CN108693138A - Quickly judge the method for elution beginning and end and application in Sodium Danshensu extracting solution macroporous resin adsorption separation process - Google Patents
Quickly judge the method for elution beginning and end and application in Sodium Danshensu extracting solution macroporous resin adsorption separation process Download PDFInfo
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- CN108693138A CN108693138A CN201810361490.6A CN201810361490A CN108693138A CN 108693138 A CN108693138 A CN 108693138A CN 201810361490 A CN201810361490 A CN 201810361490A CN 108693138 A CN108693138 A CN 108693138A
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- ZMMKVDBZTXUHFO-DDWIOCJRSA-M sodium;(2r)-3-(3,4-dihydroxyphenyl)-2-hydroxypropanoate Chemical compound [Na+].[O-]C(=O)[C@H](O)CC1=CC=C(O)C(O)=C1 ZMMKVDBZTXUHFO-DDWIOCJRSA-M 0.000 title claims abstract description 198
- 238000000034 method Methods 0.000 title claims abstract description 141
- 238000010828 elution Methods 0.000 title claims abstract description 57
- 239000011347 resin Substances 0.000 title claims abstract description 51
- 229920005989 resin Polymers 0.000 title claims abstract description 51
- 238000000926 separation method Methods 0.000 title claims abstract description 34
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 31
- 238000001228 spectrum Methods 0.000 claims abstract description 67
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 47
- 230000008569 process Effects 0.000 claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 238000010561 standard procedure Methods 0.000 claims abstract description 16
- 238000012937 correction Methods 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 17
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 15
- 229910052708 sodium Inorganic materials 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 235000017276 Salvia Nutrition 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 11
- 239000003643 water by type Substances 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008213 purified water Substances 0.000 claims description 5
- 230000003595 spectral effect Effects 0.000 claims description 5
- 238000004611 spectroscopical analysis Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 240000007164 Salvia officinalis Species 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 15
- 238000001514 detection method Methods 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 49
- 238000009795 derivation Methods 0.000 description 14
- 238000007781 pre-processing Methods 0.000 description 13
- PAFLSMZLRSPALU-MRVPVSSYSA-N (2R)-3-(3,4-dihydroxyphenyl)lactic acid Chemical compound OC(=O)[C@H](O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-MRVPVSSYSA-N 0.000 description 10
- PAFLSMZLRSPALU-QMMMGPOBSA-N Danshensu Natural products OC(=O)[C@@H](O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-QMMMGPOBSA-N 0.000 description 10
- 241001072909 Salvia Species 0.000 description 10
- PAFLSMZLRSPALU-UHFFFAOYSA-N Salvianic acid A Natural products OC(=O)C(O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-UHFFFAOYSA-N 0.000 description 10
- 238000012216 screening Methods 0.000 description 8
- 241000208340 Araliaceae Species 0.000 description 7
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 7
- 235000003140 Panax quinquefolius Nutrition 0.000 description 7
- 235000008434 ginseng Nutrition 0.000 description 7
- 238000005457 optimization Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 229940079593 drug Drugs 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 230000009466 transformation Effects 0.000 description 5
- 239000004480 active ingredient Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 238000010187 selection method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 3
- 238000013528 artificial neural network Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000010606 normalization Methods 0.000 description 3
- 238000012706 support-vector machine Methods 0.000 description 3
- 238000012795 verification Methods 0.000 description 3
- 241000304195 Salvia miltiorrhiza Species 0.000 description 2
- 235000011135 Salvia miltiorrhiza Nutrition 0.000 description 2
- 230000017531 blood circulation Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000001976 improved effect Effects 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000010238 partial least squares regression Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 150000007965 phenolic acids Chemical class 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010007247 Carbuncle Diseases 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 208000001431 Psychomotor Agitation Diseases 0.000 description 1
- 206010038743 Restlessness Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229940093181 glucose injection Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002107 myocardial effect Effects 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000009452 shenxiong glucose Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- 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
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
Abstract
The present invention provides method and applications that beginning and end is eluted in a kind of quick judgement Sodium Danshensu extracting solution macroporous resin adsorption separation process, are related to Chinese medicine quality of production detection technique field.The judgment method, the Sodium Danshensu efflux for the different batches that macroreticular resin elution process obtains is chosen first as sample, constitute calibration samples collection, Sodium Danshensu content in calibration samples collection each sample is measured using standard method, then the original near infrared spectrum data of each sample is acquired, processing, obtain the characteristic spectrum data of each sample, the characteristic spectrum data of each sample are concentrated to establish corresponding calibration model with Sodium Danshensu content calibration samples using chemometrics method, calibration model is finally used to predict the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, it can determine whether the elution beginning and end of elution process.Judgment method provided by the invention is quick and easy, accurate and reliable, favorable reproducibility.
