CN103235029B - Chinese herbal processing process identification method based on sparse recognition algorithm and time-of-flight mass spectrometry - Google Patents
Chinese herbal processing process identification method based on sparse recognition algorithm and time-of-flight mass spectrometry Download PDFInfo
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Abstract
The invention discloses a Chinese herbal processing process identification method based on a sparse recognition algorithm and a time-of-flight mass spectrometry. According to the method, a time-of-flight mass spectrometry technology is adopted as a detection method and a sparse code compression sensing theory is adopted as a foundation to construct a recognition method, and a pattern recognition technology and a spectrogram analysis technology are combined so as to provide a method widely used for Chinese herbal processing product identification, wherein experiment results show that the method has characteristics of high detection efficiency, high detection sensitivity, and accurate and reliable detection result, and provides important significance for Chinese herbal processing product quality control and clinical medication safety assurance, and an application range is wide.
Description
Technical field
The discrimination method of a kind of Chinese herbal medicine processed product involved in the present invention, is specifically related to a kind of discrimination method of the Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum.
Background technology
Chinese medicine in the medical history of the Chinese nation in occupation of irreplaceable status, for multiplying and living of the Chinese nation has made indelible contribution.China is one of the world four great tradition medicine systems (China, Egypt, Greece and India), and traditional Chinese medicine is the system that theory is the most complete, medical practice is the abundantest, curative effect is the most definite.
Chinese crude drug mostly is the dry organ of plant, because the physical environment of complexity, social condition and people are for the reason such as obscuring, causes the complicacy of Chinese crude drug in application aspect.The Chinese crude drug of the same race of different concocting method, the activity chemistry component contained by them is discrepant identical, and this will inevitably have influence on clinical efficacy and the quality of the Chinese patent drug (compound Chinese medicinal preparation) produced using it as raw material.
Along with progress and the development of modern instrument isolation technics and Computerized Information Processing Tech, set up the important step that Chinese medicine modern mass appraisement system has become modernization of Chinese medicine development.The traditional Chinese medicine fingerprint Quality Control technical research carried out in conjunction with the present Research of International Plant drug assessment method, become field the most popular in traditional Chinese medicine research, control and a kind of effective means of quality assessment as traditional Chinese medicine quality, it can from raw-materially introducing a fine variety, cultivate, the specification of Chinese patent drug production technology and optimization, formulation to target level of product quality provides omnibearing quality assurance, traditional Chinese medicine fingerprint be a kind of comprehensively, quantifiable chemical identification means.So as to evaluating the authenticity of Chinese crude drug and Chinese medicine preparation semi-manufactured goods quality, Optimality and stability, " globality " and " ambiguity " is its distinguishing feature.Its not only characteristic embodiment but also Qualitive test can be used as use, the also concept of the amount of embodying, the concept of introduction volume, quantitatively and qualitative combining traditional Chinese medicine fingerprint can be made to have larger effect.
At present, quality control centered by chemical composition is mainly concentrated on to the traditional Chinese medicine fingerprint of Chinese herbal medicine processed product quality assessment, namely clear with molecular structure, medicinal materials fingerprint is set up based on the known active component that structure-activity relationship is clear and definite, to detect, the shortcomings such as there is reference substance deficiency, trace routine is loaded down with trivial details, and detection efficiency is not high.
Therefore, necessary on the basis of prior art, research relates to a kind of simple operation, and reference substance demand is few, and energy is accurate, quick, the new method of comprehensive identification Chinese herbal medicine processed product.
Summary of the invention
Goal of the invention: the object of the invention is to solve the deficiencies in the prior art, there is provided a kind of reference substance demand few, detection speed is fast, simple to operate, favorable repeatability, highly sensitive, can accurately, fast, the discrimination method based on sparse recognition algorithm and flight time mass spectrum of the different Chinese herbal medicine processed product of efficient qualification.
The present invention adopts flight time mass spectrum mass analyzer to be analysis means, compared with the mass analyzer of other types, time of flight mass analyzer neither needs magnetic field, do not need the scanning of electric field, have that structure is simple, analysis speed is fast yet, resolution and highly sensitive, that mass range is wide advantage.It adopts soft ionization source technology that the fragmention of ionization is greatly reduced, and simplifies spectrum analysis, the identification capacity of mass spectrum to complex mixture is greatly improved.
