CN105181630A - Detection method based on terahertz spectrum technology for hairyvein agrimonia herbs in full-ingredient granules - Google Patents
Detection method based on terahertz spectrum technology for hairyvein agrimonia herbs in full-ingredient granules Download PDFInfo
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Abstract
The invention relates to the field of Chinese herb detection, in particular to a detection method based on a terahertz spectrum technology for hairyvein agrimonia herbs in full-ingredient granules. According to the detection method, the full-ingredient Chinese herb granules are characterized through the broad-band terahertz spectrum technology to obtain fingerprint peaks in a broad band of the full-ingredient Chinese herb granules, and different kinds of the full-ingredient Chinese herb granules are distinguished through the characteristics of the terahertz fingerprint peaks in the broad band. According to the method, the problems of measuring spectral characterization and variety distinguish of the full-ingredient granules are solved; auxiliary of chemical reagents is reduced, and the detection method is purely physical; the method is easy to operate, data processing is fast, and the result is precise.
Description
Technical field
The present invention relates to Chinese crude drug detection field, be specifically related to the detection method of a kind of full ingredient granules agent Chinese herbal medicine hairyvein agrimony based on terahertz light spectral technology.
Background technology
Chinese medical extract is the new product of Chinese traditional herbs in conjunction with modern pharmaceutical technology, set up effectively analyze, identify, discrimination method promotes significant by contributing to the international market of Chinese medical extract for Chinese herbal medicine.At present, the mixture system such as full component extract granule of Chinese medical extract commonly single compound or complexity.Chinese medicine is complicated mixture system, and the advantage of Chinese medicine is " many arm of the services combined operation ", and namely compound is cured the disease, and conventional yin-yang and five elements theory is come back and described the character of Chinese medicine general performance, does not need certain the concrete composition knowing medicine.The natural component of Chinese medicine is very complicated, and perhaps a kind of medicine just has tens kinds of even tens kinds of compositions, and perhaps compound ten several drugses, have hundreds of kind composition.If certain constituents extraction of Chinese medicine out, extract although it take Chinese medicine as raw material, but the compound of single component has been Western medicine in fact, and Western medicine be cannot instruct by the thought theory of the traditional Chinese medical science and diagnose, prescription, treatment, so the specific aim of single component medicine is limited.Therefore, as a kind of Chinese herbal medicine, its drug effect is not from any single active component, its drug action should be that the result of various active composition collaborate is for this problem, full component extract granule mode just can overcome the medical problem that single component extracting method brings, collocation treatment can be carried out by full ingredient granules agent combination, also solve the drawback solving Chinese medicine and be not easy to take simultaneously.So analyze the full ingredient granules after traditional Chinese medicine extraction, differentiate that its structure is extremely important basic work, and dactylogram is the most effective mode of this work.
For various forms of Chinese herbal medicine, dactylogram information is its best recognition feature, and dactylogram refers to the collection of illustrative plates of the feature in order to characterize chemical composition of Chinese materia medica that chemical composition of Chinese materia medica adopts spectrum, chromatogram and other analytical approachs to set up.According to traditional Chinese medicine fingerprint can be used at present Chinese medicine preparation research, production run each stage such as: Chinese crude drug (raw medicinal material) finger-print, Chinese medicine material medicine (comprising medicine materical crude slice, compatibility particle) finger-print and Chinese medicine preparation finger-print, and for the finger-print of art production process intermediate product.
The finger-print of the feature in order to characterize chemical composition of Chinese materia medica that Chemistry for Chinese Traditional Medicine (composition) finger-print usually adopts spectrum, chromatogram and other analytical approachs to set up.That spectrum is the most frequently used is infrared spectrum (IR), and the Sun Suqin of such as Tsing-Hua University utilizes infrared spectrum to obtain the fingerprint peaks of Chinese medicinal material, Chinese medicinal granule, Chinese medicine preparation, traditional Chinese medicine; That chromatogram is the most frequently used is high performance liquid chromatography (HPLC), as the patent " a kind of high-efficiency liquid chromatography method for detecting distinguishing different cultivars yncaria stem with hooks " etc. of Guangdong Pharmaceutical University's application.In the use of these technology, have adding of thinning agent in infrared spectrum technology and bring probabilistic interference and the spectrum more crucially measured only to reflect a kind of intramolecular interaction force situation of medicine, the interaction between multi-medicament molecule in Chinese medicine complex mixture can not be detected; The identification at the extraneous factor meeting interference fingerprint peak such as the diversity selection of solvent and the complexity of operation steps in high-efficient liquid phase chromatogram technology, and its repeatability measured more has much room for improvement.Can see according to above analysis, obtaining the high dactylogram feature of effective quality is the important prerequisite realizing Chinese medicine material identification.In order to address this problem, the present invention carries out from the disposal route of Chinese crude drug and spectrographic detection means two aspects.
