CN110244003A - A method of gentianae macrophyllae grade is differentiated using electronic nose - Google Patents
A method of gentianae macrophyllae grade is differentiated using electronic nose Download PDFInfo
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Abstract
The present invention provides a kind of methods that gentianae macrophyllae grade is differentiated using electronic nose, the following steps are included: respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the standard sample of 2-3cm, it respectively weighs 1.50-3.00g standard sample to be fitted into ml headspace bottle, heats 30-60min in 40-50 DEG C of insulating box;The running parameter that electronic nose is arranged is 23-28 DEG C of environment temperature, and the head space time is 300-900s, testing time 180-200s, sampling interval duration 1-2s;Electronic nose examination criteria sample is counted using smell finger print information of the principal component analysis to different brackets gentianae macrophyllae, establishes odor identification model, analyzes the difference of different brackets gentianae macrophyllae smell.The grade of unknown sample is predicted by Assessing parameters analysis model.Gentianae macrophyllae commercial grade determination method of the invention, sample pre-treatments are simple, and finding speed is fast, and the commercial grade for being fully available for gentiana macrophylla medicine divides.
Description
Technical field
The invention belongs to electronic noses to test and analyze technical field, be related to a kind of side that gentianae macrophyllae grade is differentiated using electronic nose
Method.
Background technique
Gentianae macrophyllae is conventional Chinese medicine, first recorded in Shennong's Herbal, is classified as middle product, has wind-damp dispelling, removes obstruction in channels to relieve pain, moves back void
The effect of heat, clearing away damp-heat, higher medical value makes the long-term xcessive digging of people, and wild resource is caused greatly to be broken
Three-level national key protected plant that is bad, being put into " Key Protected medicinal material species register ", at present artificial growth Qin
Macrophylla has achieved success.
Chinese medicine is the raw material of the prepared slices of Chinese crude drugs and Chinese patent drug, and the safety that the superiority and inferiority of quality directly affects clinical application has
Effect, and Chinese medicine commercial specification grade is the mark of its quality good or not, but the commercial grade of gentiana macrophylla medicine kind divide mainly by
Experience, standard still use 1986 " 76 kinds of medicinal material commodity specification standards ", by personal sense organ, lack accuracy and
Objectivity, random larger, cause to circulate irregular quality of medicinal material in the market, commercial specification, grade are chaotic, need to adopt
With advanced quick detection means, gentiana macrophylla medicine kind commercial grade is distinguished, medicinal herb grower is instructed rationally to be planted, adopted
It receives, scientific divided rank, guarantees quality of medicinal material.
Electronic nose is that using multiple there is metal oxide semiconductor sensor of different nature to be combined into sensor array,
In conjunction with specific intelligent self-learning, a kind of smell bionic system constructed from recognition mode recognizer.When one or more wind
When taste substance passes through full-automatic electronic nose, " the smell fingerprint " of the flavor substance can be perceived by sensor and pass through special intelligence
Can algorithm for pattern recognition extract, utilize difference " smell fingerprint " information of different flavor substance, so that it may since distinguish, identification it is different
Gas sample, certain specific flavor substances can characterize just sample the different places of origin of raw materials, different goods receiving times,
Comprehensive quality information under the influence of the multivariables such as different processing conditions, different storage environments, therefore can use electronic nose pair
Different samples carry out discrimination differentiation.
Therefore, how to provide the method using electronic nose differentiation gentianae macrophyllae grade that one kind is accurate, easy is art technology
The problem of personnel's urgent need to resolve.
