CN110346306A - A kind of rapid detection method of Resina Draconis crude drug quality - Google Patents
A kind of rapid detection method of Resina Draconis crude drug quality Download PDFInfo
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- CN110346306A CN110346306A CN201910690217.2A CN201910690217A CN110346306A CN 110346306 A CN110346306 A CN 110346306A CN 201910690217 A CN201910690217 A CN 201910690217A CN 110346306 A CN110346306 A CN 110346306A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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Abstract
The invention discloses a kind of rapid detection methods of Resina Draconis crude drug quality, including following detecting step: collecting the dragon tree medicinal material in different sources source, select 10 batches of samples to collect sample as verifying, remaining is as calibration set sample；The near infrared spectrum of verifying collection sample and calibration set sample is acquired using near-infrared diffusing reflection spectrum；Measure every batch of sample total polyphenols and moisture content；Near-Infrared Quantitative Analysis model is established using Partial Least Squares；Verify the stability and precision of prediction of model built.The invention has the benefit that utilizing near-infrared spectrum technique and partial least-square regression method, establish the Quantitative Analysis Model between Resina Draconis crude drug-dragon tree medicinal material near infrared spectrum and its effective component total polyphenols and moisture content, compared with traditional detection method, with the advantages such as quick, lossless, the quick detection of raw material is realized, to realize the quality for controlling Resina Draconis product from source.
Description
Technical field
The present invention relates to traditional Chinese medicine quality detection technique field, in particular to a kind of quick detections of Resina Draconis crude drug quality
Method.
Background technique
Resina Draconis has the function of promoting blood circulation to remove blood stasis, analgesic therapy hemostasis and expelling pus and promoting granulation, for coronary heart disease, local trauma go out
The hemorrhagic diseases such as blood, hemostasis, gynaecology's palace blood, upper gastrointestinal bleeding, hemorrhoid and nosebleed have good curative effect.Used in Resina Draconis
Crude drug is the material containing tallow wood and bark of liliaceous plant swordleaf dragon tree.Crude drug inspection is procedure quality analysis and control
Source, due to the factors difference such as planting conditions, growing environment, the content and kind of the same class medicinal materials of different sources in active constituent
It often differs greatly in class, therefore it is very necessary to carry out quality evaluation to crude drug.At present still not to raw medicine used in Resina Draconis
The effective means that material-dragon tree medicinal material quality is used for quickly detecting.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the above technological deficiency, a kind of the fast of Resina Draconis crude drug quality is provided
Fast detection method realizes Determination of Polyphenols and moisture in Resina Draconis crude drug-dragon tree medicinal material using NIR technology
Quickly detection, realizes the Fast Evaluation of quality.
In order to achieve the above object of the invention, the technical solution adopted by the present invention are as follows: a kind of Resina Draconis crude drug quality it is fast
Fast detection method, including following detecting step:
(1) the dragon tree medicinal material for collecting different sources source is no less than 50 batches, randomly chooses 10 batches of samples as verifying collection
Sample, remaining sample carry out the foundation of quantitative calibration models as calibration set sample；
(2) dragon tree medicinal material sample is taken, is crushed, 80-100 mesh is crossed, acquires verifying collection using near-infrared diffusing reflection spectrum
The near infrared spectrum of sample and calibration set sample；
(3) content of total polyphenols in every batch of dragon tree medicinal material is measured respectively；
(4) moisture content in every batch of dragon tree medicinal material is measured respectively；
(5) according to the Determination of Polyphenols and moisture content and step of step (3) and the resulting calibration set sample of step (4)
(1) near infrared spectrum of resulting calibration set sample is associated, and is established using Partial Least Squares total more in dragon tree medicinal material
The Near-Infrared Quantitative Analysis model of phenol, moisture content；
(6) atlas of near infrared spectra of verifying collection sample is calculated by the Near-Infrared Quantitative Analysis model that step (5) are established,
The Determination of Polyphenols and moisture content being verified in collection sample, to verify the stability and precision of prediction of model built；
(7) dragon tree medicinal material sample to be detected is taken, is crushed, 80-100 mesh is crossed, is adopted using near-infrared diffusing reflection spectrum
Collect near infrared spectrum, is calculated through model, obtain the content of the moisture content and effective component total polyphenols in dragon tree medicinal material sample.
