CN106932418A - Paris polyphylla or the discrimination method of Yunnan Rhizoma Paridis - Google Patents
Paris polyphylla or the discrimination method of Yunnan Rhizoma Paridis Download PDFInfo
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- CN106932418A CN106932418A CN201710166975.5A CN201710166975A CN106932418A CN 106932418 A CN106932418 A CN 106932418A CN 201710166975 A CN201710166975 A CN 201710166975A CN 106932418 A CN106932418 A CN 106932418A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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Abstract
The invention provides paris polyphylla or the discrimination method of Yunnan Rhizoma Paridis, it is realized using x-ray powder diffraction.Using the above method, the certified products of paris polyphylla or Yunnan Rhizoma Paridis can be differentiated, for the identification of paris polyphylla or Yunnan Rhizoma Paridis provides new method by comparing the similarity of standard finger-print and medicinal materials fingerprint to be checked.
Description
Technical field
The present invention relates to Chinese medicine quality testing field, and in particular to the discrimination method of paris polyphylla or Yunnan Rhizoma Paridis.
Background technology
Paris polyphylla is liliaceous plant P.polyphylla Smith var.chinensis (Franch.) Hara.
Dry rhizome, version in 2015《Pharmacopoeia of People's Republic of China》Regulation with chonglou saponin be its criteria of quality evaluation, it and cloud
South heavy building Paris polyphylla Smith var.yunnanensis (Franch.) Hand.-Mazz. is by States Pharmacopoeia specifications
It is the regular source of Paris polyphylla.Paris polyphylla steroid saponin is the main active of Paris polyphylla, with antitumor, anti-inflammatory, hemostasis, antibacterial,
Analgesia, calm, anti-oxidant, immunological regulation, suppression angiogenesis, protection liver and renal effect.
The relevant enterprises such as Yunnan Baiyao group, Sichuan Guangda Pharmaceutical Co., Ltd and TongHua WanTong Pharmacy Co., Ltd
It is big to rhizoma paris rhizome resources requirement, wild resource is excessively excavated, the market price rises suddenly and sharply, and current rhizoma paris rhizome wild resource is increasingly
It is in imminent danger, meanwhile, artificial growth there is no high-quality, the introduces a collection supply market of stabilization at present, cause the rhizome of non-pharmacopeia Paris polyphylla plant species
Commodity market is full of, the bottleneck of restriction Paris polyphylla pharmaceutical industries sustainable development is had become, the rhizoma paris rhizome of medicinal material market is difficult
Accurately differentiated using methods such as conventional proterties, micro-, physics and chemistry, thin layer discriminatings, therefore, set up the new of paris polyphylla
Discrimination method seems especially necessary.
The content of the invention
It is a kind of to paris polyphylla or the discrimination method of Yunnan Rhizoma Paridis present invention aim at providing first.
Specifically, the invention provides paris polyphylla or the discrimination method of Yunnan Rhizoma Paridis, it is using x-ray powder diffraction
Realize, concrete operations are as follows：
(1) more than 10 batches paris polyphyllas or Yunnan Rhizoma Paridis are taken, is detected using x-ray powder diffraction, with each batch of sample
Based on each diffraction maximum peak intensity average value and the corresponding 2 θ values of each diffraction maximum in detection data, x-ray powder diffraction mark is obtained
Quasi- finger-print；
(2) medicinal material to be checked is taken, is detected using step (1) identical x-ray powder diffraction condition, obtained medicinal material to be checked and refer to
Line collection of illustrative plates；
(3) medicinal materials fingerprint to be checked and x-ray powder diffraction standard finger-print are carried out into similarity-rough set, is differentiated to be checked
The true and false of medicinal material.
The selection of step (1) Chinese medicine batch be should ensure that more than 10 batches, but concrete numerical value is not fixed, as long as meeting system
Meter learns meaning.In addition, " paris polyphylla or Yunnan Rhizoma Paridis " described in step (1), refer to known into skilled worker through other
Section is accredited as the certified products of paris polyphylla or Yunnan Rhizoma Paridis.