Summary of the invention
In view of this, the present invention provides a kind of accurate, easy methods for differentiating gentianae macrophyllae grade using electronic nose.In order to
Realize above-mentioned purpose, the present invention adopts the following technical scheme:
The present invention provides a kind of methods that gentianae macrophyllae grade is differentiated using electronic nose, comprising the following steps:
(1) respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the standard sample of 2-3cm, 1.50- is respectively weighed
3.00g standard sample is fitted into ml headspace bottle, heats 30-60min in 40-50 DEG C of insulating box;
(2) running parameter that electronic nose is arranged is 23-28 DEG C of environment temperature, and the head space time is 300-900s, testing time
For 180-200s, sampling interval duration 1-2s;
(3) electronic nose test sample is used, each standard sample 4 times parallel, sensor response characteristic information is extracted, with every
Maximum response is extracted on sensor as first eigenvector, the response of multiple moment points of response intensity large area is made
For second feature vector, respectively to electronic nose first eigenvector and second feature to amount data analyze, by 20 parts of Qin
Macrophylla first-class sample and 20 parts of second-class samples of gentianae macrophyllae establish odor identification (PCA) model as standard items, in odor identification analysis
On the basis of establish grade distinction (DFA) model to predict the grade of unknown sample.
Further, Radix Gentianae Marcrophyllae is first-class in above-mentioned gentianae macrophyllae first-class samples met national " 76 kinds of medicinal material commodity specification standards "
Specification standards, the total amount of gentiamarin and Loganic acid is 5.0% or more in the gentianae macrophyllae first-class sample.
Further, Radix Gentianae Marcrophyllae is second-class in the second-class samples met of above-mentioned gentianae macrophyllae national " 76 kinds of medicinal material commodity specification standards "
The total amount of specification standards, the second-class sample gentiamarin of the gentianae macrophyllae and Loganic acid is 2.5%-5.0%.
Gentianae macrophyllae first-class sample need to meet Radix Gentianae Marcrophyllae first-class specification standards in national " 76 kinds of medicinal material commodity specification standards ",
I.e. in cone or cylindrical, there are a longitudinal wrinkles, main root is coarse like chicken leg, radish, oxtail shape, surface lark or brown, matter
It is hard and crisp, section brownish red or brown color, center khaki, gas are special, bitter and puckery flavor, diameter 1.2cm or more under reed, no reed head,
Fibrous root impurity, damages by worms, goes mouldy, while the total amount of gentiamarin and Loganic acid is recorded by " Chinese Pharmacopoeia " 2015 version one
" gentianae macrophyllae " item under content assaying method measurement should be 5.0% or more.The second-class sample of gentianae macrophyllae need to meet national " 76 kinds of medicinal materials
Commercial specification standard " in the second-class specification standards of Radix Gentianae Marcrophyllae, i.e., in cone or it is cylindrical, have longitudinal wrinkles, main root is coarse seemingly
Chicken leg, radish, oxtail shape, surface lark or yellowish-brown, matter is hard and crisp, section brownish red or brown color, center khaki, gas
Special, bitter and puckery flavor, diameter 1.2cm under reed is hereinafter, minimum be not less than 0.6cm, and no reed head, impurity, damages by worms, goes mouldy at fibrous root, simultaneously
The total amount of gentiamarin and Loganic acid presses content assaying method under " Chinese Pharmacopoeia " version one " gentianae macrophyllae " item recorded in 2015
Measurement should be in 2.5%-5.0%.
The gas sensor array of electronic nose is to simulate the intranasal osmoreceptor cell of people, for experiencing gas when measurement
Taste information, the information that signal conditioning circuit exports sensor array are handled, and obtain the useful response signal of multidimensional, micro- place
Reason device is analyzed and processed multidimensional data using odor identification algorithm, and is obtained by algorithm for pattern recognition (PCA, DFA etc.)
The qualitative or quantitative analysis result of tested gas.
Principal component analysis (PCA) is under the premise of knowing nothing sample characteristics of for example, by carrying out to original data vector
Linear transformation, to find a kind of algorithm of the difference of sample room at certain visual angle.For excavating useful information, provide
Descriptive chart with different odor region and cluster.The algorithm does not lose any sample message, only by change reference axis
To achieve the purpose that distinguish sample.