On the one hand, experimental subjects is elected as full ingredient granules agent Chinese crude drug by the present invention.This is because facing of traditional decoction progressively shows its " inconvenience " with now decocting application method (volume is large, is inconvenient to carry and preserve; Decoct time-consuming, dose is large; Cannot decoct when travelling and work and take; Traditional Chinese medical science emergency treatment medication is limited) and " uncertainty " of curative effect (About The Quality of Sliced Herbal Medicine affects by factors such as kind, the place of production, collecting season, the processes of preparing Chinese medicine; The decocting method of user and condition cannot be unified; About The Quality of Sliced Herbal Medicine is without unified judgment criteria etc.), limit clinical practice and the Development of Chinese Medicine of traditional Chinese herbal decoction to a certain extent.So Chinese medicinal granule is raw material with the prepared slices of Chinese crude drugs meeting concocted specification, modern production technology " full composition " is utilized to extract, concentrated, dry, the single medicinal material granule of filling a prescription for doctor of granulating.With traditional medicine materical crude slice, there is identical meridian distribution of property and flavor, effect, there is safety, efficient, stable, controlled feature simultaneously, and can add and subtract with disease, embody the feature that differential diagnosis in tcm treats completely.Both maintained the property of medicine, the drug effect of traditional medicine materical crude slice decoction of medicinal ingredients, have again do not need to decoct, directly take after mixing it with water, the advantage such as dose is little, high-efficiency sanitary.On the other hand, Chinese medicine is a mixture system, is completely to rely on collocation between medicine to play drug effect, and the interaction therefore between drug molecule must be embodied.
On the other hand, for the characteristic fingerprint problem of the potpourri of acquisition Chinese medicinal material, Terahertz Technology provides a kind of new effective way.Terahertz wave band plays the attention progressively receiving scientist since eighties of last century the eighties, and is called as last wave band leaved for development on electromagnetic wave spectrum.Terahertz refers to the electromagnetic wave of frequency range at 0.3THz to 10THz, and it has filled up the blank between millimeter wave and infrared waves.Terahertz light spectral technology is the important means obtaining the physical chemistry information of the structure of matter in terahertz wave band, due to THz wave to the vibration of organic molecule and rotation mode and intermolecular interaction responsive, the tera-hertz spectra of material has fingerprint, and terahertz time-domain spectroscopic technology can obtain amplitude and phase information simultaneously, informative, and the tera-hertz spectra of material is the Fingerprint of material, there is unique feature, and Terahertz energy is low can not cause the advantages such as the ionization of biosome, therefore be suitable for very much in Object Classification.Based on above feature, Terahertz Technology is at basic natural sciences such as physics, chemistry, biologies, and the research field such as biomedicine is with a wide range of applications.At present, each research institution has utilized Terahertz Technology to expand preliminary research to Chinese crude drug both at home and abroad, such as University Of Tianjin has applied for " a kind of traditional Chinese medicine sample true and false prescreening method based on terahertz time-domain spectroscopy ", " a kind of system and method for Chinese herbal medicine detection and identification " has been invented by Shanghai University of Science and Technology, " the quick nondestructive analytical approach of the Chinese herbal medicine true and false and quality discrimination " has been invented by Shanghai Inst. of Applied Physics Chinese Academy of Sciences, the people such as Capital Normal University Zhang Zhuoyong give " a kind of THz-TDS of utilization is in conjunction with the method for Chemical Measurement qualification Chinese herbal medicine " and " a kind of THz-TDS that utilizes is in conjunction with the method for fuzzy rule expert system qualification Chinese herbal medicine ".But, the research object of these Terahertzs test is also confined on original unprocessed Chinese crude drug or herbal medicine material, the medicinal material of this form is without purification processes, therefore impurity molecule etc. are very large to the disturbing factor of spectrogram, repeatability and the correlativity of measurement are not high, and within the scope of limited 2.6THz, be difficult to the obvious characteristic fingerprint peak experimentally obtaining Chinese crude drug.
Thus, we utilize wideband terahertz time-domain spectroscopic technology to realize carrying out full ingredient granules agent Chinese crude drug the extraction of spectrographic detection and optical constant.