" medicinal material to be checked " described in step (2), can be certified products, or adulterant.The present invention is by the above method
Certified products and adulterant can be differentiated and distinguished.
Finger-print refers to the DNA of some complex materials, such as Chinese medicine, certain organism or certain tissue or cell, egg
After white matter is appropriately processed, using certain analysis means, what is obtained can indicate the chromatogram or spectrogram of its chemical feature.
" similarity ", by Chinese Pharmacopoeia Commission as a qualitative, quantitative parameter, is defined as in traditional Chinese medicine fingerprint standard one
The important evaluation index of item, is applied to the research (National Drug Administration, 2000) of chromatogram class finger-print at present.At present
, it is known that the x-ray powder pattern fingerprint collection of illustrative plates that different chemical composition draws has differences certainly, therefore, the present invention can lead to
Cross this finger-print detection technique effectively to make a distinction paris polyphylla with other medicinal materials, reach the effect of discriminating.
In a specific embodiment of the invention, x-ray powder diffraction is carried out using CuK α radiation.
Wherein, 8 °/min of sweep speed.
Wherein, DS=SS=1 ° of slit width, RS=0.3mm.
Wherein, the θ of sweep limits 2：5-65°.
Wherein, need to crush before each sample is detected, and cross 100~200 mesh sieves.
In a specific embodiment of the invention, finger-print is obtained using OriginPro software data processings.In addition,
The data processing of the finger-print, also can be using the correlation technique in patent 201410105727.6.
According to discrimination method of the present invention, in step (3), when similarity is more than 0.90, then judge that medicinal material to be checked is seven
Leaf a flower or Yunnan Rhizoma Paridis.
Using the above method, can be by comparing the similarity of standard finger-print and medicinal materials fingerprint to be checked, by seven
The certified products of leaf a flower or Yunnan Rhizoma Paridis is differentiated, for the identification of paris polyphylla or Yunnan Rhizoma Paridis provides new method.
In a specific embodiment of the invention, the method practice has arrived the discriminating to paris polyphylla.Wherein, institute
State x-ray powder diffraction standard finger-print as shown in Figure 2.If medicinal material to be checked is compared with Fig. 2, similarity is less than 0.90, then can sentence
The disconnected medicinal material to be checked is not the certified products of paris polyphylla.
In a specific embodiment of the invention, the similarity of multiple batches of paris polyphylla medicinal material is up to more than 0.9900,
Therefore, if will also be recognized that medicinal material to be checked in the present invention compared with Fig. 2, similarity is higher than 0.9900, then can determine whether the medicine to be checked
Material is the certified products of paris polyphylla.
The present invention has used two methods of correlation coefficient process, co sinus vector included angle method to calculate similarity, two in an experiment
The method of kind is the common method of similarity, and its computing formula is as follows：
In a specific embodiment of the invention, for paris polyphylla, similarity is carried out using correlation coefficient process
Judgement, its result of determination may be better than co sinus vector included angle method.
Brief description of the drawings
The X-ray diffraction finger-print of the multiple batches of paris polyphylla rhizomes of Fig. 1
The X-ray diffraction standard finger-print of Fig. 2 paris polyphylla rhizomes
Specific embodiment
Instrument and material
General analysis XD-6 types x-ray powder diffraction instrument (Beijing Puxi General Instrument Co., Ltd), IR200 Fouriers become
Change infrared spectrometer (Thermo Necolet companies of the U.S.)；HX-200 type high speeds medicinal herb grinder (Zhejiang Yongkang small stream bank hardware
Medical instrument factory)；DHG-9246 types electric heating constant-temperature blowing drying box (the upper grand experimental facilities Co., Ltd of Nereid).Agate mortar.KBr powder
Last (spectroscopic pure) (Thermo companies of the U.S.).
Paris polyphylla and rhizome are taught by Southwest University for Nationalities national medicine research institute Liu Yuan, Sichuan University's West China pharmacy
Institute professor Zhang Hao identifies that former plant specimen and medicinal material Sample storage are in Southwest University for Nationalities, HuaXi college of pharmacy, SiChuan University.Sample
Information is shown in Table 1.