Assessing parameters analyze (DFA), and it is in PCA to sample that DFA, which is a kind of statistical method for differentiating the affiliated type of sample,
A discriminant function is resettled after carrying out data analysis, is structure for differentiating any one known particular measurement index value
Established model and a kind of algorithm for identifying unknown sample.DFA can make the difference between similar group data most by mathematic(al) manipulation
It may reduce, expand as far as possible without the difference between similar group data, to establish the data model more preferably identified.
Further, above-mentioned gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are the dry root of gentianaceae plant gentianae macrophyllae,
The dry root moisture content of above-mentioned gentiana macrophylla medicine is 5.6%-6.2%.
The beneficial effects of the present invention are: electronic nose is applied to sentencing for the commercial specification grade of gentiana macrophylla medicine by the present invention for the first time
Not, by a large number of experiments, preferred optimal parameter setting range, under Parameter Conditions in the range, with known grades
Sample establishes grade distinction (DFA) model, and is verified with a large amount of unknown sample, differentiates result and the result that sample divides
It compares, accuracy rate minimum 97.5%.Using gentianae macrophyllae commercial grade determination method of the invention, sample pre-treatments are simple, measurement
Speed is fast, and the commercial grade for being fully available for gentiana macrophylla medicine divides.
Detailed description of the invention
Fig. 1 shows the PCA of gentianae macrophyllae first-class sample of the present invention to analyze recognition result;
Fig. 2 indicates that the PCA of the second-class sample of gentianae macrophyllae of the present invention analyzes recognition result;
The PCA analysis recognition result of Fig. 3 expression gentianae macrophyllae first-class sample of the present invention, second-class sample;
Fig. 4 indicates gentiana macrophylla medicine DFA grade distinction result of the present invention.
Specific embodiment
Principles and features of the present invention are described with the following Examples, the given examples are served only to explain the present invention,
It is not intended to limit the scope of the present invention.
Electronic nose instrument used in following embodiment is U.S. iNose electronic nose.Samples sources are Longde region in Ningxia gentianae macrophyllae
Planting base.
Embodiment 1
(1) respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the sample of 2cm, 1.50g sample dress is respectively weighed
Enter in ml headspace bottle, 30min, national " the 76 kinds of medicinal material commercial specifications of gentianae macrophyllae first-class samples met are heated in 40 DEG C of insulating boxs
Standard " in Radix Gentianae Marcrophyllae first-class specification standards, the total amount of gentiamarin and Loganic acid is 5.5% in the gentianae macrophyllae first-class sample.The Qin
The second-class specification standards of Radix Gentianae Marcrophyllae in the second-class samples met of Macrophylla national " 76 kinds of medicinal material commodity specification standards ", the second-class sample of the gentianae macrophyllae
The total amount of product gentiamarin and Loganic acid is 2.5%.Gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are gentianaceae plant gentianae macrophyllae
Dry root.
(2) be arranged electronic nose running parameter be 23 DEG C of environment temperature, the head space time be 300s, testing time 180s,
Sampling interval duration is 1s;
(3) electronic nose test sample, each sample 4 times parallel, sensor response characteristic information is extracted, from every sensor
Upper extraction maximum response is as first eigenvector, and the analog value of multiple moment points of response intensity large area is as second
Feature vector analyzes odiferous information data using principal component analysis (PCA), on the basis of PCA analysis, by gentianae macrophyllae one
Samples and the second-class sample of gentianae macrophyllae are waited as standard items and establishes DFA model, the grade of unknown sample is predicted by DFA model.
Embodiment 2
(1) respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the sample of 3cm, 3.00g sample dress is respectively weighed
Enter in ml headspace bottle, 60min, national " the 76 kinds of medicinal material commercial specifications of gentianae macrophyllae first-class samples met are heated in 50 DEG C of insulating boxs
Standard " in Radix Gentianae Marcrophyllae first-class specification standards, the total amount of gentiamarin and Loganic acid is 5.5% in the gentianae macrophyllae first-class sample.The Qin
The second-class specification standards of Radix Gentianae Marcrophyllae in the second-class samples met of Macrophylla national " 76 kinds of medicinal material commodity specification standards ", the second-class sample of the gentianae macrophyllae
The total amount of product gentiamarin and Loganic acid is 5.0%.Gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are gentianaceae plant gentianae macrophyllae
Dry root.