Summary of the invention
In order to overcome the deficiency of above-mentioned background technology, one has been the object of the present invention is to provide to utilize the full composition Chinese herbal medicine particle of wide-band tera-hertz spectra characterized by techniques, obtain the fingerprint peaks in its wideband spectral coverage, utilize the Terahertz fingerprint peaks feature in wide-band to distinguish different types of full composition Chinese herbal medicine particle.This method solve the spectral characterization of weighing full composition Chinese herbal medicine particle and kind distinguishes problem; Decreasing the auxiliary of chemical reagent, is a kind of detection method of pure physics; The method is simple to operate, and data processing is quick, and result is accurate.
The spectral detection of the full composition Chinese herbal medicine particle based on terahertz light spectral technology of the present invention and characterizing method, have following beneficial effect:
1) the present invention is directed to the full composition Chinese herbal medicine particle after concentration extraction, greatly reduce the spectra1 interfer-impact that the invalid components such as impurity are brought, adopt full composition Chinese herbal medicine particle to avoid the interference brought because medicinal material processing method is different, be conducive in enormous quantities, standardized detection;
2) the terahertz light spectral technology of wide-band can be greater than 3THz scope and obtaining the dactylogram of full composition Chinese herbal medicine particle, Terahertz Technology can ensure to measure the interaction between different Chinese crude drug molecule, and wide frequency technology can ensure that the position obtaining more fingerprint characteristic peak in a frequency range of more widening;
3) detection method of the present invention's employing, eliminate the externality of various chemical reagent in the detection of current medical science, and detection speed is fast, detect accurately, cost is low;
4) the present invention adopts physical detection method, is different from the detection method of other chemistry, and detection method of the present invention has without the need to adding number of chemical reagent, avoids chemical reagent to pollute, and reduces the advantages such as the wasting of resources.
For achieving the above object, the invention provides a kind of spectral detection and characterizing method of the full composition Chinese herbal medicine particle based on terahertz light spectral technology.It comprises the following steps:
(1) a kind of full composition Chinese herbal medicine particle is selected, then grinding, compressing tablet;
(2) tera-hertz spectra of wide range terahertz time-domain spectroscopy measurement device tablet is utilized;
(3) process spectroscopic data, calculate the absorption coefficient of tablet, obtain absorption peak position.
Preferably, the 1. spectral detection based on the full composition Chinese herbal medicine particle of terahertz light spectral technology and characterizing method.It is characterized in that: comprise the following steps:
(1) a kind of full composition Chinese herbal medicine particle is selected, concrete selection hairyvein agrimony particle, grinding, compressing tablet, described full composition hairyvein agrimony particle selects the product sold on the market, electronic balance is utilized to take the sample of quality for 60-100 milligram, with mortar particle porphyrize powdered, powder diameter is not more than 1mm, is then pressed into sheeter the disk that diameter is 10 to 13 millimeters.Then complete disk put into circular specimen holder and fix, as testing sample.
(2) tera-hertz spectra of wide range terahertz time-domain spectroscopy measurement device tablet is utilized, described wide spectrum tera-hertz spectra measurement mechanism is the terahertz time-domain spectroscopy system of transmission-type, test environment is the environment that sample bin is full of nitrogen, air humidity is less than 2%, temperature is at 18 DEG C-25 DEG C, and the spectral range of sample detection is at 0.2THz ~ 5THz.
(3) spectroscopic data is processed, calculate the absorption coefficient of tablet, obtain absorption peak position, spectroscopic data is treated to and utilizes Fourier transform that time-domain spectroscopy is converted into frequency domain spectra, and the data processing model recycled based on fresnel formula obtains the extinction coefficient κ of sample, absorption coefficient and meets following equation along with Terahertz frequency change:
κ＝(c/2πdv)ln(4n/(A(1+n)
2))＝αc/4πv，n＝(cφ/2πdv)+1
In above-mentioned parameter, A represents amplitude, and d is the thickness of sample, and v is frequency, and c is the light velocity in vacuum, and φ is the phase differential between reference signal and sample signal.Absorption peak position refers to the frequency values occurred corresponding to absorption peak.
2., as claimed in claim 1 based on spectral detection and the characterizing method of the full composition Chinese herbal medicine of terahertz light spectral technology, the wide spectrum source in described step (2) produces and detection system is produced and air detection System's composition by air.Measurement in described step (2) uses wide spectrum source to produce terahertz pulse wavelength-division not through empty specimen holder when not filling sample and the specimen holder that sample is housed, and obtain the terahertz pulse time domain spectroscopic signal of transmissive respectively, namely with reference to time-domain signal and sample time domain signal.A coordinate axis of the terahertz light modal data display collection of illustrative plates form obtained is the time, and another coordinate axis is the time domain data point of intensity.