Description
Technical field
The present invention relates to Chinese medicine quality of production detection technique fields, quickly judging Sodium Danshensu in particular to one kind
Method and the application of beginning and end are eluted in extracting solution macroporous resin adsorption separation process.
Background technology
Radix Salviae Miltiorrhizae is traditional rare Chinese medicine, be labiate Radix Salviae Miltiorrhizae Salvia miltiorrhiza Bge. dry root and
Rhizome, bitter, cold nature, the thoughts of returning home, liver two pass through, and have effects that promoting blood circulation, inducing meastruation to relieve menalgia, relieving restlessness that clears away heart-fire, cool blood to disappear carbuncle.It is red
Water-soluble phenolic acrylic component in ginseng mainly has danshensu, tanshin polyphenolic acid B etc..Modern pharmacological studies have shown that root of red-rooted salvia phenolic acid constituents
Have the effects that improve cycle, inhibit platelet aggregation, is anti-oxidant, increasing coronary flow and myocardial oxygen consumption, be Radix Salviae Miltiorrhizae dissolving stasis,
The main active of promoting blood circulation.
Since the danshensu in root of red-rooted salvia phenolic acid constituents is unstable, the form of Sodium Danshensu is usually made.Danshensu
There are many extraction processes of sodium, wherein carries out one kind that adsorbing separation is common using macroreticular resin, therefore macroporous resin adsorption is divided
From an important link in stage and Radix Salviae Miltiorrhizae industrialized production, the height of purification efficiency determines that can its subsequent production
Smoothly carry out, it is therefore necessary to which Sodium Danshensu extracting solution macroporous resin adsorption separation phase is furtherd investigate.
Currently, in Sodium Danshensu extracting solution macroporous resin adsorption separation phase elute beginning and end judgement, mainly according to
By practical production experience, this method causes eluting solvent waste occur, there are relatively large deviation, Wu Fazhun for the amount of collection eluent
The beginning and end for really judging elution, causes sample quality irregular, the monitoring analysis being less useful in actual production process.
Therefore, from the angle for improving production efficiency, there is an urgent need to study one kind quickly, efficiently, accurately judging that Sodium Danshensu carries
Take the method that beginning and end is eluted in liquid macroporous resin adsorption separation phase.
In view of this, special propose the present invention.
Invention content
First of the present invention is designed to provide one kind and quickly judging that Sodium Danshensu extracting solution macroporous resin adsorption detaches
The method for eluting beginning and end in the process, this method is quick and easy, accurate and reliable, favorable reproducibility, can be used for Sodium Danshensu and carries
The quick measurement for taking liquid macroporous resin adsorption separation phase active ingredient improves eluent in existing Radix Salviae Miltiorrhizae adsorption separation process
The problems such as dosage is excessive, elution time is long.
Second object of the present invention is that providing one kind quickly judging that Sodium Danshensu extracting solution macroporous resin adsorption detaches
Application of the method for elution beginning and end in Radix Salviae Miltiorrhizae extraction in the process.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme:
The present invention provide it is a kind of quickly judge to elute in Sodium Danshensu extracting solution macroporous resin adsorption separation process starting point with
The method of terminal, includes the following steps;
(a) foundation of calibration model
Choose the Sodium Danshensu efflux for the different batches that Sodium Danshensu extracting solution is obtained using macroreticular resin elution process
As sample, calibration samples collection is constituted;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method, meanwhile, and to correction
The original near infrared spectrum data of each sample is acquired, handles in sample set, obtains the characteristic spectrum data of each sample, uses
Calibration samples are concentrated the correction corresponding with the foundation of Sodium Danshensu content of the characteristic spectrum data of each sample by chemometrics method
Model;
(b) calibration model is used to predict the content of Sodium Danshensu in Sodium Danshensu efflux to be measured
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, danshensu to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through calibration model meter by the characteristic spectrum data of sodium efflux
It calculates and obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, and then judge the elution beginning and end of elution process.
