CN104089915A - Method for detecting total flavone in production of herba epimedii - Google Patents
Method for detecting total flavone in production of herba epimedii Download PDFInfo
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- CN104089915A CN104089915A CN201410339050.2A CN201410339050A CN104089915A CN 104089915 A CN104089915 A CN 104089915A CN 201410339050 A CN201410339050 A CN 201410339050A CN 104089915 A CN104089915 A CN 104089915A
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Abstract
The invention discloses a method for detecting total flavone in the production of herba epimedii. The method comprises the following steps: (1) preparing a herba epimedii extraction solution and sampling; (2) collecting a near infrared spectrum corresponding to a spectrum by using an AOTF (Acousto Optic Tunable Filter) near-infrared spectroscopy; (3) collecting the content of the total flavone in the collected samples by using an ultraviolet spectrophotometry in an offline manner; (4) associating near-infrared spectroscopic data and off-line detection data by using mathematical measuring software, and establishing a correction model; (5) detecting the content of the total flavone in the extraction solution in the production process by using the established correction model in an on-line manner. According to the method, a correction sample set in the process is collected and extracted, the content of the total favone in the sample is detected by using the ultraviolet spectrophotometry, the correction model is established by using TheUnscambler analysis software, and the content of the total favone in the herba epimedii extraction solution in the production process is monitored in real time by using the established correction model. By virtue of the method, the near infrared spectroscopy is successfully used in the production process of traditional Chinese medicine and controlling the quality of the traditional Chinese medicine in the production process in real time in the on-line manner.
Description
Technical field
The present invention relates to field of medicaments, specifically, relate to the detection method of general flavone in a kind of barrenwort production.
Background technology
Barrenwort is Berberidaceae plant, has very high medical value.Taste is returned through acrid, sweet, warm.Return liver, kidney channel to cure mainly function: kidney-replenishing, strengthening the bones and muscles, wines used as antirheumatic.In its extract, mainly contain containing flavone compound, lignanoid, alkaloid, volatilization wet goods.To the evaluation of barrenwort extract, mainly taking the content of general flavone wherein as standard, the content detection of general flavone is calculated and obtains with spectrophotometric method.Need to use high performance liquid chromatography as will be further obtained the wherein content of icariin, this kind of method need to consume a large amount of medicines and reagent, and detection time is longer, and testing result lags behind, can not meet the large production of modernization to ageing requirement, and the demand of line Quality Control.Near-infrared spectrum technique is as a kind of on-line monitoring technique, have quick without harmless feature, be used widely in various fields, this experiment is with acousto-optic turnable filter (Acousto-Optic Tunable Filter, AOTF) near infrared spectrum of barrenwort extract near infrared spectrometer online acquisition extraction process stage pipeline, set up quantitative model prediction, realize near infrared to fast detecting in Chinese medicine Quality Control and ensure the stable of tcm product quality.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide the detection method of general flavone in a kind of barrenwort production, to realize the line Quality Control of general flavone content in barrenwort production run.
To achieve these goals, the present invention adopts following technical scheme:
A detection method for general flavone in barrenwort production, comprises the following steps:
(1) prepare barrenwort extract, sampling;
(2) utilize AOTF near infrared spectrometer to gather the near infrared spectrum corresponding with spectrum;
(3) general flavone content of ultraviolet spectrophotometry offline inspection collected specimens;
(4) utilize the associated near infrared spectrum data of mathematics measuring software and offline inspection data, set up calibration model;
(5) utilize the calibration model of setting up to detect online in production run general flavone content in extract.
In above-mentioned barrenwort is produced in the detection method of general flavone, the preparation of barrenwort extract comprises: barrenwort 25～50kg/ tank is dropped into multifunctional extracting pot, extracting in water 1～3 time, that extracts for the first time adds 10～15 times of volume water gagings, second and third time all adds 10 times of volume water gagings, respectively seethes with excitement 1～2 hour; Extract is thick through 60～100 mesh sieves, is cooled to 40～60 DEG C, and centrifugate merges, for subsequent use.
