of method mensuration closely, relative deviation, between 0.7-8.6%, illustrates that lossless detection method that the present invention sets up accurately and reliably.
Lucidum spore powder is as high-end health products, and its price remains high always.The present invention's application near-infrared spectrum technique and multivariate statistics method carry out Fast nondestructive evaluation to ganoderma spove powder sporoderm-broken rate, greatly can reduce testing cost, improve detection speed, are beneficial to the quality monitoring of product.
Accompanying drawing explanation
Fig. 1 is the near infrared light spectrogram of training sample of the present invention.
Fig. 2 is the microphoto of non-ganoderma spove powder in the embodiment of the present invention.
Fig. 3 is the typical curve of non-ganoderma spove powder quality and number in the present invention.
Fig. 4 is the microphoto of training sample in the embodiment of the present invention.
Fig. 5 is the load diagram of first three factor of the near infrared spectrum major component of training sample in the embodiment of the present invention.
The correlativity figure that Fig. 6 is adopt the present invention to detect predicted value that training sample draws and adopts blood counting chamber method to detect between reference value that training sample draws.
Fig. 7 is the near infrared spectrum data of sample to be tested spectrogram after pretreatment in the embodiment of the present invention.
Embodiment
When the present invention carries out sporoderm-broken rate detection to ganoderma spove powder to be measured, near infrared spectrometer is first adopted to gather the near infrared spectrum data of sample to be tested; Afterwards multiplicative scatter correction pre-service is carried out to gathered near infrared spectrum data; Then 9411.6-5446.4cm after pre-service is chosen
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, adopt the sporoderm-broken rate forecast model set up according to partial least-squares regression method to detect the sporoderm-broken rate of sample to be tested.
The sporoderm-broken rate forecast model set up is:
Y＝A
0+A
1×X
1+A
2×X
2+A
3×X
3+A
4×X
4+A
5×X
5+A
6×X
6+A
7×X
7+A
8×X
8+A
9×X
9+A
10×X
10(1)
In formula (1): Y is sporoderm-broken rate, A
0, A
1..., A
10be constant, X
1for spectroscopic data factor I score after principal component analysis (PCA) dimensionality reduction, X
2for spectroscopic data factor Ⅱ score after principal component analysis (PCA) dimensionality reduction, X
3for spectroscopic data factor III score after principal component analysis (PCA) dimensionality reduction, X
4for spectroscopic data CA++ score after principal component analysis (PCA) dimensionality reduction, X
5for spectroscopic data accelerator factor score after principal component analysis (PCA) dimensionality reduction, X
6for spectroscopic data factor Va score after principal component analysis (PCA) dimensionality reduction, X
7for spectroscopic data factor VII score after principal component analysis (PCA) dimensionality reduction, X
8for spectroscopic data Factor VIII score after principal component analysis (PCA) dimensionality reduction, X
9for spectroscopic data factor IX score after principal component analysis (PCA) dimensionality reduction, X
10for spectroscopic data factor X score after principal component analysis (PCA) dimensionality reduction; Described spectroscopic data is near infrared spectrum data 9411.6-5446.4cm after pretreatment
-1and 4613.2-4243cm
-1the data of two spectrum ranges.
Below the contents such as the foundation of sporoderm-broken rate forecast model in the present invention, the concrete form of sporoderm-broken rate forecast model set up and the collection of near infrared spectrum data are described in detail.
Adopt partial least-squares regression method to set up sporoderm-broken rate forecast model, specifically comprise the steps:
A, choose some ganoderma spove powders with different sporoderm-broken rate as the training sample set up needed for sporoderm-broken rate forecast model.
B, employing near infrared spectrometer gather the near infrared spectrum data of training sample.