The terahertz time-domain spectroscopy system that the method utilizing terahertz time-domain spectroscopy to detect tablet provided by the present invention adopts, it comprises titanium sapphire femto-second laser and amplifier system 1, and (centre wavelength is 800nm (nanometer), repetition frequency is 1KHz (KHz), pulse width is 35fs (femtosecond), energy is the LASER Light Source of 1.5mJ), the 800nm light source exported arrives beam splitter 3 through catoptron 2, after part light is irradiated to bbo crystal 4 and half-wave plate 5 as pump light, focused on by parabolic lens 6 again and form air plasma, thus generation terahertz emission, then terahertz emission and 800nm pump light penetrate through parabolic lens 8 reflected parallel and arrive parabolic lens 9, following beam splitting chip 20 blocks 800nm pump light, terahertz emission can arrive sample 10 through beam splitting chip 20, subsequently terahertz emission and the sample flashlight that is excited out together polished object mirror 11 reflex to parabolic lens 12, simultaneously, another part detecting light beam that beam splitter 3 separates arrives catoptron 16 successively after the time delay system that catoptron 13,14,15 forms, then focus on after through parabolic lens 12 through lens 17 and assemble with terahertz light, sample signal light simultaneously, eventually pass filter plate and enter the collection that photomultiplier carries out signal.
Accompanying drawing explanation
Fig. 1 is transmission-type terahertz time-domain spectroscopy index path.
Fig. 2 is the measurement result figure of the terahertz wave band of hairyvein agrimony.
Embodiment
In order to there be understanding clearly to technical scheme of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
The present embodiment provides a kind of method utilizing terahertz time-domain spectroscopic technology to detect hairyvein agrimony, and it comprises the following steps:
1), preparation of samples: sample used is the full composition Chinese medicine hairyvein agrimony particle that Beijing Kangrentang Medicine Co., Ltd produces, the hairyvein agrimony particle of about 60 milligrams is taken with electronic balance, then in mortar, fine powdered is ground to form, next shape in sheeter, pressure is added to 5 tons, 8 minutes time, will obtain the disk that diameter is 13 millimeters like this, two sides is smooth, and thickness is below 0.4 millimeter.
2), sample test: open laser instrument until after stable output power, the collimate light situation in calibration light path; Open notebook computer, arrange the measurement parameter on tera-hertz spectra system software program panel, laser preheating was measured after one hour; Ready empty specimen holder is put into the sample bin position in light path; Start inflated with nitrogen subsequently until storehouse humidity is reduced to less than 1%, gather the Terahertz transmission time-domain spectroscopy of empty specimen holder; With the terahertz time-domain waveform of empty specimen holder for reference signal.Next, put the tablet suppressed in empty specimen holder and put into again on the position of sample bin, rush nitrogen, repeat to adopt above method can obtain the Terahertz transmission time-domain spectroscopy data of traditional Chinese medicine sample, using this terahertz time-domain waveform as sample signal.For improving accuracy and degree of accuracy, often kind of sample duplicate measurements at least three times, averages as final reference signal and sample signal.
3), data processing: signal transacting: the time domain waveform of Reference Signal and sample signal carries out Fast Fourier Transform (FFT), then utilizes the data processing model based on Fresnel principle to calculate the absorption coefficient (v) of Chinese crude drug hairyvein agrimony at effective terahertz wave band:
κ＝(c/2πdv)ln(4n/(A(1+n)
2))＝αc/4πv
Wherein, φ is the phase differential between sample electric field (electric field of tablet samples) and reference electric field (empty specimen holder electric field), and d is thickness of sample, and v is the frequency of radiation, and c is the light velocity of vacuum.
Wherein, what effective terahertz wave band frequency range obtained after terahertz time-domain system can be utilized to carry out Scanning Detction to sample comprise the time, the multi-group data of oscillator intensity calculates.
4), spectrum analysis: can see from the wide absorption spectrogram (Fig. 2) of hairyvein agrimony particle medicinal material, owing to being greater than within the scope of 3THz wide-band, therefore can obtain and have more effective absorption peak position than the terahertz time-domain spectroscopy systematic survey of routine, these absorption peaks derive between medicinal material interior molecules or intramolecular various interaction force.