Technical scheme: in order to reach above object, the technical scheme that the present invention takes is:
Based on the discrimination method of the Chinese herbal medicine processing procedure of sparse recognition algorithm and flight time mass spectrum, comprise the pre-treatment of Chinese herbal medicine processed product, the spectrogram information collection of Chinese herbal medicine processed product flight time mass spectrum and spectrum analysis and sparse recognition algorithm;
(1) pre-treatment of Chinese herbal medicine processed product comprises the following steps:
Add ethanol after getting the pulverizing of Chinese herbal medicine processed product, drying, adopt ultrasonic extraction or soxhlet extraction, merge extract, concentrated, solution obtains test sample after crossing 0.45 μm of filter membrane;
Preferably, described heating and refluxing extraction method: get 10g Chinese herbal medicine processed product powder (as the Radix Astragali) in 250mL round-bottomed flask, add the ethanol water heating and refluxing extraction 2 hours that 100mL concentration is 70%, extract is evaporated near dry, also constant volume is in 5mL measuring bottle to add methyl alcohol dissolving, and solution obtains need testing solution after crossing 0.45 μm of filter membrane;
Preferably, described soxhlet extraction: get 10g Chinese herbal medicine processed product (as the Radix Astragali) in apparatus,Soxhlet's, add concentration be 70% ethanol water appropriate, refluxing extraction 6 hours, extract is evaporated near dry, also constant volume is in 5mL measuring bottle to add methyl alcohol dissolving, and solution obtains need testing solution after crossing 0.45 μm of filter membrane;
(2) collection of Chinese herbal medicine processed product flight time mass spectrum spectrogram information comprises the following steps:
In the sample injection bottle of 10mL, load the need testing solution of 1mL, under adopting room temperature, the direct Head-space sampling of atmospheric pressure kapillary is analyzed, major parameter condition: ionization mode: Single-photon ionization; Be evacuated to 0.8X10
-3pa ~ 1.8X10
-3pa; Ionized region air pressure 7.0 ~ 8.0Pa; Accelerating region voltage is 2650 ~ 2700V, and 250 micron capillary column direct injected, without heating measures; Often opening the TOF mass spectrum full From Spectral Signal cumulative time is 15s;
(3) spectral data analysis and sparse recognition algorithm comprise the following steps:
Sparse recognition algorithm is using the perception data of the original spectrogram of Chinese herbal medicine processed product flight time mass spectrum as feature interpretation, then under bringing the compressed sensing feature of Chinese herbal medicine processed product test sample book and Chinese herbal medicine processed product training sample set the framework of sparse identification into, and by solving a l
1induce one norm optimization problem to obtain classification results, specific as follows:
First, be vector description x ∈ R by Chinese herbal medicine processed product test sample book image stretch
n;
Secondly, by k class Chinese herbal medicine processed product training sample, every class n, carry out same stretching composition Chinese herbal medicine processed product training sample set X:
X=[X
(1),X
(2),…,X
(k)]∈R
n×k
X
(i)=[x
1 (i),x
2 (i),…,x
n (i)],i=1,…,k
Wherein
represent the i-th class jth Chinese herbal medicine processed product training sample;
Again, according to
Carry out the sampling of compressed sensing, wherein Φ determines perception matrix or observing matrix for owing, and y is called the perception data of x;
Chinese herbal medicine processed product test sample book x and Chinese herbal medicine processed product training sample set X is projected to aware space, on this basis in conjunction with formula
min||r||
1s.t.Xr=x
Carry out l
1norm solves:
y=Φx,Y=ΦX
min||r||
1s.t.Yr=ΦXr=Φx=y
Wherein y is the perception data of Chinese herbal medicine processed product test sample book, and Y is the compressed sensing matrix of the perception data composition of Chinese herbal medicine processed product training sample, and Φ plays the effect that dimension about subtracts in formula;
Finally, each classification subset in the element of r is sued for peace, chooses the taxonomic identification result of maximal value as Chinese herbal medicine processed product test sample book x:
Wherein element
for the correlation degree tolerance of a class jth Chinese herbal medicine processed product training sample in raw data territory i-th under aware space.
Preferably, the discrimination method of the above-described Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum, the ethanol described in step (1) is concentration 30 ~ 95%.
Preferably, the discrimination method of the above-described Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum, the collection of step (2) flight time mass spectrum spectrogram information comprises the following steps:
In the sample injection bottle of 10mL, load the need testing solution of 1mL, under adopting room temperature, the direct Head-space sampling of atmospheric pressure kapillary is analyzed, major parameter condition: ionization mode: Single-photon ionization; Be evacuated to 0.8X10
-3pa ~ 1.8X10
-3pa; Ionized region air pressure 7.0Pa; Accelerating region voltage is 2650V, and 250 micron capillary column direct injected, without heating measures; Often opening the TOF mass spectrum full From Spectral Signal cumulative time is 15s.
