AU2021102210A4 - Method for detecting all-ingredient chinese herbal medicine caulis bambusae granules based on terahertz spectroscopy - Google Patents
Method for detecting all-ingredient chinese herbal medicine caulis bambusae granules based on terahertz spectroscopy Download PDFInfo
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
- G01N21/3586—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation by Terahertz time domain spectroscopy [THz-TDS]
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Abstract
The present invention relates to the field of detection of traditional Chinese
medicinal materials, and particularly relates to a method for detecting
all-ingredient Chinese herbal medicine Caulis bambusae granules based on
terahertz spectroscopy. A purpose of the present invention is to provide a method
for characterizing all-ingredient Chinese herbal medicine granules by utilizing
wide-band terahertz spectroscopy to obtain fingerprint peaks in a wide frequency
spectrum and distinguishing different types of the all-ingredient Chinese herbal
medicine granules by utilizing the characteristics of terahertz fingerprint peaks in
the wide band. The method solves the problem that spectroscopic characterization
and type distinguishing of the all-ingredient Chinese herbal medicine granules
cannot be measured, decreases assistance of chemical reagents and is a purely
physical detection method. The method is simple in operation, rapid in data
processing and accurate in result.
Drawings of Description
214 oP%15
FI.
13
4 8 12
5 17
6 16 1
720 18
FIG. 1
3
2
0
1 2 345
Frequency (THz)
FIG. 2
1
Description
Drawings of Description
214 oP%15
13
4 8 12 5 17 6 16 1 FI. 720 18
FIG. 1
3
2
1 2 345
Frequency (THz)
FIG. 2
Description
Technical Field
The present invention relates to the field of detection of traditional Chinese medicinal materials, and particularly relates to a method for detecting all-ingredient Chinese herbal medicine Caulis bambusae granules based on terahertzspectroscopy.
Background
Traditional Chinese medicine extract is a novel product produced in combination with traditional Chinese herbal medicines and modem pharmaceutical technologies. Establishing an effective analysis, recognition and identification method has important significances for international market promotion of Chinese herbal medicines by the traditional Chinese medicine extract. At present, a common form of the traditional Chinese medicine extract is a single compound or a complex mixture system, such as all-ingredient extract granules. Traditional Chinese medicine is a complex mixture system, and has an advantage of "combination of multiple ingredients", that is, diseases are treated with multiple compounds. The overall performance of the traditional Chinese medicine is described by a common theory of yin-yang and five elements, and certain specific components of the medicine do not need to be known. Natural ingredients of the traditional Chinese medicine are complex; one medicine may include more than ten or even dozens of ingredients; and a compound medicine is prepared from more than ten medicines and may include hundreds of types of ingredients. If a certain ingredient of the traditional Chinese medicine is extracted, although the ingredient is extracted by taking the traditional Chinese medicine as a raw material,
Description
the compound of a single ingredient is already a Western medicine, while the Western medicine cannot be used for guidance, diagnosis, composition and treatment by using thoughts and theories of the traditional Chinese medicine. Thus, the single-ingredient medicine has limited targeted property. Therefore, as a Chinese herbal medicine, a pharmaceutical effect of the single-ingredient medicine is not from any single active ingredient; and pharmacodynamic effects shall be cooperative results of multiple active ingredients. With respect to such a problem, medical problems brought by a single-ingredient extraction method can be solved by an all-ingredient extract granule manner. Matched treatment may be conducted by an all-ingredient granule combination; and the defect that the traditional Chinese medicine is inconvenient to take is overcome. Therefore, analyzing the all-ingredient granules extracted from the traditional Chinese medicine and identifying structures of the all-ingredient granules are extremely important basic jobs, while a fingerprint spectrum is the most effective manner of the jobs. For Chinese herbal medicines in various forms, fingerprint spectrum information is the best recognition feature. The fingerprint spectrum is a map of chemical ingredients of the traditional Chinese medicine that is established by spectrums, chromatography and other analysis methods and used for characterizing the features of the chemical ingredients of the traditional Chinese medicine. At present, traditional Chinese medicine fingerprint spectrums have been already applied to study of traditional Chinese medicine preparations and various stages of production processes, such as a traditional Chinese medicinal material (raw medicinal material) fingerprint spectrum, a traditional Chinese medicine raw material (including decoction piece and compatibility particle) fingerprint spectrum, a traditional Chinese medicine preparation fingerprint spectrum, and an intermediate product fingerprint spectrum used in the technical production process. A traditional Chinese medicine chemistry (ingredient) fingerprint spectrum is a fingerprint spectrum that is often established by the spectrums, chromatography