First some training samples selected in step a are dried 48 hours at 30 DEG C, then each training sample is respectively charged in a sample cup.Adopt German BRUKER company MPA type Fourier transform near infrared instrument to scan training sample in each sample cup respectively with diffuse reflectance mode afterwards, obtain each training sample at 12500-4000cm
-1spectroscopic data in scope.Tackle the noise of Fourier transform near infrared instrument, wavelength accuracy and reappearance before each scanning to diagnose; The scanning resolution of Fourier transform near infrared instrument is 8cm
-1, average after 32 times are scanned to each training sample.Adopt the near infrared spectrum data (mean value) of related software to gathered each training sample to process, the near infrared light spectrogram of each training sample can be drawn.The near infrared light spectrogram of each training sample is shown with reference to figure 1, Fig. 1.As seen from Figure 1, the near infrared light spectrogram of the ganoderma spove powder of different sporoderm-broken rate seems to be more or less the same, therefore directly can not analyze from spectrogram, but need to carry out pre-service to gathered near infrared spectrum data, partial least-squares regression method could be adopted to set up sporoderm-broken rate forecast model to realize the sporoderm-broken rate of Non-Destructive Testing ganoderma spove powder according to pretreated spectroscopic data afterwards.Concrete preprocess method and employing partial least-squares regression method set up sporoderm-broken rate forecast model can see steps d.
C, blood counting chamber method is adopted to detect the sporoderm-broken rate of training sample, using as the training sample sporoderm-broken rate reference value set up needed for sporoderm-broken rate forecast model.
This step can comprise again the several step of calculating of sample (non-ganoderma spove powder) dilution, film-making, counting, drawing standard curve and training sample sporoderm-broken rate, specific as follows:
The AR1140 type electronic balance (precision is 0.1mg) of c1, employing Mettler-Toledo Instrument (Shanghai) Co., Ltd. accurately takes non-ganoderma spove powder 0.01g, 0.02g, 0.03g, 0.04g and 0.05g dry 5h under 60 DEG C (± 1 DEG C) after respectively, is respectively charged in the color comparison tube of 5 25mL by taken 5 parts of non-ganoderma spove powders.During oven dry, instrument is that Beijing letter reaches a day square DHG-9023A type constant temperature blast drying oven.
In c2, employing step c1, electronic balance used takes 5 parts of each 1.25g of sucrose powder after grinding again after 100 mesh sieves screenings respectively, 5 parts of sucrose powder are added respectively in 5 color comparison tubes in step c1, make the lucidum spore powder in the sucrose powder that adds and corresponding color comparison tube be mixed to color and luster homogeneous.
C3, in each color comparison tube, add distilled water to dissolve sucrose powder in corresponding color comparison tube and lucidum spore powder, backward each color comparison tube in add 0.2mL Tween 80, then with distilled water, each color comparison tube is settled to 25mL.
The YQ-220D ultrasonic cleaner of c4, employing Shanghai Yi Jing ultrasonic instrument company limited, at room temperature make each color comparison tube ultrasonic vibration 30min, period carries out manually rocking of several times every 10min to each color comparison tube, and the lucidum spore powder in each color comparison tube is fully disperseed.
C5, respectively in each color comparison tube draw 8.0 μ L lucidum spore powder suspending liquid, respectively by the lucidum spore powder hanging drop of 5 part of 8.0 μ L at the edge of 5 cover glasses, utilize and inhale rainbow phenomenon and makes in the blood counting chamber grid below corresponding lid slide, to be full of corresponding lucidum spore powder suspending liquid.
Before draw lucidum spore powder suspending liquid in each color comparison tube, by hand color comparison tube, the lucidum spore powder in color comparison tube is uniformly dispersed, draws 8.0 μ L lucidum spore powder suspending liquid afterwards at once.The different lucidum spore powder suspending liquid drawn from 5 color comparison tubes is dripped the edge in 5 cover glasses respectively, and the below of each cover glass is provided with a blood counting chamber, that is: cover glass covers above blood counting chamber; Can make to be full of corresponding lucidum spore powder suspending liquid in each blood counting chamber grid by inhaling rainbow phenomenon.Grid on blood counting chamber comprises 25 middle lattice, and in each, lattice are divided into again 16 little lattice.
C6, make each lucidum spore powder suspending liquid in corresponding blood counting chamber grid leave standstill 30s, adopt the BX51 system optics microscope of OLYMPUS company afterwards, under 400 times of enlargement factors, observation counting is carried out to the number containing complete lucidum spore powder in 4 drift angles and central authorities on each blood counting chamber totally 5 middle lattice.With reference to figure 2, Fig. 2 shows the microphoto of non-ganoderma spove powder on one of them blood counting chamber (the non-ganoderma spove powder of corresponding 0.04g), can find out by figure, the equal ovalize of each lucidum spore powder is granular, namely without the lucidum spore powder of broken wall.