(2) be arranged electronic nose running parameter be 28 DEG C of environment temperature, the head space time be 900s, testing time 200s,
Sampling interval duration is 2s;
(3) electronic nose test sample, each sample 4 times parallel, sensor response characteristic information is extracted, from every sensor
Upper extraction maximum response is as first eigenvector, and the analog value of multiple moment points of response intensity large area is as second
Feature vector, using principal component analysis, linear discriminant analysis respectively to electronic nose first eigenvector and second feature to amount
Data are analyzed, and establish DFA model using gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae as standard items, by DFA model come
Predict the grade of unknown sample.
Embodiment 3
(1) respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the sample of 2cm, 1.50g sample dress is respectively weighed
Enter in ml headspace bottle, 35min, national " the 76 kinds of medicinal material commercial specifications of gentianae macrophyllae first-class samples met are heated in 402 DEG C of insulating boxs
Standard " in Radix Gentianae Marcrophyllae first-class specification standards, in the gentianae macrophyllae first-class sample total amount of gentiamarin and Loganic acid be 5.0% with
On.The second-class specification standards of Radix Gentianae Marcrophyllae in the second-class samples met of gentianae macrophyllae national " 76 kinds of medicinal material commodity specification standards ", the gentianae macrophyllae
The total amount of second-class sample gentiamarin and Loganic acid is 3%.Gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are gentianaceae plant
The dry root of gentianae macrophyllae.
(2) be arranged electronic nose running parameter be 24 DEG C of environment temperature, the head space time be 400s, testing time 185s,
Sampling interval duration is 1s;
(3) electronic nose test sample, each sample 4 times parallel, sensor response characteristic information is extracted, from every sensor
Upper extraction maximum response is as first eigenvector, and the analog value of multiple moment points of response intensity large area is as second
Feature vector analyzes odiferous information data using principal component analysis (PCA), on the basis of PCA analysis, by gentianae macrophyllae one
Samples and the second-class sample of gentianae macrophyllae are waited as standard items and establishes DFA model, the grade of unknown sample is predicted by DFA model.
Embodiment 4
(1) respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the sample of 3cm, 3.00g sample dress is respectively weighed
Enter in ml headspace bottle, 50min, national " the 76 kinds of medicinal material commercial specifications of gentianae macrophyllae first-class samples met are heated in 48 DEG C of insulating boxs
Standard " in Radix Gentianae Marcrophyllae first-class specification standards, in the gentianae macrophyllae first-class sample total amount of gentiamarin and Loganic acid be 5.0% with
On.The second-class specification standards of Radix Gentianae Marcrophyllae in the second-class samples met of gentianae macrophyllae national " 76 kinds of medicinal material commodity specification standards ", the gentianae macrophyllae
The total amount of second-class sample gentiamarin and Loganic acid is 4.5%.Gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are Gentianaceae plant
The dry root of object gentianae macrophyllae.
(2) be arranged electronic nose running parameter be 26 DEG C of environment temperature, the head space time be 800s, testing time 200s,
Sampling interval duration is 2s;
(3) electronic nose test sample, each sample 4 times parallel, sensor response characteristic information is extracted, from every sensor
Upper extraction maximum response is as first eigenvector, and the analog value of multiple moment points of response intensity large area is as second
Feature vector analyzes odiferous information data using principal component analysis (PCA), on the basis of PCA analysis, by gentianae macrophyllae one
Samples and the second-class sample of gentianae macrophyllae are waited as standard items and establishes DFA model, the grade of unknown sample is predicted by DFA model.