Preferably, the discrimination method of the above-described Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum, can be widely used in the discriminating of different Chinese herbal medicine processed product, described Chinese herbal medicine processed product is preparing astragalus membranaceus and wine astragalus root etc.
Beneficial effect: the discrimination method of the Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum provided by the invention, the method take ionization time of flight as detection means, recognition methods is built based on sparse coding compressive sensing theory, mode identification technology is combined with spectrum analysis technology, proposes one and be widely used in Chinese herbal medicine processed product mirror method for distinguishing.Experimental result shows, the method detection efficiency is high, and detection sensitivity is high, and testing result accurately and reliably, for controlling the quality of Chinese medicine preparation product, ensureing that clinical drug safety is significant, having wide range of applications.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Based on the discrimination method of the Chinese herbal medicine processing procedure of sparse recognition algorithm and flight time mass spectrum, comprise the pre-treatment of Chinese herbal medicine processed product, the spectrogram information collection of Chinese herbal medicine processed product flight time mass spectrum and spectrum analysis and sparse recognition algorithm;
(1) preparing astragalus membranaceus and the pre-treatment of wine astragalus root comprise the following steps:
Get preparing astragalus membranaceus and each 40 batches of wine astragalus root medicine materical crude slice sample, pulverize, get 10g preparing astragalus membranaceus and wine astragalus root medicine materical crude slice respectively in 250mL round-bottomed flask, add the ethanol water heating and refluxing extraction 2 hours that 100mL concentration is 70%, extract is evaporated near dry, also constant volume is in 5mL measuring bottle to add methyl alcohol dissolving, and solution obtains preparing astragalus membranaceus and wine astragalus root need testing solution after crossing 0.45 μm of filter membrane;
(2) preparing astragalus membranaceus and the collection of wine astragalus root flight time mass spectrum spectrogram information comprise the following steps:
In the sample injection bottle of 10mL, be respectively charged into step (1) 40 batch of preparing astragalus membranaceus and the wine astragalus root need testing solution of 1mL, under adopting room temperature respectively, the direct Head-space sampling of atmospheric pressure kapillary is analyzed, major parameter condition: ionization mode: Single-photon ionization; Be evacuated to 0.8X10
-3pa ~ 1.8X10
-3pa; Ionized region air pressure 7.0Pa; Accelerating region voltage is 2650V, and 250 micron capillary column direct injected, without heating measures; Often opening the TOF mass spectrum full From Spectral Signal cumulative time is 15s;
(3) spectral data analysis and sparse recognition algorithm comprise the following steps:
Sparse recognition algorithm is using the perception data of preparing astragalus membranaceus and the original spectrogram of wine astragalus root flight time mass spectrum as feature interpretation, then by preparing astragalus membranaceus and wine astragalus root test sample book 10 batches and preparing astragalus membranaceus and wine astragalus root training sample 40 batches, compressed sensing feature bring the framework of sparse identification under, and by solving a l
1draw youngster's norm optimization problem to obtain classification results, specific as follows:
First, 40 batches of preparing astragalus membranaceus and wine astragalus root sample image are stretched as vector description x ∈ R
n;
Secondly, by preparing astragalus membranaceus and wine astragalus root training sample, every class 40, carry out same stretching composition preparing astragalus membranaceus and wine astragalus root training sample set X:
X=[X
(1),X
(2),…,X
(k)]∈R
n×k
X
(i)=[x
1 (i),x
2 (i),…,x
x (i)],i=1,…,k
Wherein
represent the i-th class jth middle preparing astragalus membranaceus and wine astragalus root training sample;
Again, according to
Carry out the sampling of compressed sensing, wherein Φ determines perception matrix or observing matrix for owing, and y is called the perception data of x;
Preparing astragalus membranaceus and wine astragalus root test sample book x and preparing astragalus membranaceus and wine astragalus root training sample set X are projected to aware space, on this basis in conjunction with formula:
min||r||
1s.t.Xr=x
Carry out l
1norm solves:
y=Φx,Y=ΦX
min||r||
1s.t.Yr=ΦXr=Φx=y
Wherein y is the perception data of preparing astragalus membranaceus and wine astragalus root test sample book, and Y is the compressed sensing matrix of the perception data composition of preparing astragalus membranaceus and wine astragalus root training sample, and Φ plays the effect that dimension about subtracts in formula;
Finally, each classification subset in the element of r is sued for peace, chooses the taxonomic identification result of maximal value as preparing astragalus membranaceus and wine astragalus root test sample book x:
Wherein element
for the correlation degree tolerance of a class jth Chinese herbal medicine processed product training sample in raw data territory i-th under aware space.