When the number of contained complete lucidum spore powder is added up in 5 middle lattice on blood counting chamber, if there is part lucidum spore powder to be on the sideline of middle lattice, the number of the lucidum spore powder be arranged on wherein two adjacent sidelines in lattice four sidelines during counting, should be added up.The larger value that peels off should be removed in statistic processes, counting effectively be observed 5 times to the number of complete lucidum spore powder contained in 5 middle lattice on each blood counting chamber, then calculates its mean value.
C7, with the quality of take in step c1 5 parts of non-ganoderma spove powders for horizontal ordinate, to contain the number of complete lucidum spore powder in 5 middle lattice on each blood counting chamber added up in step c6 for ordinate, make the typical curve of non-ganoderma spove powder quality and number, specifically see Fig. 3, the fit equation of typical curve shown in Fig. 3 is y=1706.6x-2.0173, and linearly dependent coefficient is R
2=0.999; As seen from Figure 3, the quality of non-ganoderma spove powder is directly proportional to number, and quality is larger, and contained by it, the number of complete lucidum spore powder is more.
C8, make all training samples all at 60 DEG C, dry 5h, take respectively afterwards each dry after training sample 0.04g, taken different training sample is put into different color comparison tubes respectively; The number containing complete lucidum spore powder in 5 middle lattice on blood counting chamber corresponding to each training sample is added up respectively according to step c2 ~ c6.With reference to figure 4, there is shown one of them training sample microphoto under an optical microscope, as can be seen from Figure, lucidum spore powder in training sample is a lot of all broken, thus form granular structure not of uniform size, by statistics the number of complete lucidum spore powder that remains, can the sporoderm-broken rate of calculation training sample.
The number N of the complete lucidum spore powder of search quality corresponding to the non-ganoderma spove powder of 0.04g in c9, the typical curve drawn from step c7
a, according to formula
Calculate the sporoderm-broken rate of each training sample; In formula (2): X is the sporoderm-broken rate of training sample, N
bfor the number containing complete lucidum spore powder in 5 middle lattice on the blood counting chamber that the training sample added up in step c8 is corresponding.
The sporoderm-broken rate value of all training samples calculated is as the training sample sporoderm-broken rate reference value set up needed for sporoderm-broken rate forecast model.
D, multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of training sample, choose 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, combined training sample sporoderm-broken rate reference value, adopts partial least-squares regression method to set up sporoderm-broken rate forecast model.
Conventional near infrared spectrum data preprocess method has multiplicative scatter correction method, First derivative spectrograply, vector normalization method, second derivative method, deduct straight line method, to eliminate Changshu Offset method of frequency measurement etc. multiple.In order to set up best sporoderm-broken rate forecast model, a kind of preprocess method of optimum should be selected; The preprocess method of this optimum, the raw information of each training sample of reservation that should be able to be maximum, can also reduce the impact of spectroscopic data by the factor such as random noise of uneven, the light scattering of training sample and instrument, improve precision of prediction and the stability of model.
Except choosing optimum preprocess method, also answer optimum choice characteristic spectrum interval and because of subnumber.
Near infrared spectrum is 12500-4000cm
-1spectrum range, it mainly reflects that the frequency multiplication of hydrogeneous group (as C-H, N-H, O-H etc.) and sum of fundamental frequencies absorb information.Choosing the characteristic spectrum interval in close relations with ganoderma spove powder sporoderm-broken rate is the effective ways improving forecast model accuracy.
The way substituted into piecemeal in all band has been abandoned in the selection in characteristic spectrum interval of the present invention, according to the load diagram (see Fig. 5) of first three factor of principal component analysis (PCA), selects several spectrum range (9411.6-5446.4cm that load value is larger
-1, 4613.2-4243cm
-1, 7513.9-6094.4cm
-1, 5461.8-4243cm
-1, 7436.7-5446.3cm
-1, 7513.9-5446.4cm
-1) be in optimized selection, thus greatly reduce the workload of characteristic spectrum interval selection.
In partial least-squares regressive analysis, huge data matrix will reduce to only several factor.Factor number will lose more information very little, and factor number is too large then can overfitting, therefore choose suitable to be very important because of subnumber.