Embodiment 5
(1) respectively by gentianae macrophyllae first-class sample and the second-class sample shear of gentianae macrophyllae at the sample of 2cm, 2.00g sample dress is respectively weighed
Enter in ml headspace bottle, 50min, national " the 76 kinds of medicinal material commercial specifications of gentianae macrophyllae first-class samples met are heated in 45 DEG C of insulating boxs
Standard " in Radix Gentianae Marcrophyllae first-class specification standards, in the gentianae macrophyllae first-class sample total amount of gentiamarin and Loganic acid be 5.0% with
On.The second-class specification standards of Radix Gentianae Marcrophyllae in the second-class samples met of gentianae macrophyllae national " 76 kinds of medicinal material commodity specification standards ", the gentianae macrophyllae
The total amount of second-class sample gentiamarin and Loganic acid is 4%.Gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are gentianaceae plant
The dry root of gentianae macrophyllae.
(2) be arranged electronic nose running parameter be 25 DEG C of environment temperature, the head space time be 500s, testing time 190s,
Sampling interval duration is 1s;
(3) electronic nose test sample, each sample 4 times parallel, sensor response characteristic information is extracted, from every sensor
Upper extraction maximum response is as first eigenvector, and the analog value of multiple moment points of response intensity large area is as second
Feature vector analyzes odiferous information data using principal component analysis (PCA), on the basis of PCA analysis, by gentianae macrophyllae one
Samples and the second-class sample of gentianae macrophyllae are waited as standard items and establishes DFA model, the grade of unknown sample is predicted by DFA model.
Performance test
Establish grade distinction (DFA) model.Sample is gentianaceae plant gentianae macrophyllae Gentiana through base chiller
The dry root of macrophylla Pall., is divided into first-class, second-class 2 kinds of samples, and every kind 20 parts of sample, every part of about 50g.
First-class sample meets Radix Gentianae Marcrophyllae first-class specification standards in national " 76 kinds of medicinal material commodity specification standards ", simultaneously
The total amount of gentiamarin and Loganic acid presses content assaying method under " Chinese Pharmacopoeia " version one " gentianae macrophyllae " item recorded in 2015
Measurement is 5.0% or more.Second-class sample meets two isotactic of Radix Gentianae Marcrophyllae in national " 76 kinds of medicinal material commodity specification standards "
Case marker is quasi-, while the total amount of gentiamarin and Loganic acid presses " Chinese Pharmacopoeia " version one " gentianae macrophyllae " Xiang Xiahan recorded in 2015
Quantity measuring method measures in 2.5%-5.0%.
By sample shear at the consistent sample of 2cm length, 3g sample is weighed respectively and (is accurately packed into ml headspace bottle to 0.01g)
In, 45min is heated in 40 DEG C of insulating boxs, keeps smell to be checked full of standing in ml headspace bottle, each sample 4 times are parallel.Sample
Detection parameters are 23-28 DEG C of environment temperature, and the head space time is 600s, testing time 200s, sampling interval duration 1s.From every
Maximum response is extracted on root sensor as first eigenvector, the analog value of multiple moment points of response intensity large area
As second feature vector.Using principal component analysis (PCA), constructing, there is the descriptive figure of different brackets specification to see Fig. 1, Fig. 2.
Principal component analysis (PCA) the result shows that: the cumulative variance tribute of first-class sample first principal component (PC1) and Second principal component, (PC2)
Rate is offered up to 94%, 5.7%, wherein the sum of cumulative proportion in ANOVA of PC1 and PC2 is 99.7%, is greater than 85%, this illustrates PC1
With most information of PC2 included sample, it is able to reflect the Global Information of sample.Second-class sample first principal component
(PC1) and the cumulative proportion in ANOVA of Second principal component, (PC2) is up to 96.8%, 2.1%, the wherein cumulative variance tribute of PC1 and PC2
Offering the sum of rate is 98.9%, is greater than 85%, this illustrates most information of PC1 and PC2 included sample, is able to reflect sample
The Global Information of product.