The taxonomic identification result of 10 batches of preparing astragalus membranaceus and wine astragalus root test sample book is as shown in table 1:
The taxonomic identification result of table 1 10 batches of preparing astragalus membranaceus and wine astragalus root test sample book
Processed product | Test sample book number | The sample number of correct identification | Discrimination | Accuracy |
Preparing astragalus membranaceus | 10 | 10 | 100% | 100% |
Wine astragalus root | 10 | 10 | 100% | 100% |
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. based on the discrimination method of the Chinese herbal medicine processing procedure of sparse recognition algorithm and flight time mass spectrum, it is characterized in that comprising the pre-treatment of Chinese herbal medicine processed product, the spectrogram information collection of Chinese herbal medicine processed product flight time mass spectrum and spectrum analysis and sparse recognition algorithm;
(1) pre-treatment of Chinese herbal medicine processed product comprises the following steps:
Add ethanol after getting the pulverizing of Chinese herbal medicine processed product, drying, adopt ultrasonic extraction or soxhlet extraction, merge extract, concentrated, solution obtains test sample after crossing 0.45 μm of filter membrane;
(2) collection of Chinese herbal medicine processed product flight time mass spectrum spectrogram information comprises the following steps:
In the sample injection bottle of 10mL, load the need testing solution of 1mL, under adopting room temperature, the direct Head-space sampling of atmospheric pressure kapillary is analyzed, major parameter condition: ionization mode: Single-photon ionization; Be evacuated to 0.8X10
-3pa ~ 1.8X10
-3pa; Ionized region air pressure 7.0 ~ 8.0Pa; Accelerating region voltage is 2650 ~ 2700V, and 250 micron capillary column direct injected, without heating measures; Often opening the TOF mass spectrum full From Spectral Signal cumulative time is 15s;
(3) spectral data analysis and sparse recognition algorithm comprise the following steps:
First, be vector description x ∈ R by Chinese herbal medicine processed product test sample book image stretch
n;
Secondly, by k class Chinese herbal medicine processed product training sample, every class n, carry out same stretching composition Chinese herbal medicine processed product training sample set X:
X=[X
(1),X
(2),…,X
(k)]∈R
n×k
X
(i)=[x
1 (i),x
2 (i),…,x
n (i)],i=1,…,k
Wherein
represent the i-th class jth Chinese herbal medicine processed product training sample;
Again, according to
Carry out the sampling of compressed sensing, wherein Φ determines perception matrix or observing matrix for owing, and y is called the perception data of x;
Chinese herbal medicine processed product test sample book x and Chinese herbal medicine processed product training sample set X is projected to aware space, on this basis in conjunction with formula
min||r||
1s.t. Xr=x
Carry out l
1norm solves:
y=Φx,Y=ΦX
min||r||
1s.t. Yr=ΦXr=Φx=y
Wherein y is the perception data of Chinese herbal medicine processed product test sample book, and Y is the compressed sensing matrix of the perception data composition of Chinese herbal medicine processed product training sample, and Φ plays the effect that dimension about subtracts in formula;
Finally, each classification subset in the element of r is sued for peace, chooses the taxonomic identification result of maximal value as Chinese herbal medicine processed product test sample book x:
Wherein element
for the correlation degree tolerance of a class jth Chinese herbal medicine processed product training sample in raw data territory i-th under aware space.
2. the discrimination method of the Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum according to claim 1, it is characterized in that, the collection of step (2) flight time mass spectrum spectrogram information comprises the following steps:
In the sample injection bottle of 10mL, load the need testing solution of 1mL, under adopting room temperature, the direct Head-space sampling of atmospheric pressure kapillary is analyzed, major parameter condition: ionization mode: Single-photon ionization; Be evacuated to 0.8X10
-3pa ~ 1.8X10
-3pa; Ionized region air pressure 7.0Pa; Accelerating region voltage is 2650V, and 250 micron capillary column direct injected, without heating measures; Often opening the TOF mass spectrum full From Spectral Signal cumulative time is 15s.
3. the discrimination method of the Chinese herbal medicine processing procedure based on sparse recognition algorithm and flight time mass spectrum according to claim 1, it is characterized in that, described Chinese herbal medicine processed product is preparing astragalus membranaceus and wine astragalus root.
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Effective date of registration: 20210514 Address after: 210046 12th floor, building B2, Huizhi Science Park, Hengtai Road, Nanjing Economic and Technological Development Zone, Nanjing City, Jiangsu Province Patentee after: Nanjing Pulian life science and Technology Research Institute Co.,Ltd. Address before: 210046 No.3, Wenyuan Road, Qixia District, Nanjing City, Jiangsu Province Patentee before: JIANGSU PROVINCE INSTITUTE OF QUALITY & SAFETY ENGINEERING |