Further, in step (a), in the characteristic spectrum data and Sodium Danshensu content that calibration samples are concentrated to each sample
It establishes after corresponding calibration model, further includes the steps that using parametric test and filtering out optimal calibration model.
Further, in step (a), using near infrared spectrometer calibration samples are concentrated with the original near infrared light of each sample
Modal data is acquired, and obtained original near infrared spectrum data is selected by Pretreated spectra and wave-length coverage, is obtained each
Calibration samples are concentrated the characteristic spectrum data and Radix Salviae Miltiorrhizae of each sample using chemometrics method by the characteristic spectrum data of sample
Plain sodium content establishes corresponding calibration model, and using the parametric test calibration model, filters out optimal calibration model.
Further, in step (a), using near infrared spectrometer calibration samples are concentrated with the original near infrared light of each sample
Modal data is acquired, and each Sample Scan is primary, pre- to original near infrared spectrum data using chemometrics application software
Processing and wavelength band selection, remove background interference, spectral drift and other noise jammings, obtain the characteristic spectrum number of each sample
According to using chemometrics method that the characteristic spectrum data of calibration samples concentration sample are corresponding with the foundation of Sodium Danshensu content
Calibration model, and using the parametric test calibration model, filter out optimal calibration model.
Further, in step (a), the test sample method of original near infrared spectra collection:Transmission/transflector measures, and differentiates
Rate is 1nm or 8cm-1, scanning times 1~64 time, light path 1,2,5,10mm, scanning range:Wave-length coverage be 800~
2500nm。
Further, Sodium Danshensu extracting solution elution process includes the following steps:
By Sodium Danshensu extracting solution through macroreticular resin loading absorption after, be rinsed with purified water, from start collect Radix Salviae Miltiorrhizae
While plain sodium efflux, sample collection is carried out to Sodium Danshensu efflux every 1~10min, separation obtains different batches
Sodium Danshensu efflux.
Further, in Sodium Danshensu extracting solution elution process, Sodium Danshensu extracting solution is inhaled through macroreticular resin loading
Attached to be rinsed with 3BV~15BV purified waters, flow velocity is 3BV/h~15BV/h;
And/or separation, preferably 0.45 μm -0.8 μm of miillpore filter are filtered using miillpore filter, it is further excellent
It is selected as 0.45 μm of miillpore filter.
Further, the Sodium Danshensu efflux of obtained different batches is sealed at room temperature;
And/or Sodium Danshensu extracting solution is extracted by salvia piece and is made.
Further, starting point and end are eluted in the quick judgement Sodium Danshensu extracting solution macroporous resin adsorption separation process
The method of point includes the following steps:
(a) foundation of calibration model
In Sodium Danshensu extracting solution elution process, Sodium Danshensu extracting solution is used into 3BV after the absorption of macroreticular resin loading
~15BV purified waters are rinsed, and flow velocity is 3BV/h~15BV/h, and sample is carried out to Sodium Danshensu efflux every 1~10min
Acquisition crosses 0.45 μm of miillpore filter, the Sodium Danshensu efflux for obtaining different batches is sealed;
The Sodium Danshensu efflux for the different batches that Sodium Danshensu extracting solution elution process obtains is chosen as sample, is constituted
Calibration samples collection;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method, meanwhile, using close red
External spectrum instrument concentrates the original near infrared spectrum data of each sample to be acquired calibration samples, the original near infrared light that will be obtained
Modal data is selected by Pretreated spectra and wave-length coverage, the characteristic spectrum data of each sample is obtained, using Chemical Measurement side
Calibration samples are concentrated the characteristic spectrum data of each sample to establish corresponding calibration model with Sodium Danshensu content by method, and using ginseng
Number examines the calibration model, filters out optimal calibration model;
(b) content of Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted using optimal calibration model
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, danshensu to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through optimal correction by the characteristic spectrum data of sodium efflux
Model, which calculates, obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, so judge the elution starting point of elution process with
Terminal.
Quickly judge to elute in Sodium Danshensu extracting solution macroporous resin adsorption separation process the present invention also provides a kind of
Application of the method for point and terminal in Radix Salviae Miltiorrhizae production.