In above-mentioned barrenwort is produced in the detection method of general flavone, sampling method comprises: extracting the sample valve sampling of installing on the pipeline of tank body, record sample time, sampling plan is that first 40 minutes per minutes are got sample one time, within latter 20 minutes every 5 minutes, get one time sample, every sub-sampling 50mL.
In above-mentioned barrenwort is produced, in the detection method of general flavone, what step (2) collection near infrared spectrum used is the Luminar3060 type near infrared spectrometer of Brimrose company, installs fluid probe additional.Step (2) whole production process gathers spectrum, and spectra collection adopts " Ratio mode " in the mode of perspective, the barrenwort water extraction liquid in pipeline to be carried out to spectra collection by the fibre-optical probe that is connected in fluid sample measuring device.Wavelength coverage 1100～2300; Wavelength increment: 2.0nm, scanning times: 200.Adopt transmission detection mode, light path is 5nm.
In above-mentioned barrenwort is produced, in the detection method of general flavone, the described mathematics measuring software of step (4) is CAMA company's T he Unscrambler analysis software.
In above-mentioned barrenwort is produced, in the detection method of general flavone, step (3) ultraviolet spectrophotometry is that precision measures barrenwort water extraction liquid 0.5mL, puts in 50mL volumetric flask.Add methyl alcohol to scale, shake up, as need testing solution.Separately get icariin reference substance appropriate, accurately weighed, add methyl alcohol and make the solution of every 1mL containing 10 μ g, product solution in contrast.Get respectively need testing solution and reference substance solution, taking corresponding reagent as blank, according to UV-VIS spectrophotometry, measure absorbance at 270nm wavelength place, calculate, to obtain final product.
In above-mentioned barrenwort is produced, in the detection method of general flavone, step (4) spectrum adopts single order differential level and smooth (Savitzy-golay) to carry out pre-service to original spectrum at 9.The detection data of treated spectroscopic data and off-line are associated, adopt partial least square method (PLS1), intersection-proof method (Cross-validation), sets up model with The Uscrambler quantitative analysis software.
Compared with prior art, the present invention has following beneficial effect: the present invention has realized in barrenwort production run the real-time online of general flavone content is detected.Comprise the Calibration gathering in extraction process, adopt ultraviolet spectrophotometry to detect sample general flavone content, utilize The Unscambler analysis software to set up calibration model, use the good calibration model of setting up to barrenwort extract general flavone content Real-Time Monitoring in production run.The present invention successfully applies to near-infrared spectrum technique in Chinese Traditional Medicine, realizes real-time, the online quality control of Chinese Traditional Medicine.
Brief description of the drawings:
Fig. 1 decocts primary light spectrogram for the first time for extracting;
Fig. 2 is for extracting primary light spectrogram for the second time;
Fig. 3 decocts primary light spectrogram for extracting three;
Fig. 4 decocts PLS1 regression model figure for extracting one;
Fig. 5 decocts PLS1 regression model figure for extracting two;
Fig. 6 decocts PLS1 regression model figure for extracting three.
Embodiment:
Embodiment 1:
1, prepare barrenwort extract
Barrenwort 25kg/ tank is dropped into multifunctional extracting pot, extracting in water 3 times, that extracts for the first time adds 15 times of water gagings, and second and third time all adds 10 times of volume water gagings, respectively seethes with excitement 1 hour.Extract is thick through 60～100 mesh sieves, is cooled to 40～60 DEG C, and centrifugate merges, for subsequent use.
2, sampling method
First 40 minutes per minutes of water extraction remove sample one time, within latter 20 minutes every 5 minutes, get one time sample.Every sub-sampling 50mL
3, general flavone detection method
Precision measures barrenwort water extraction liquid 0.5mL, puts in 50mL volumetric flask.Add methyl alcohol to scale, shake up, as need testing solution.Separately get icariin reference substance appropriate, accurately weighed, add methyl alcohol and make the solution of every 1mL containing 10 μ g, product solution in contrast.Get respectively need testing solution and reference substance solution, taking corresponding reagent as blank, according to UV-VIS spectrophotometry, measure absorbance at 270nm wavelength place, calculate, to obtain final product.