It further, the use of near-infrared diffusing reflection spectrum sampling number is 32 times in step (2), resolution ratio 8cm-1,
Using air as reference, spectral scanning range 4000-10000cm-1, each sample multiple scanning 3 times is averaged, environment item
Part is 23 DEG C ± 0.5 DEG C of temperature, relative humidity 40% ± 2%.
Further, the near infrared spectrum is handled by first differential and Norris derivative filtering.
Further, the moisture content of dragon tree medicinal material measures by the following method in step (4):
S1: taking dragon tree medicinal material, smashes it through 80-100 mesh；
S2: it takes appropriate medicinal powder to be placed in 105 DEG C of thermostatic drying chambers and dries to constant weight；
S3: according to the weight of less loss, the moisture content of dragon tree medicinal material is calculated.
Further, the content of total polyphenols measures by the following method in dragon tree medicinal material in step (3):
S1: taking dragon tree medicinal material, smashes it through 80-100 mesh；
S2: taking appropriate medicinal powder in 250mL flask, and it is molten that the ethyl alcohol that volume fraction is 60-80% is measured in 6-8 times of addition
Liquid stirs evenly；
S3: placing refluxing extraction device in thermostat water bath, and bath temperature is 70-90 DEG C, extracts 50min, extracts
2-3 times, combined extract；
S4: extracting solution takes supernatant with 2000-3000r/min centrifugation 15-20min, extracting liquid volume is measured, using forint
The total polyphenols concentration of phenol method measurement extracting solution.
The invention has the benefit that this case utilizes near-infrared spectrum technique and partial least-square regression method, dragon is established
Quantitative analysis mould between dragon's blood crude drug-dragon tree medicinal material near infrared spectrum and its effective component total polyphenols and moisture content
Type has the advantages such as quick, lossless, realizes the quick detection of raw material compared with traditional detection method, to realize from source
Control the quality of Resina Draconis product.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the rapid detection method of Resina Draconis crude drug quality of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one
A kind of rapid detection method of Resina Draconis crude drug quality, including following detecting step:
(1) the dragon tree medicinal material for collecting different sources source is no less than 50 batches, randomly chooses 10 batches of samples as verifying collection
Sample, remaining sample carry out the foundation of quantitative calibration models as calibration set sample；
(2) dragon tree medicinal material sample is taken, is crushed, 80 meshes are crossed, acquires verifying collection sample using near-infrared diffusing reflection spectrum
With the near infrared spectrum of calibration set sample；It the use of near-infrared diffusing reflection spectrum sampling number is 32 times, resolution ratio 8cm-1, with sky
Gas is reference, spectral scanning range 4000-10000cm-1, each sample multiple scanning 3 times is averaged, and environmental condition is
23 DEG C ± 0.5 DEG C of temperature, relative humidity 40% ± 2%；
(3) content of total polyphenols in every batch of dragon tree medicinal material is measured respectively, and the content of total polyphenols passes through in dragon tree medicinal material
Following methods measure:
S1: taking dragon tree medicinal material, smashes it through 80 meshes；
S2: taking appropriate medicinal powder in 250mL flask, and the ethanol solution that 6 times of amount volume fractions are 60%, stirring is added
Uniformly；
S3: placing refluxing extraction device in thermostat water bath, and bath temperature is 70 DEG C, extracts 50min, extracts 2 times,
Combined extract；
S4: extracting solution takes supernatant with 2000r/min centrifugation 15min, measures extracting liquid volume, is measured using Forint phenol method
The total polyphenols concentration of extracting solution.