Compared with prior art, starting point is eluted in quick judgement Radix Salviae Miltiorrhizae macroporous resin adsorption separation process provided by the invention
It is had the advantages that with the method for terminal and application:
(1) quickly judge to elute in Sodium Danshensu extracting solution macroporous resin adsorption separation process the present invention provides a kind of
The method of point and terminal chooses the Sodium Danshensu efflux for the different batches that macroreticular resin elution process obtains as sample first
Product constitute calibration samples collection, the Sodium Danshensu content in calibration samples collection each sample are measured using standard method, then to correction
The original near infrared spectrum data of each sample is acquired, handles in sample set, obtains the characteristic spectrum data of each sample, uses
Calibration samples are concentrated the correction corresponding with the foundation of Sodium Danshensu content of the characteristic spectrum data of each sample by chemometrics method
Model finally uses calibration model to predict the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, you can to judge elution process
Elution beginning and end;
Compared with the conventional method, judgment method minute provided by the invention shortens dramatically, and usually each sample exists
It is completed within 1min, entire deterministic process is quick and easy, accurate and reliable, favorable reproducibility, and accuracy of detection also approaches standard method,
Can in Accurate Prediction Sodium Danshensu efflux to be measured Sodium Danshensu content, it can be achieved that Sodium Danshensu extracting solution macroreticular resin
The judgement that elution beginning and end is carried out in adsorption separation process, is effectively improved Radix Salviae Miltiorrhizae macroreticular resin elution process in the prior art
The problems such as middle eluent dosage is excessive, elution time is long.
(2) in quick judgement Sodium Danshensu extracting solution macroporous resin adsorption separation process provided by the invention elute starting point and
The method of terminal, advanced, science, finding speed are fast, and while ensuring drug quality and production efficiency, testing cost is low,
With very strong exploitativeness and operability, it can be used for laboratory and examine soon, produce on-line measurement etc., being Chinese Traditional Medicine has
The big innovation that effective component content measures, has good economic and social benefit.
(3) the present invention also provides quickly judge to elute starting point in Sodium Danshensu extracting solution macroporous resin adsorption separation process
With the application of the method for terminal in Radix Salviae Miltiorrhizae production.Above-mentioned quick judgment method is that the increased quality of salvia miltiorrhiza traditional Chinese herbal preparation is provided with
The technical guarantee of power, while the quick judgment method can also be used for the fast of Radix Salviae Miltiorrhizae Chinese Traditional Medicine other key production technology thereof points
Speed on-line monitoring, the starting point for production process judges and endpoint and quality control provide a kind of real-time online and quickly examine
Survey method.In view of advantage possessed by above-mentioned judgment method so that the judgment method has good in Radix Salviae Miltiorrhizae production process
Using.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is to predict that Sodium Danshensu contains in Sodium Danshensu efflux to be measured using the calibration model in the embodiment of the present invention 1
The tendency chart of amount;
Fig. 2 is to predict that Sodium Danshensu contains in Sodium Danshensu efflux to be measured using the calibration model in the embodiment of the present invention 2
The tendency chart of amount.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
It is well known that Chinese medicine is made of plurality of active ingredients, and different Chinese medicine character difference are very big, and Chinese medicine extract exists
The judgment method meeting " different because of medicine " of elution beginning and end is collected during isolating and purifying.And currently, for how quickly to sentence
Beginning and end is eluted in disconnected Sodium Danshensu extracting solution macroporous resin adsorption separation process, the research of this respect is less.
For this purpose, according to an aspect of the invention, there is provided a kind of quickly judging that Sodium Danshensu extracting solution macroreticular resin is inhaled
Fufen includes the following steps from the method for eluting beginning and end in the process;
(a) foundation of calibration model
Choose the Sodium Danshensu efflux for the different batches that Sodium Danshensu extracting solution is obtained using macroreticular resin elution process
As sample, calibration samples collection is constituted;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method, meanwhile, and to correction
The original near infrared spectrum data of each sample is acquired, handles in sample set, obtains the characteristic spectrum data of each sample, uses
Calibration samples are concentrated the correction corresponding with the foundation of Sodium Danshensu content of the characteristic spectrum data of each sample by chemometrics method
Model;
(b) calibration model is used to predict the content of Sodium Danshensu in Sodium Danshensu efflux to be measured
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, danshensu to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through calibration model meter by the characteristic spectrum data of sodium efflux
It calculates and obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, and then judge the elution beginning and end of elution process.