4, spectra collection and processing
Spectra collection adopts " Ratio mode " in the mode of perspective, the barrenwort water extraction liquid in pipeline to be carried out to spectra collection by the fibre-optical probe that is connected in fluid sample measuring device.Wavelength coverage 1100～2300; Wavelength increment: 2.0nm scanning times: 200.Adopt transmission detection mode, light path is 5nm,
Spectrum adopts single order differential level and smooth (Savitzy-golay) to carry out pre-service to original spectrum at 9.The detection data of treated spectroscopic data and off-line are associated, adopt partial least square method (PLS1), intersection-proof method (Cross-validation), sets up model with The Uscrambler quantitative analysis software.
5, prediction
These vertical three models of building together, are respectively extraction and decoct for the first time, extract for the second time to decoct, extract for the third time and decoct, and respectively the sample that participates in modeling sample and randomly draw are predicted the outcome as table 1,2,3,4.By internal verification and the external certificate of model, AOTF near infrared spectrum detects the relative deviation of general flavone content in prediction barrenwort production run online in 10% left and right, can effectively realize the quality control of real-time online in actual production process.In the research in later stage, the combined factors such as raw material batch, the place of production feeding intake is considered to modeling, reduce systematic error.Later stage model maintenance need to strengthen data acquisition amount, to enrich model gradient, makes model more plentiful, and gradient is launched, and makes Model suitability better more accurate.Fig. 1 decocts primary light spectrogram for the first time for extracting; Fig. 2 is for extracting primary light spectrogram for the second time; Fig. 3 decocts primary light spectrogram for extracting three; Fig. 4 decocts PLS1 regression model figure for extracting one; Fig. 5 decocts PLS1 regression model figure for extracting two; Fig. 6 decocts PLS1 regression model figure for extracting three.
Table 1 decocts the internal verification result of model for the first time
Table 2 decocts the internal verification result of model for the second time
Table 3 decocts the internal verification result of model for the third time
The external certificate result of table 4 model
Claims (6)
1. a detection method for general flavone in barrenwort production, is characterized in that comprising the following steps:
(1) prepare barrenwort extract, sampling;
(2) utilize AOTF near infrared spectrometer to gather the near infrared spectrum corresponding with spectrum;
(3) general flavone content of ultraviolet spectrophotometry offline inspection collected specimens;
(4) utilize the associated near infrared spectrum data of mathematics measuring software and offline inspection data, set up calibration model;
(5) utilize the calibration model of setting up to detect online in production run general flavone content in extract.
2. the detection method of general flavone in barrenwort production according to claim 1, the preparation that it is characterized in that barrenwort extract comprises: barrenwort 25 ~ 50 kg/ tanks are dropped into multifunctional extracting pot, extracting in water 1 ~ 3 time, that extracts for the first time adds 10 ~ 15 times of volume water gagings, second and third time all adds 10 times of volume water gagings, respectively seethes with excitement 1 ~ 2 hour; Extract is thick through 60～100 mesh sieves, is cooled to 40～60 DEG C, and centrifugate merges, for subsequent use.
3. the detection method of general flavone in barrenwort production according to claim 1, it is characterized in that sampling method comprises: extracting the sample valve sampling of installing on the pipeline of tank body, record sample time, sampling plan is that first 40 minutes per minutes are got sample one time, within latter 20 minutes every 5 minutes, get one time sample, every sub-sampling 50 mL.
4. the detection method of general flavone in barrenwort production according to claim 1, is characterized in that: what step (2) collection near infrared spectrum used is the Luminar3060 type near infrared spectrometer of Brimrose company, installs fluid probe additional.
5. the detection method of general flavone in barrenwort production according to claim 1, is characterized in that: the wavelength coverage 1100～2300 of the spectrum of the described collection of step (2); Wavelength increment: 2.0 nm, scanning times: 200; Adopt transmission detection mode, light path is 5nm.
6. the detection method of general flavone in barrenwort production according to claim 1, is characterized in that, the described mathematics measuring software of step (4) is CAMA company's T he Unscrambler analysis software.
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Cited By (1)
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Application publication date: 20141008 |