Description
and other analysis methods and used for characterizing the features of the chemical ingredients of the traditional Chinese medicine. The most commonly used spectrum is an infrared spectrum (IR). For example, fingerprint peaks of traditional Chinese medicinal materials, traditional Chinese medicine granules in prescriptions, traditional Chinese medicine preparations and traditional Chinese medicine injection are obtained by Suqin Sun in Tsinghua University by utilizing the IR. The most commonly used chromatography is high performance liquid chromatography (HPLC), e.g., a patent "HPLC Detection Method for Distinguishing Different Types of UncariaRhynchophylla" applied by Guangdong Pharmaceutical University. In use of these technologies, uncertain interference may be brought by addition of a diluent in the IR technology, and more critically, the measured spectrum only reflects interaction force in molecules of the medicine, and thus interactions among multiple medicine molecules in the complex traditional Chinese medicine mixture cannot be detected. Recognition of the fingerprint peaks may be interfered by external factors such as diversified options of solvents and complicated operating steps in the HPLC technology; and repeatability of measurement needs to be improved. According to the above analysis, it can be seen that, acquiring effective high-quality fingerprint spectrum features is an important precondition of recognizing the traditional Chinese medicine materials. To solve the problem, the present invention is described from two aspects, that is, treatment methods of traditional Chinese medicinal materials and spectrum detection means. On one hand, experimental objects are selected from all-ingredient traditional Chinese medicinal material granules in the present invention because an immediately decocting medication manner of traditional decoction has already gradually shown "inconvenience" (the decoction is large in volume and inconvenient to carry and preserve, is time-consuming to decoct and large in dose, and cannot be decocted to take during travel and work; and emergency use of
Description
traditional Chinese medicine is limited) and "uncertainty" of curative effects (quality of traditional Chinese medicine decoction pieces is affected by factors such as variety, place of production, harvesting seasons and preparation; decocting methods and conditions of patients cannot be unified; and the quality of the traditional Chinese medicine decoction pieces has no uniform evaluation criteria), thereby limiting clinical applications of the traditional Chinese medicine decoctions and the development of the traditional Chinese medicine to a certain degree. Then, traditional Chinese medicine formula granules are single-ingredient traditional Chinese medicine granules for doctor formulation prepared by taking traditional Chinese Medicine decoction pieces that conform to preparation standards as raw materials by utilizing modem production processes such as "all-ingredient" extraction, concentration, drying and granulation. The traditional Chinese medicine formula granules have the same tropism of taste, effects and major functions as the traditional decoction pieces, have the characteristics of safety, efficiency, stability and controllability, can be increased or decreased according to symptoms, and completely reflect the dialectical therapy characteristics of the traditional Chinese medicine. The traditional Chinese medicine formula granules maintain medicinal properties and medicinal effects of the traditional decoction pieces and decoctions and have the advantages of no decocting need, direct administration after dissolving, small dose, high efficiency and sanitation. Further, the traditional Chinese medicine is a mixture system, and medicinal effects are achieved by completely matching various medicines. Therefore, the interactions among the medicine molecules must be reflected. On the other hand, with respect to the problem that characteristic fingerprints of a mixture of the traditional Chinese medicinal materials cannot be obtained, the terahertz technology provides a new effective way. Since the 1980s, the terahertz band has gradually received attention from scientists, and was called the last to-be-developed band in an electromagnetic spectrum. Terahertz refers to an
Description