Gentianae macrophyllae first-class sample of the present invention, second-class sample PCA analysis recognition result see Fig. 3, the results show that first principal component
Contribution rate be 90.4%, the contribution rate rate of Second principal component, is 8.2%, and adding up variance contribution ratio is 98.6%, contribution rate
Numerical value shows that the differentiation of sample is significant close to 1, and two principal components cover most of raw information of sample substantially, first-class
There are apparent differences on smell with second-class sample for sample, can carry out grade distinction using odiferous information.
Grade distinction (DFA) model is established using 20 parts of first-class samples and 20 parts of second-class samples as standard sample, passes through DFA
Model predicts grade that unknown sample belongs to.
The verifying of gentianae macrophyllae commercial specification grade discrimination model is carried out with electronic nose
20 parts of gentianae macrophyllae are taken, by sample shear at the consistent sample of 2cm length, weighs 3g sample respectively (accurately to 0.01g)
It is fitted into ml headspace bottle, heats 45min in 40 DEG C of insulating boxs, make smell full of in ml headspace bottle, stand to be checked, each sample 4 times
In parallel.The detection parameters of sample are 26 DEG C of environment temperature, and the head space time is 500s, testing time 200s, sampling interval duration
For 1s.
Data result inputs established grade distinction (DFA) model, as a result sees Fig. 4.The result shows that the present invention described
The classification accuracy of method product is 97.5%.Show that established DFA model for the gentiana macrophylla medicine of different commercial grades, has
Preferable Division identification ability, the popularization and application distinguished suitable for gentianae macrophyllae commercial grade.
Claims (4)
1. a kind of method for differentiating gentianae macrophyllae grade using electronic nose, which comprises the following steps:
(1) gentianae macrophyllae first-class sample and the second-class sample of gentianae macrophyllae are selected, it is every kind 20 parts of sample, every part of 45-55g, respectively that gentianae macrophyllae is first-class
Sample and the second-class sample shear of gentianae macrophyllae respectively weigh 1.50-3.00g standard sample and are fitted into ml headspace bottle at the standard sample of 2-3cm,
30-60min is heated in 40-50 DEG C of insulating box;
(2) running parameter that electronic nose is arranged is 23-28 DEG C of environment temperature, and the head space time is 300-900s, and the testing time is
180-200s, sampling interval duration 1-2s.
(3) electronic nose test sample is used, each standard sample 4 times parallel, extracts sensor response characteristic information, senses with every
Maximum response is extracted on device as first eigenvector, the responses of multiple moment points of response intensity large area is as the
Two feature vectors, respectively to electronic nose first eigenvector and second feature to amount data analyze, by 20 portions of gentianae macrophyllae one
Samples and 20 parts of second-class samples of gentianae macrophyllae are waited as standard items and establish odor identification model, are established on the basis of odor identification analysis
Grade distinction model predicts the grade of unknown sample.
2. a kind of method for differentiating gentianae macrophyllae grade using electronic nose according to claim 1, which is characterized in that the gentianae macrophyllae
First-class sample and the second-class sample of gentianae macrophyllae are the dry root of gentianaceae plant gentianae macrophyllae.
3. a kind of method for differentiating gentianae macrophyllae grade using electronic nose according to claim 2, which is characterized in that the gentianae macrophyllae
Radix Gentianae Marcrophyllae first-class specification standards in first-class samples met national " 76 kinds of medicinal material commodity specification standards ", the gentianae macrophyllae first-class sample
The total amount of middle gentiamarin and Loganic acid is 5.0% or more.
4. a kind of method for differentiating gentianae macrophyllae grade using electronic nose according to claim 2, which is characterized in that the gentianae macrophyllae
The second-class specification standards of Radix Gentianae Marcrophyllae in second-class samples met national " 76 kinds of medicinal material commodity specification standards ", the second-class sample of the gentianae macrophyllae
The total amount of gentiamarin and Loganic acid is 2.5%-5.0%.
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