(4) moisture content in every batch of dragon tree medicinal material is measured respectively, and the moisture content of dragon tree medicinal material passes through with lower section
Method measures:
S1: taking dragon tree medicinal material, smashes it through 80 meshes；
S2: it takes appropriate medicinal powder to be placed in 105 DEG C of thermostatic drying chambers and dries to constant weight；
S3: according to the weight of less loss, the moisture content of dragon tree medicinal material is calculated；
(5) according to the Determination of Polyphenols and moisture content and step of step (3) and the resulting calibration set sample of step (4)
(1) near infrared spectrum of resulting calibration set sample is associated, and is established using Partial Least Squares total more in dragon tree medicinal material
The Near-Infrared Quantitative Analysis model of phenol, moisture content；The near infrared spectrum is flat by first differential and the filtering of Norris derivative
Sliding processing；
(6) atlas of near infrared spectra of verifying collection sample is calculated by the Near-Infrared Quantitative Analysis model that step (5) are established,
The Determination of Polyphenols and moisture content being verified in collection sample, to verify the stability and precision of prediction of model built；
(7) dragon tree medicinal material sample to be detected is taken, is crushed, 80 meshes are crossed, is acquired using near-infrared diffusing reflection spectrum close
Infrared spectroscopy is calculated through model, obtains the content of the moisture content and effective component total polyphenols in dragon tree medicinal material sample.
Embodiment two
A kind of rapid detection method of Resina Draconis crude drug quality, including following detecting step:
(1) the dragon tree medicinal material for collecting different sources source is no less than 50 batches, randomly chooses 10 batches of samples as verifying collection
Sample, remaining sample carry out the foundation of quantitative calibration models as calibration set sample；
(2) dragon tree medicinal material sample is taken, crushes, sieves with 100 mesh sieve, acquires verifying collection sample using near-infrared diffusing reflection spectrum
With the near infrared spectrum of calibration set sample；It the use of near-infrared diffusing reflection spectrum sampling number is 32 times, resolution ratio 8cm-1, with sky
Gas is reference, spectral scanning range 4000-10000cm-1, each sample multiple scanning 3 times is averaged, and environmental condition is
23 DEG C ± 0.5 DEG C of temperature, relative humidity 40% ± 2%；
(3) content of total polyphenols in every batch of dragon tree medicinal material is measured respectively, and the content of total polyphenols passes through in dragon tree medicinal material
Following methods measure:
S1: taking dragon tree medicinal material, smashes it through 100 meshes；
S2: taking appropriate medicinal powder in 250mL flask, and the ethanol solution that 8 times of amount volume fractions are 80%, stirring is added
Uniformly；
S3: placing refluxing extraction device in thermostat water bath, and bath temperature is 90 DEG C, extracts 50min, extracts 3 times,
Combined extract；
S4: extracting solution takes supernatant with 3000r/min centrifugation 20min, measures extracting liquid volume, is measured using Forint phenol method
The total polyphenols concentration of extracting solution.
(4) moisture content in every batch of dragon tree medicinal material is measured respectively, and the moisture content of dragon tree medicinal material passes through with lower section
Method measures:
S1: taking dragon tree medicinal material, smashes it through 100 meshes；
S2: it takes appropriate medicinal powder to be placed in 105 DEG C of thermostatic drying chambers and dries to constant weight；
S3: according to the weight of less loss, the moisture content of dragon tree medicinal material is calculated；
(5) according to the Determination of Polyphenols and moisture content and step of step (3) and the resulting calibration set sample of step (4)
(1) near infrared spectrum of resulting calibration set sample is associated, and is established using Partial Least Squares total more in dragon tree medicinal material
The Near-Infrared Quantitative Analysis model of phenol, moisture content；The near infrared spectrum is flat by first differential and the filtering of Norris derivative
Sliding processing；
(6) atlas of near infrared spectra of verifying collection sample is calculated by the Near-Infrared Quantitative Analysis model that step (5) are established,
The Determination of Polyphenols and moisture content being verified in collection sample, to verify the stability and precision of prediction of model built；
(7) dragon tree medicinal material sample to be detected is taken, crushes, sieves with 100 mesh sieve, is acquired using near-infrared diffusing reflection spectrum close
Infrared spectroscopy is calculated through model, obtains the content of the moisture content and effective component total polyphenols in dragon tree medicinal material sample.
The present invention and its embodiments have been described above, this description is no restricted, only reality of the invention
One of mode is applied, actual embodiment is not limited thereto.All in all if those skilled in the art are opened by it
Show, without departing from the spirit of the invention, not inventively design embodiment similar with the technical solution,
It is within the scope of protection of the invention.