electromagnetic wave in a frequency range of 0.3-10 THz, and fills a gap between millimeter waves and infrared waves. Terahertz spectroscopy is an important means of acquiring physicochemical information of a material structure in the terahertz band. Since the terahertz wave is sensitive to vibration and rotation modes of organic molecules and intermolecular interactions, the terahertz spectrum of the material has fingerprint property. Moreover, amplitude and phase information may be simultaneously obtained by terahertz time-domain spectroscopy, and the information is rich. Further, the terahertz spectrum of the material is a fingerprint spectrum of the material, has the unique feature, and has the advantage that ionization of organisms is not caused due to low terahertz energy. Therefore, the terahertz technology is very suitable for material recognition. Based on the above characteristics, the terahertz technology has wide application prospects in the research fields of basic natural sciences such as physics, chemistry and biology, as well as biomedicine. At present, preliminary study has been conducted on the traditional Chinese medicinal materials by various research institutions in China and abroad by utilizing the terahertz technology. For example, "Method for Preliminarily Screening of Authenticity of Traditional Chinese Medicine Samples based on Terahertz Time-domain Spectroscopy" was applied by Tianjin University; "System and Method for Detecting and Identifying Chinese Herbal Medicines" was invented by University of Shanghai for Science and Technology; "Rapid Nondestructive Analysis Method for Identifying Authenticity and Quality of Chinese Herbal Medicines" was invented by Shanghai Research Institute of Applied Physics in Chinese Academy of Sciences; and "Method for Identifying Chinese Herbal Medicines in Combination with THz-TDS and Chemometrics" and "Method for Identifying Chinese Herbal Medicines in Combination with THz-TDS and Fuzzy Rule Expert System" were provided by Zhuoyong Zhang, et al. in Capital Normal University. However, research objects in these terahertz tests are still limited to original untreated traditional Chinese
Description
medicinal materials or Chinese medicinal herbs; and the medicinal materials in this form are not purified. Therefore, impurity molecules and the like have greater interference to the spectrum chart; measurement repeatability and correlation are low; and obvious characteristic fingerprint peaks of the traditional Chinese medicinal materials are difficult to be obtained from experiments in a limited range of 2.6 THz. Thus, the all-ingredient traditional Chinese medicinal material granules are subjected to spectrum detection and optical constant reading by utilizing the wide-band terahertz time-domain spectroscopy.
Summary To overcome the defects in the above background, a purpose of the present invention is to provide a method for characterizing all-ingredient Chinese herbal medicine granules by utilizing wide-band terahertz spectroscopy to obtain fingerprint peaks in a wide frequency spectrum and distinguishing different types of the all-ingredient Chinese herbal medicine granules by utilizing the characteristics of terahertz fingerprint peaks in the wide band. The method solves the problem that spectroscopic characterization and type distinguishing of the all-ingredient Chinese herbal medicine granules cannot be measured, decreases assistance of chemical reagents and is a purely physical detection method. The method is simple in operation, rapid in data processing and accurate in result The spectrum detection and characterization method for the all-ingredient Chinese herbal medicine granules based on the terahertz spectroscopy in the present invention has beneficial effects as follows: 1) In the present invention, with respect to the concentrated and extracted all-ingredient Chinese herbal medicine granules, spectral interference effects brought by impurities and other inactive ingredients are greatly decreased; and interference brought by differences of medicinal material preparation methods is
Description
avoided by the all-ingredient Chinese herbal medicine granules, thereby facilitating large-scale standardized detection. 2) The fingerprint spectrums of the all-ingredient Chinese herbal medicine granules can be obtained in a range greater than 3 THz by the wide-band terahertz spectroscopy; the interactions among the molecules of different traditional Chinese medicinal materials can be measured by the terahertz technology; and by virtue of the terahertz technology, more fingerprint feature peak positions can be obtained in a wider frequency range. 3) The detection method in the present invention avoids external influences of the various chemical reagents in the current medical detection, and is high in detection speed, accurate in detection and low in cost. 4) The physical detection method adopted in the present invention is different from other chemical detection methods. The detection method in the present invention has the advantages that multiple chemical reagents do not need to be added, contamination of the chemical reagents is avoided and waste of resources is decreased. To achieve the above purpose, the present invention provides the spectrum detection and characterization method for the all-ingredient Chinese herbal medicine granules based on the terahertz spectroscopy. The method includes the following steps: (1) selecting a kind of all-ingredient Chinese herbal medicine granules; and then grinding and tabletting the granules; (2) measuring a terahertz spectrum of the tablets by utilizing a wide-band terahertz time-domain spectroscopy device; (3) processing spectroscopic data; and calculating an absorption coefficient of the tablets to obtain the locations of absorption peaks.