Pass through orthogonal test, interval to different near infrared spectrum data preprocess method, characteristic spectrum and contrast because of subnumber respectively, comparing result is in table 1, and result shows, multiplicative scatter correction preprocess method is adopted, at 9411.6-5446.4cm near infrared spectrum data
-1and 4613.2-4243cm
-1data are chosen in two spectrum ranges, because of subnumber be 10 time, validation-cross root-mean-square error (RMSECV) is minimum, and what namely now adopt partial least-squares regression method to set up is used for predicting that the model performance of ganoderma spove powder sporoderm-broken rate is best, and the expression of this best model is:
A
0＝0；
Y＝0.06866×X
1+0.046809×X
2+0.019892×X
3+0.125289×X
4+0.06593×X
5+0.019621×X
6+0.053336×X
7+0.018258×X
8+0.094993×X
9+0.079206×X
10(3)
In formula (3): Y is sporoderm-broken rate, X
1for spectroscopic data factor I score after principal component analysis (PCA) dimensionality reduction, X
2for spectroscopic data factor Ⅱ score after principal component analysis (PCA) dimensionality reduction, X
3for spectroscopic data factor III score after principal component analysis (PCA) dimensionality reduction, X
4for spectroscopic data CA++ score after principal component analysis (PCA) dimensionality reduction, X
5for spectroscopic data accelerator factor score after principal component analysis (PCA) dimensionality reduction, X
6for spectroscopic data factor Va score after principal component analysis (PCA) dimensionality reduction, X
7for spectroscopic data factor VII score after principal component analysis (PCA) dimensionality reduction, X
8for spectroscopic data Factor VIII score after principal component analysis (PCA) dimensionality reduction, X
9for spectroscopic data factor IX score after principal component analysis (PCA) dimensionality reduction, X
10for spectroscopic data factor X score after principal component analysis (PCA) dimensionality reduction; Described spectroscopic data is near infrared spectrum data 9411.6-5446.4cm after pretreatment
-1and 4613.2-4243cm
-1the data of two spectrum ranges.
Under this condition, when the sporoderm-broken rate of lucidum spore powder is within the scope of 20.0-99.0%, sporoderm-broken rate predicted value and reference value correlativity are R
2=99.8, RMSECV=1.39 (see Fig. 6).
Table 1 partial least-squares regression method detects the condition optimizing result of ganoderma spove powder sporoderm-broken rate
After sporoderm-broken rate forecast model successfully constructs, when needing to carry out the detection of sporoderm-broken rate to sample to be tested, near infrared spectrometer only need be adopted to gather the near infrared spectrum data of sample to be tested, multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of sample to be tested, chooses 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, adopt above-mentioned set up sporoderm-broken rate forecast model to detect the sporoderm-broken rate of sample to be tested.
Choose 14 samples to be tested in the present embodiment, 14 samples to be tested are all dried 48 hours at 30 DEG C, is then respectively charged in different sample cups; Adopt Fourier transform near infrared instrument with the sample to be tested in diffuse reflectance mode scanning each sample cup, obtain each sample to be tested at 12500-4000cm
-1spectroscopic data in scope, the scanning resolution of Fourier transform near infrared instrument is 8cm
-1; Average after 32 times are scanned to each testing sample.
First the near infrared spectrum data (mean value) of 14 samples to be tested is carried out multiplicative scatter correction pre-service, showing sample number into spectrum with reference to figure 7, Fig. 7 is that the near infrared spectrum data of the sample to be tested of P01 is through the pretreated spectrogram of multiplicative scatter correction; In figure, interval A is 9411.6-5446.4cm
-1spectrum range, interval B is 4613.2-4243cm
-1spectrum range.After pre-service is carried out to the near infrared spectrum data of sample to be tested, choose from pretreated data and be positioned at 9411.6-5446.4cm
-1and 4613.2-4243cm
-1data in spectrum range, select because subnumber is 10, utilize partial least-squares regression method to draw front ten factor scores of selected spectroscopic data after principal component analysis (PCA) dimensionality reduction, namely draw X
1, X
2..., X
10, by X
1, X
2..., X
10in substitution formula (3), the sporoderm-broken rate of sample to be tested can be detected.