Table 4-1 paris polyphylla sample Ji Yuan and place of production information
Embodiment 1
Detection method：
Sample treatment：Paris polyphylla rhizome sample comminution is taken, 60 DEG C of drying 6h cross 100 mesh sieves standby.Experimental condition：
CuK α are radiated；Scan mode：It is qualitative, step-scan；Voltage/current：36kV/20mA；Sweep speed：8°/min；DS=SS=
1 °, RS=0.3mm；Step width：0.02°；The θ of sweep limits 2：5-65°.
Testing result：
1st, total Test data OriginPro 8.5 processes (smooth) at 35 points, powder diffraction spectrum is obtained, as a result as schemed
1。
2nd, the foundation of X diffraction standards finger-print
Before similarity analysis are carried out, referred to as X diffraction standards with the average value of 10 parts of paris polyphylla rhizome peak intensities
The peak intensity of line collection of illustrative plates, the X diffraction standards finger-print such as Fig. 2 for finally giving.
3rd, X diffracting spectrums similarity analysis
Conventional similarity analysis method has two kinds of " correlation coefficient process " and " co sinus vector included angle method ", and computing formula is such as
Under：
Using similarity (coefficient correlation and included angle cosine) between form calculating each sample.
The Similarity Measure result of table 2
Above-described embodiment calculates the peak for obtaining X diffraction standard finger-prints according to the matching result at peak using mean value method
Value；Interplanar distance d diffraction relative intensities I/I0Represent diffraction peak；With the θ of angle 2 as abscissa, diffraction peak (d/I/I0) it is vertical
Coordinate, forms paris polyphylla rhizome X diffraction standard finger-prints, and carried out the comparing of similarity.More than vector angle
When string method calculates similarity, S8 is illustrated and the quality condition of sample is had certain relation with to compare similarity low compared with other samples, but
It is that data result of calculation is extremely approached, gap is not obvious, is unfavorable for the comparing of sample room；And when being calculated with correlation coefficient process, its
Result then has larger difference.Premenstruum (premenstrua) identifies S8 chonglou saponins content well below States Pharmacopoeia specifications 0.6%, and its similarity exists
0.9987, this analysis result is consistent with infrared spectrum identification result；The similarity of remaining X diffracting spectrum and standard finger-print
More than 0.9992.0.9900 is all higher than according to the visible similarity of result of the comparison, phase very high each other is embodied
Like property, the relative stability of the different Paris polyphylla rhizome quality of Sichuan is further illustrated, built while also illustrate that
Vertical X diffraction standard finger-print reliability.
From analysis, similarity point is carried out to the X pattern fingerprints collection of illustrative plates of paris polyphylla rhizome using correlation coefficient process
During analysis, its result more can exactly reflect the actual mass situation of paris polyphylla rhizome, can be used for paris polyphylla medicinal material
The discriminating and quality evaluation of root medicinal material.
Claims (10)
1. the discrimination method of paris polyphylla or Yunnan Rhizoma Paridis, it is characterised in that：It realizes having using x-ray powder diffraction
Gymnastics is made as follows：
(1) more than 10 batches paris polyphyllas or Yunnan Rhizoma Paridis are taken, is detected using x-ray powder diffraction, with each batch of sample detection
Based on each diffraction maximum peak intensity average value and the corresponding 2 θ values of each diffraction maximum in data, obtain x-ray powder diffraction standard and refer to
Line collection of illustrative plates；
(2) medicinal material to be checked is taken, is detected using step (1) identical x-ray powder diffraction condition, obtain medicinal material fingerprint image to be checked
Spectrum；
(3) medicinal materials fingerprint to be checked and x-ray powder diffraction standard finger-print are carried out into similarity-rough set, differentiates medicinal material to be checked
The true and false.
2. discrimination method according to claim 1, it is characterised in that：X-ray powder diffraction is carried out using CuK α radiation.