Claims (5)
1. a kind of rapid detection method of Resina Draconis crude drug quality, it is characterised in that: including following detecting step:
(1) the dragon tree medicinal material for collecting different sources source is no less than 50 batches, randomly chooses 10 batches of samples as verifying and collects sample,
Remaining sample carries out the foundation of quantitative calibration models as calibration set sample；
(2) dragon tree medicinal material sample is taken, is crushed, 80-100 mesh is crossed, acquires verifying collection sample using near-infrared diffusing reflection spectrum
With the near infrared spectrum of calibration set sample；
(3) content of total polyphenols in every batch of dragon tree medicinal material is measured respectively；
(4) moisture content in every batch of dragon tree medicinal material is measured respectively；
(5) according to the Determination of Polyphenols and moisture content of step (3) and the resulting calibration set sample of step (4) and step (1) institute
The near infrared spectrum of the calibration set sample obtained is associated, and establishes total polyphenols, water in dragon tree medicinal material using Partial Least Squares
Divide the Near-Infrared Quantitative Analysis model of content；
(6) atlas of near infrared spectra of verifying collection sample is calculated by the Near-Infrared Quantitative Analysis model that step (5) are established, is obtained
Determination of Polyphenols and moisture content in verifying collection sample, to verify the stability and precision of prediction of model built；
(7) dragon tree medicinal material sample to be detected is taken, is crushed, 80-100 mesh is crossed, is acquired using near-infrared diffusing reflection spectrum close
Infrared spectroscopy is calculated through model, obtains the content of the moisture content and effective component total polyphenols in dragon tree medicinal material sample.
2. a kind of rapid detection method of Resina Draconis crude drug quality according to claim 1, it is characterised in that: in step
It (2) the use of near-infrared diffusing reflection spectrum sampling number is 32 times in, resolution ratio 8cm-1, using air as reference, spectral scan model
It encloses for 4000-10000cm-1, each sample multiple scanning 3 times is averaged, and environmental condition is 23 DEG C ± 0.5 DEG C of temperature, relatively
Humidity 40% ± 2%.
3. a kind of rapid detection method of Resina Draconis crude drug quality according to claim 1, it is characterised in that: described close
Infrared spectroscopy is handled by first differential and Norris derivative filtering.
4. a kind of rapid detection method of Resina Draconis crude drug quality according to claim 1, it is characterised in that: step
(4) moisture content of dragon tree medicinal material measures by the following method in:
S1: taking dragon tree medicinal material, smashes it through 80-100 mesh；
S2: it takes appropriate medicinal powder to be placed in 105 DEG C of thermostatic drying chambers and dries to constant weight；
S3: according to the weight of less loss, the moisture content of dragon tree medicinal material is calculated.
5. a kind of rapid detection method of Resina Draconis crude drug quality according to claim 1, it is characterised in that: step
(3) content of total polyphenols measures by the following method in dragon tree medicinal material in:
S1: taking dragon tree medicinal material, smashes it through 80-100 mesh；
S2: taking appropriate medicinal powder in 250mL flask, is added 6-8 times and measures the ethanol solution that volume fraction is 60-80%, stirs
It mixes uniformly；
S3: placing refluxing extraction device in thermostat water bath, and bath temperature is 70-90 DEG C, extracts 50min, extracts 2-3
It is secondary, combined extract；
S4: extracting solution takes supernatant with 2000-3000r/min centrifugation 15-20min, extracting liquid volume is measured, using Forint phenol method
Measure the total polyphenols concentration of extracting solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113189045A (en) * | 2021-06-17 | 2021-07-30 | 天津科技大学 | Method for rapidly determining content of total phenols in pear powder by utilizing near infrared spectrum technology |
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| CN101059426A (en) * | 2007-05-29 | 2007-10-24 | 浙江大学 | Method for non-destructive measurement for tea polyphenol content of tea based on near infrared spectrum technology |
| CN101299022A (en) * | 2008-06-20 | 2008-11-05 | 河南中医学院 | Method for evaluating Chinese medicine comprehensive quality using near infrared spectra technique |
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| CN113189045A (en) * | 2021-06-17 | 2021-07-30 | 天津科技大学 | Method for rapidly determining content of total phenols in pear powder by utilizing near infrared spectrum technology |
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