Description
As a preferred embodiment, 1, the spectrum detection and characterization method for the all-ingredient Chinese herbal medicine granules based on the terahertz spectroscopy includes the following steps: (1) selecting a kind of all-ingredient Chinese herbal medicine granules; selecting Caulis bambusae granules; grinding and tabletting the granules, wherein the all-ingredient Caulis bambusae granules are selected from commercially available products; weighing samples having the mass of 60-100 mg by an electronic scale; grinding the granules into powder having a particle size not more than 1 mm by a mortar; tabletting the powder into wafers having a diameter of -13 mm by a tablet press; and putting the complete wafers into a circular sample holder and fixing the wafers as to-be-detected samples; (2) measuring a terahertz spectrum of the tablets by utilizing the wide-band terahertz time-domain spectroscopy device, wherein the wide-band terahertz time-domain spectroscopy device is a transmission type terahertz time-domain spectroscopy system; the test environment is a sample storehouse environment filled with nitrogen; air humidity is less than 2%; the temperature is 18-25°C; and a frequency spectrum range of sample detection is 0.2-5 THz; (3) processing spectroscopic data; and calculating an absorption coefficient of the tablets to obtain the locations of absorption peaks, wherein the operation of processing the spectroscopic data is as follows: a time-domain spectrum is converted into a frequency-domain spectrum by utilizing Fourier transform; and an extinction coefficientKand an absorption coefficient a of the samples are obtained by utilizing a data processing model based on Fresnel's Formula, and meet the following equation along the terahertz frequency change: x = (c/2jr-dv)ln(4n/(A(1+n)')) = ac/4 xv,n= (cc4p/2xdv)+1
In the above parameters, A represents the amplitude; d is a thickness of the samples; v is the frequency; c is light velocity in vacuum; and <D is a phase
Description
difference between a reference signal and a sample signal. The locations of the absorption peaks refer to frequency values corresponding to the absorption peaks. 2. In the spectrum detection and characterization method for the all-ingredient Chinese herbal medicine granules based on the terahertz spectroscopy of claim 1, a wide frequency spectrum source generation and detection system in the step (2) is composed of an air generation system and an air detection system. The measurement in the step (2) includes: generating terahertz pulse waves by a wide frequency spectrum source; enabling the terahertz pulse waves to respectively transmit an empty sample holder without samples and a sample holder filled with samples; and respectively acquiring transmitted terahertz pulse time-domain wave spectrum signals, i.e., a reference time-domain signal and a sample time-domain signal. The acquired terahertz spectroscopic data shows that, one coordinate axis of a map format is time; and the other coordinate axis is time-domain data points of the strength. The method for detecting tablets by utilizing the terahertz time-domain spectrum provided by the present invention adopts a terahertz time-domain spectrum system which includes a titanium sapphire femtosecond laser and an amplifier system 1 (a laser light source having a central wavelength of 800 nm (nanometers), a repetition frequency of 1 KHz (kilohertz), a pulse width of 35 fs (femtoseconds) and energy of 1.5 mJ. The outputted 800 nm light source reaches a beam splitter 3 via a reflector 2. One part of light serving as pump light irradiates a BBO crystal 4 and a half-wave plate 5, and is focused by a parabolic reflector 6 to form air plasma so as to produce terahertz radiation. Next, the terahertz radiation and the 800 nm pump light are reflected by a parabolic reflector 8 and then emitted in parallel to reach a parabolic reflector 9; then, the 800 nm pump light is blocked by a beam splitter 20; the terahertz radiation can reach a sample 10 via the beam splitter 20; and then the terahertz radiation and signal light excited by the sample are reflected to a parabolic reflector 12 by a parabolic reflector 11 together.