3. discrimination method according to claim 2, it is characterised in that：8 °/min of sweep speed.
4. discrimination method according to claim 2, it is characterised in that：DS=SS=1 ° of slit width, RS=0.3mm.
5. discrimination method according to claim 2, it is characterised in that：The θ of sweep limits 2：5-65°.
6. discrimination method according to claim 1, it is characterised in that：Each sample needs to crush before being detected, and crosses 100
~200 mesh sieves.
7. discrimination method according to claim 1, it is characterised in that：Using OriginPro software processing finger-prints.
8. discrimination method according to claim 1, it is characterised in that：In step (3), when similarity is more than 0.90,
Then judge that medicinal material to be checked is paris polyphylla or Yunnan Rhizoma Paridis.
9. the discrimination method according to claim 1~8 any one, it is characterised in that：Methods described is seven leaves one of discriminating
The method of branch flower.
10. discrimination method according to claim 9, it is characterised in that：The x-ray powder diffraction standard finger-print is as schemed
Shown in 2.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108490007A (en) * | 2018-06-04 | 2018-09-04 | 西南民族大学 | The method that subdigitate wormwood herb and subdigitate wormwood herb charcoal are distinguished using X-ray diffraction method |
| CN109055603A (en) * | 2018-10-11 | 2018-12-21 | 湖北省农业科学院中药材研究所 | A method of building paris plant finger-print is marked using CDDP |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103913476A (en) * | 2014-03-20 | 2014-07-09 | 青海师范大学 | Method for obtaining powder diffraction file of plant medicinal material |
| CN104034743A (en) * | 2014-05-29 | 2014-09-10 | 南京中医药大学 | Method for establishing X-ray powder diffraction Fourier fingerprint spectrum of limonite, standard fingerprint spectrum and application of X-ray powder diffraction Fourier fingerprint spectrum |
| CN105115934A (en) * | 2015-09-17 | 2015-12-02 | 大恒新纪元科技股份有限公司 | Method for detecting full ingredient granule Chinese herbal rhizoma paridis based on terahertz spectrum technology |
| CN106353417A (en) * | 2016-08-14 | 2017-01-25 | 西南民族大学 | UPLC (ultra-performance liquid chromatography) detection method of multiple steroid saponins in Yunnan rhizoma paridis or its polygerm strain |
-
2017
- 2017-03-20 CN CN201710166975.5A patent/CN106932418A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103913476A (en) * | 2014-03-20 | 2014-07-09 | 青海师范大学 | Method for obtaining powder diffraction file of plant medicinal material |
| CN104034743A (en) * | 2014-05-29 | 2014-09-10 | 南京中医药大学 | Method for establishing X-ray powder diffraction Fourier fingerprint spectrum of limonite, standard fingerprint spectrum and application of X-ray powder diffraction Fourier fingerprint spectrum |
| CN105115934A (en) * | 2015-09-17 | 2015-12-02 | 大恒新纪元科技股份有限公司 | Method for detecting full ingredient granule Chinese herbal rhizoma paridis based on terahertz spectrum technology |
| CN106353417A (en) * | 2016-08-14 | 2017-01-25 | 西南民族大学 | UPLC (ultra-performance liquid chromatography) detection method of multiple steroid saponins in Yunnan rhizoma paridis or its polygerm strain |
Non-Patent Citations (1)
| Title |
|---|
| 何立巍 等: "中药石膏炮制品的X 射线衍射分析及指纹图谱的建立", 《天津中医药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108490007A (en) * | 2018-06-04 | 2018-09-04 | 西南民族大学 | The method that subdigitate wormwood herb and subdigitate wormwood herb charcoal are distinguished using X-ray diffraction method |
| CN108490007B (en) * | 2018-06-04 | 2021-02-26 | 西南民族大学 | Method for distinguishing artemisia rupestris L and artemisia rupestris L charcoal by adopting X-ray diffraction method |
| CN109055603A (en) * | 2018-10-11 | 2018-12-21 | 湖北省农业科学院中药材研究所 | A method of building paris plant finger-print is marked using CDDP |
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