In order to verify that the present invention detects the accuracy of sporoderm-broken rate, after adopting the present invention to detect the sporoderm-broken rate of 14 samples to be tested, recycle traditional blood counting chamber method carries out sporoderm-broken rate detection to 14 samples to be tested, testing result is sporoderm-broken rate reference value, and the testing result of two kinds of methods is in table 2.Result shows, closely, relative deviation, between 0.7-8.6%, illustrates that lossless detection method that this invention sets up accurately and reliably to the sporoderm-broken rate that two kinds of methods measure.
The sporoderm-broken rate analysis result of table 2 sample to be tested
Claims (6)
1. a method for Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate, is characterized in that, comprises the steps:
A, employing near infrared spectrometer gather the near infrared spectrum data of sample to be tested;
B, multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of described sample to be tested;
C, choose 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, adopt the sporoderm-broken rate forecast model set up according to partial least-squares regression method to detect the sporoderm-broken rate of described sample to be tested;
Described sporoderm-broken rate forecast model in described step c is:
Y＝0.06866×X
1+0.046809×X
2+0.019892×X
3+0.125289×X
4+0.06593×X
5+0.019621×X
6+0.053336×X
7+0.018258×X
8+0.094993×X
9+0.079206×X
10
In formula: Y is sporoderm-broken rate, X
1for spectroscopic data factor I score after principal component analysis (PCA) dimensionality reduction, X
2for spectroscopic data factor Ⅱ score after principal component analysis (PCA) dimensionality reduction, X
3for spectroscopic data factor III score after principal component analysis (PCA) dimensionality reduction, X
4for spectroscopic data CA++ score after principal component analysis (PCA) dimensionality reduction, X
5for spectroscopic data accelerator factor score after principal component analysis (PCA) dimensionality reduction, X
6for spectroscopic data factor Va score after principal component analysis (PCA) dimensionality reduction, X
7for spectroscopic data factor VII score after principal component analysis (PCA) dimensionality reduction, X
8for spectroscopic data Factor VIII score after principal component analysis (PCA) dimensionality reduction, X
9for spectroscopic data factor IX score after principal component analysis (PCA) dimensionality reduction, X
10for spectroscopic data factor X score after principal component analysis (PCA) dimensionality reduction; Described spectroscopic data is near infrared spectrum data 9411.6-5446.4cm after pretreatment
-1and 4613.2-4243cm
-1the data of two spectrum ranges.
2. the method for Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate according to claim 1, it is characterized in that, described step a specifically comprises the steps:
A1, described sample to be tested to be dried 48 hours at 30 DEG C, then load in sample cup;
A2, employing Fourier transform near infrared instrument scan sample to be tested with diffuse reflectance mode, obtain sample to be tested at 12500-4000cm
-1spectroscopic data in scope; The scanning resolution of described Fourier transform near infrared instrument is 8cm
-1;
Average after a3, scanning testing sample 32 times.
3. the method for Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate according to claim 1, is characterized in that, the concrete construction method of sporoderm-broken rate forecast model described in described step c is as follows:
C1, choose some ganoderma spove powders with different sporoderm-broken rate as the training sample set up needed for sporoderm-broken rate forecast model;
C2, employing near infrared spectrometer gather the near infrared spectrum data of described training sample;
C3, blood counting chamber method is adopted to detect the sporoderm-broken rate of described training sample, using as the training sample sporoderm-broken rate reference value set up needed for sporoderm-broken rate forecast model;
C4, multiplicative scatter correction pre-service is carried out to the near infrared spectrum data of described training sample, choose 9411.6-5446.4cm after pre-service
-1and 4613.2-4243cm
-1the data of two spectrum ranges, under being the condition of 10 because of subnumber, in conjunction with described training sample sporoderm-broken rate reference value, adopt partial least-squares regression method to set up sporoderm-broken rate forecast model.
4. the method for Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate according to claim 3, is characterized in that, 9411.6-5446.4cm in described step c4
-1and 4613.2-4243cm
-1two spectrum ranges to choose process specific as follows:
According to the load diagram of first three factor of described near infrared spectrum data principal component analysis (PCA), select several spectrum ranges that load value is larger, draw 9411.6-5446.4cm by optimum choice afterwards
-1and 4613.2-4243cm
-1two spectrum ranges.