Description
Meanwhile, the other part of detected beams split by the beam splitter 3 passes through a time delay system composed of reflectors 13, 14 and 15 in sequence to reach the reflector 16, are focused via a lens 17 to pass through the parabolic reflector 12, then converge with the terahertz light and sample signal light, and finally enter a photomultiplier via a filter so as to perform signal acquisition.
Description of Drawings
Fig. 1 is an optical path diagram of a transmission type terahertz time-domain spectrum; and Fig. 2 is a measurement result diagram of terahertz bands of Caulis bambusae.
Detailed Description
To more clearly understand technical solutions, purposes and beneficial effects of the present invention, the technical solutions of the present invention are described below in detail. However, the technical solutions shall not be understood as a limitation to an implementable scope of the present invention. Embodiment 1 The present embodiment provides a method for detecting Caulis bambusae by utilizing terahertz time-domain spectroscopy. The method includes the following steps: 1) Sample preparation: the used samples are all-ingredient traditional Chinese medicine Caulis bambusae granules produced by Beijing Kangrentang Pharmaceutical Co., Ltd. About 60 mg of Caulis bambusae granules were weighed by an electronic scale; the granules were ground into fine powder in a mortar; then the fine powder was shaped in a table press under a pressure of 5 tons for 8 minutes to obtain wafers having a diameter of 13 mm, wherein two sides of the wafers were smooth, and a thickness of the wafers was less than 0.4 mm.
Description
2) Sample test: a laser was turned on until output power was stable; light collimation conditions in an optical path were calibrated; a laptop was started to set the measuring parameters on a program panel of terahertz spectrum system software; measurement was conducted within an hour after laser preheating; a prepared empty sample holder was put at a sample storehouse position in the optical path; then nitrogen was filled until humidity in the storehouse was decreased to be less than 1%; a terahertz transmission time-domain spectrum of the empty sample holder was acquired; and a terahertz time-domain waveform of the empty sample holder was used as a reference signal. Then, the pressed tablets were put into the empty sample holder and then put at the position of the sample storehouse; the nitrogen is filled; and the above methods were repeated to obtain the terahertz transmission time-domain spectrum data of the traditional Chinese medicine sample. The terahertz time-domain waveform was used as the sample signal. To increase accuracy and precision, each sample shall be repeatedly measured for at least three times; and the mean value was used as the final reference signal and sample signal. 3) Data processing: signal processing: the time-domain waveforms of the reference signal and the sample signal were subjected to fast Fourier transform; and then an absorption coefficient a(v) of the traditional Chinese medicinal material, that is, Caulis bambusae, at an effective terahertz band was calculated by utilizing a data processing model based on Fresnel's Formula: K = (c/2Txdv)in(4n/(A(1+n))) = ac/4 v In the above parameters, <D is a phase difference between a sample electric field (an electric field of tablet samples) and a reference electric field (an electric field of the empty sample holder); d is a thickness of the sample; v is a radiation frequency; and c is light velocity in vacuum.
Description
A frequency range of the effective terahertz band may be calculated from multiple groups of data including the time and amplitude intensity obtained after scanning and detecting the samples by utilizing the terahertz time-domain system. 4) Spectrum analysis: it can be seen from a wide-absorption spectrogram (Fig. 2) of the Caulis bambusae medicinal granules that, because of the wide-band range more than 3 THz, locations of more effective absorption peaks can be obtained compared with those measured by the conventional terahertz time-domain spectrum system. These absorption peaks come from various intermolecular or intramolecular interactions inside the medicinal materials. To sum up, the above only describes preferred embodiments of the present invention, rather than limits the protection scope of the present invention. Any modification, equivalent replacement and improvement made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.
Claims (5)
1. A spectrum detection method for all-ingredient Chinese herbal medicine granules based on terahertz spectroscopy, comprising the following steps: (1) selecting all-ingredient Chinese herbal medicine Caulis bambusae granules; and then grinding and tabletting the granules; (2) measuring a terahertz spectrum of the tablets by utilizing a wide-band terahertz time-domain spectroscopy device; (3) processing spectroscopic data; and calculating an absorption coefficient of the tablets to obtain the locations of absorption peaks.