In sum, these are only preferred embodiment of the present invention, be not intended to limit protection scope of the present invention.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1., based on a spectral method of detection for the full composition Chinese herbal medicine particle of terahertz light spectral technology, it is characterized in that comprising the following steps:
(1) choose full composition Chinese herbal medicine hairyvein agrimony particle, then ground, compressing tablet;
(2) tera-hertz spectra of wide range terahertz time-domain spectroscopy measurement device tablet is utilized;
(3) process spectroscopic data, calculate the absorption coefficient of tablet, obtain absorption peak position.
2., as claimed in claim 1 based on the spectral method of detection of the full composition Chinese herbal medicine of terahertz light spectral technology, it is characterized in that:
Step (1) is for choosing Chinese herbal medicine hairyvein agrimony particle, then grinding, compressing tablet, electronic balance is utilized to take the sample of quality for 60-100 milligram, with mortar particle porphyrize powdered, powder diameter is not more than 0,1mm, is then pressed into sheeter the disk that diameter is 10 to 13 millimeters, then complete disk put into circular specimen holder and fix, as testing sample;
Step (2) is for utilizing the tera-hertz spectra of wide range terahertz time-domain spectroscopy measurement device tablet, described wide spectrum tera-hertz spectra measurement mechanism is the terahertz time-domain spectroscopy system of transmission-type, test environment is the environment that sample bin is full of nitrogen, air humidity is less than 2%, temperature is at 18 DEG C-25 DEG C, and the spectral range of sample detection is at 0.2THz ~ 5THz.
Step (3) is process spectroscopic data, calculate the absorption coefficient of tablet, obtain absorption peak position, spectroscopic data is treated to and utilizes Fourier transform that time-domain spectroscopy is converted into frequency domain spectra, and the data processing model recycled based on fresnel formula obtains the extinction coefficient κ of sample, absorption coefficient and meets following equation along with Terahertz frequency change:
κ＝(c/2πdv)ln(4n/(A(1+n)
2))＝αc/4πv.n＝(cφ/2πdv)+1
In above-mentioned parameter, A represents amplitude, and d is the thickness of sample, and v is frequency, and c is the light velocity in vacuum, and φ is the phase differential between reference signal and sample signal, and absorption peak position refers to the frequency values occurred corresponding to absorption peak.
3. as claimed in claim 2 based on the spectral method of detection of the full composition Chinese herbal medicine of terahertz light spectral technology, wide spectrum source in described step (2) produces and detection system is constructed as follows: (centre wavelength is 800nm (nanometer) for titanium sapphire femto-second laser and amplifier system 1, repetition frequency is 1KHz (KHz), pulse width is 35fs (femtosecond), energy is the LASER Light Source of 1.5mJ), the 800nm light source exported arrives beam splitter 3 through catoptron 2, after part light is irradiated to bbo crystal 4 and half-wave plate 5 as pump light, focused on by parabolic lens 6 again and form air plasma, thus generation terahertz emission, then terahertz emission and 800nm pump light penetrate through parabolic lens 8 reflected parallel and arrive parabolic lens 9, following beam splitting chip 20 blocks 800nm pump light, terahertz emission can arrive sample 10 through beam splitting chip 20, subsequently terahertz emission and the sample flashlight that is excited out together polished object mirror 11 reflex to parabolic lens 12, simultaneously, another part detecting light beam that beam splitter 3 separates arrives catoptron 16 successively after the time delay system that catoptron 13,14,15 forms, then focus on after through parabolic lens 12 through lens 17 and assemble with terahertz light, sample signal light simultaneously, eventually pass filter plate and enter the collection that photomultiplier carries out signal.
4. as claimed in claim 2 based on the spectral method of detection of the full composition Chinese herbal medicine of terahertz light spectral technology, it is characterized in that: the measurement in described step (2) uses wide spectrum source to produce terahertz pulse wavelength-division not through empty specimen holder when not filling sample and the specimen holder that sample is housed, and obtain the terahertz pulse time domain spectroscopic signal of transmissive respectively, namely with reference to time-domain signal and sample time domain signal.
5. as claimed in claim 2 based on the spectral method of detection of the full composition Chinese herbal medicine of terahertz light spectral technology, it is characterized in that: a coordinate axis of the terahertz light modal data display collection of illustrative plates form that described step (2) obtains is the time, and another coordinate axis is the time domain data point of intensity.
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| CN1614391A (en) * | 2003-11-03 | 2005-05-11 | 中国科学院上海应用物理研究所 | Rapid non-loss analyzing method for Chinese Medicinal herb quality discrimination |
| CN102621083A (en) * | 2012-03-08 | 2012-08-01 | 中国石油大学(北京) | Method and system for measuring rock optical parameters based on Terahertz time-domain spectroscopy |
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