5. the method for Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate according to claim 3, it is characterized in that, described step c2 specifically comprises the steps:
C21, described training sample to be dried 48 hours at 30 DEG C, then load in sample cup;
C22, employing Fourier transform near infrared instrument scan training sample with diffuse reflectance mode, obtain each training sample at 12500-4000cm
-1spectroscopic data in scope; The scanning resolution of described Fourier transform near infrared instrument is 8cm
-1;
C23, to average to after each training Sample Scan 32 times.
6. the method for Fast nondestructive evaluation ganoderma spove powder sporoderm-broken rate according to claim 3, it is characterized in that, described step c3 specifically comprises the steps:
C31, take non-ganoderma spove powder 0.01g, 0.02g, 0.03g, 0.04g and 0.05g dry 5h at 60 DEG C after respectively, be then respectively charged in 5 color comparison tubes;
C32, respectively take 5 parts through grinding after again through 100 mesh sieves screening after each 1.25g of sucrose powder, 5 parts of sucrose powder are added respectively in 5 color comparison tubes in described step c31, make the lucidum spore powder in the sucrose powder that adds and corresponding color comparison tube be mixed to color and luster homogeneous;
C33, in each color comparison tube, add distilled water to dissolve sucrose powder in corresponding color comparison tube and lucidum spore powder, backward each color comparison tube in add 0.2mL Tween 80, then with distilled water, each color comparison tube is settled to 25mL;
C34, at room temperature make each color comparison tube ultrasonic vibration 30min, period carries out manually rocking of several times every 10min to each color comparison tube, and the lucidum spore powder in each color comparison tube is fully disperseed;
C35, in each color comparison tube, draw 8.0 μ L lucidum spore powder suspending liquid respectively in the edge of 5 different cover glasses, utilize and inhale rainbow phenomenon and makes in the blood counting chamber grid below corresponding lid slide, to be full of corresponding lucidum spore powder suspending liquid;
C36, to leave standstill after 30s, adopt the optical microscope of 400 times of enlargement factors to add up the number containing complete lucidum spore powder in 4 drift angles and central authorities on each blood counting chamber totally 5 middle lattice respectively, average after statistics 5 times is observed to each blood counting chamber;
C37, with the quality of take in described step c31 5 parts of non-ganoderma spove powders for horizontal ordinate, to contain the number of complete lucidum spore powder in 5 middle lattice on each blood counting chamber added up in described step c36 for ordinate, make the typical curve of non-ganoderma spove powder quality and number;
C38, respectively take each at 60 DEG C, dry 5h after training sample 0.04g, put into different color comparison tubes; The number containing complete lucidum spore powder in 5 middle lattice on blood counting chamber corresponding to each training sample is added up respectively according to described step c32 ~ c36;
The number N of the complete lucidum spore powder of search quality corresponding to the non-ganoderma spove powder of 0.04g in c39, the typical curve drawn from described step c37
a, according to formula
Calculate the sporoderm-broken rate of each training sample; In formula: X is the sporoderm-broken rate of training sample, N
bfor the number containing complete lucidum spore powder in 5 middle lattice on the blood counting chamber that the training sample added up in described step c38 is corresponding.
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| CN101446581A (en) * | 2008-10-06 | 2009-06-03 | 福建仙芝楼生物科技有限公司 | Method for measuring wall breaking rate of ganoderma lucidum spores |
| CN102768195A (en) * | 2012-06-29 | 2012-11-07 | 杭州中美华东制药有限公司 | Method for quickly detecting moisture content of cordyceps mycelia powder |
| CN102768194A (en) * | 2012-06-29 | 2012-11-07 | 杭州中美华东制药有限公司 | Method for quickly detecting adenosine content of cordyceps mycelia powder |
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| CN101446581A (en) * | 2008-10-06 | 2009-06-03 | 福建仙芝楼生物科技有限公司 | Method for measuring wall breaking rate of ganoderma lucidum spores |
| CN102768195A (en) * | 2012-06-29 | 2012-11-07 | 杭州中美华东制药有限公司 | Method for quickly detecting moisture content of cordyceps mycelia powder |
| CN102768194A (en) * | 2012-06-29 | 2012-11-07 | 杭州中美华东制药有限公司 | Method for quickly detecting adenosine content of cordyceps mycelia powder |
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| 灵芝孢子油制取工艺的研究;张新新;《中国优秀硕士学位论文全文数据库》;20140215(第02期);第1-80页 * |
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