2. The spectrum detection method for all-ingredient Chinese herbal medicine granules based on terahertz spectroscopy according to claim 1, comprising: step (1): selecting Chinese herbal medicine Caulis bambusae granules; then grinding and tabletting the granules; weighing samples having the mass of 60-100 mg by an electronic scale; grinding the granules into powder having a particle size not more than 0.1 mm by a mortar; tabletting the powder into wafers having a diameter of 10-13 mm by a tablet press; and putting the complete wafers into a circular sample holder and fixing the wafers as to-be-detected samples; step (2): measuring a terahertz spectrum of the tablets by utilizing the wide-band terahertz time-domain spectroscopy device, wherein the wide-band terahertz time-domain spectroscopy device is a transmission type terahertz time-domain spectroscopy system; the test environment is a sample storehouse environment filled with nitrogen; air humidity is less than 2%; the temperature is 18-25°C; and a frequency spectrum range of sample detection is 0.2-5 THz; step (3): processing spectroscopic data; and calculating an absorption coefficient of the tablets to obtain the locations of absorption peaks, wherein the operation of processing the spectroscopic data is as follows: a time-domain spectrum is converted into a frequency-domain spectrum by utilizing Fourier transform; and an extinction coefficient Kand an absorption coefficient a of the
Claims
samples are obtained by utilizing a data processing model based on Fresnel's Formula, and meet the following equation along the terahertz frequency change: Y = (c/2 " dv) in (4n/(A (1+n)2)) = a c/4 v, n = (c+ /2 m dv)+1
in the above parameters, A represents the amplitude; d is a thickness of the samples; v is the frequency; c is light velocity in vacuum; <D is a phase difference between a reference signal and a sample signal; and the locations of the absorption peaks refer to frequency values corresponding to the absorption peaks.
3. The spectrum detection method for all-ingredient Chinese herbal medicine granules based on terahertz spectroscopy according to claim 2, wherein a wide frequency spectrum source generation and detection system in the step (2) is composed of a titanium sapphire femtosecond laser and an amplifier system 1 (a laser light source having a central wavelength of 800 nm (nanometers), a repetition frequency of 1 KHz (kilohertz), a pulse width of 35 fs (femtoseconds) and energy of 1.5 mJ; the outputted 800 nm light source reaches a beam splitter 3 via a reflector 2; one part of light serving as pump light irradiates a BBO crystal 4 and a half-wave plate 5, and is focused by a parabolic reflector 6 to form air plasma so as to produce terahertz radiation; next, the terahertz radiation and the 800 nm pump light are reflected by a parabolic reflector 8 and then emitted in parallel to reach a parabolic reflector 9; then, the 800 nm pump light is blocked by a beam splitter 20; the terahertz radiation can reach a sample 10 via the beam splitter 20; and then the terahertz radiation and signal light excited by the sample are reflected to a parabolic reflector 12 by a parabolic reflector 11 together; meanwhile, the other part of detected beams split by the beam splitter 3 passes through a time delay system composed of reflectors 13, 14 and 15 in sequence to reach the reflector 16, are focused via a lens 17 to pass through the parabolic reflector 12, then converge with the terahertz light and sample signal light, and finally enter a photomultiplier via a filter so as to perform signal acquisition.
Claims
4. The spectrum detection method for all-ingredient Chinese herbal medicine granules based on terahertz spectroscopy according to claim 2, wherein the measurement in the step (2) comprises: generating terahertz pulse waves by a wide frequency spectrum source; enabling the terahertz pulse waves to respectively transmit an empty sample holder without samples and a sample holder filled with samples; and respectively acquiring transmitted terahertz pulse time-domain wave spectrum signals, i.e., a reference time-domain signal and a sample time-domain signal.
5. The spectrum detection method for all-ingredient Chinese herbal medicine granules based on terahertz spectroscopy according to claim 2, wherein the terahertz spectroscopic data acquired in the step (2) shows that one coordinate axis of a map format is time; and the other coordinate axis is time-domain data points of the strength.
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