Specifically, Sodium Danshensu is the sodium salt of the primary water-soluble active ingredient danshensu in Radix Salviae Miltiorrhizae.Radix Salviae Miltiorrhizae Chinese medicine is adopted
Salvia piece is obtained with physics mode, then salvia piece is required according to actual production, produce and Sodium Danshensu extracting solution is made.
It is mentioned in the present invention " to concentrate the Sodium Danshensu content of each sample to survey calibration samples according to standard method
" standard method " in calmly " can be found in " shenxiong glucose injection quality standard ", and standard number is:WS-10001-(HD-
1136) -2002-2012-2017, this is the conventional method of ability domain measurement Sodium Danshensu content.
Efflux starts target effective ingredient occur when " elution starting point " refers to elution, and " elution terminal " refers to active ingredient
Content relative concentration change rate tends to sample point when set threshold value, and the threshold value is different due to the difference of object.
It should be noted that in the gatherer process of original near infrared spectrum data, inevitably due to instrument state,
The nuance of environmental disturbances and determination condition leads to the variation of spectrum, by being pre-processed spectral signal to eliminate this
Class influences, and improves the performance of calibration model.Preprocessing procedures can be without pretreatment, convolution is smooth, the derivation of single order convolution, two
The derivation of rank convolution, standard normal variable transformation, the correction of polynary scattered color or normalization and the one kind being combined with each other in algorithm or extremely
Few two kinds of combination.
In addition, calibration model will constantly update amendment and maintenance.When the determination condition (time or space) of sample is sent out
When raw change, it is necessary to be verified using verification the set pair analysis model, if it find that the predictive ability of model reduces, it is necessary to correct
Increase this sample survey in sample sets, and changes calibration samples collection according to above-mentioned steps again.One prediction effect it is good and
Stable model needs constantly to carry out perfect, could play maximum effect in practical applications.
Quickly judge to elute starting point in Sodium Danshensu extracting solution macroporous resin adsorption separation process the present invention provides a kind of
With the method for terminal, compared with the conventional method, the judgment method process is quick and easy, accurate and reliable, favorable reproducibility, accuracy of detection
Also approach standard method, can in Accurate Prediction Sodium Danshensu efflux to be measured Sodium Danshensu content, it can be achieved that Radix Salviae Miltiorrhizae
The judgement that elution beginning and end is carried out in macroporous resin adsorption separation process, is effectively improved Radix Salviae Miltiorrhizae macroreticular resin in the prior art
The problems such as eluent dosage is excessive in elution process, elution time is long.
As a kind of preferred embodiment of the present invention, in step (a), in the characteristic light that calibration samples are concentrated to each sample
Further include using parametric test and filtering out optimal school after modal data establishes corresponding calibration model with Sodium Danshensu content
The step of positive model.
Model evaluation parameter SECV, SEC etc. can be used and compare calibration model, filter out optimal calibration model, to improve
The accuracy of calibration model.
As a kind of preferred embodiment of the present invention, in step (a), calibration samples are concentrated using near infrared spectrometer
The original near infrared spectrum data of each sample is acquired, by obtained original near infrared spectrum data by Pretreated spectra and
Wave-length coverage selects, and obtains the characteristic spectrum data of each sample, calibration samples are concentrated each sample using chemometrics method
Characteristic spectrum data and Sodium Danshensu content establish corresponding calibration model, and using the parametric test calibration model, screening
Go out optimal calibration model.
As a kind of preferred embodiment of the present invention, in step (a), calibration samples are concentrated using near infrared spectrometer
The original near infrared spectrum data of each sample is acquired, and each Sample Scan is primary, using chemometrics application software pair
Original near infrared spectrum data pretreatment and wavelength band selection, remove background interference, spectral drift and other noise jammings, obtain
To the characteristic spectrum data of each sample, calibration samples are concentrated to the characteristic spectrum data and pellet of sample using chemometrics method
The plain sodium content of ginseng establishes corresponding calibration model, and using the parametric test calibration model, filters out optimal calibration model.
During the foundation of calibration model, using no Pretreated spectra, convolution is smooth, convolution derivation, polynary scattered color correction,
The methods of standard normal variable transformation and its intercombination mode pre-process collected spectrum, and then selection is suitable
Range of wavelengths, with best regression algorithm such as Partial Least Squares (PLS), artificial neural network, support vector machines etc., to various kinds
The characteristic spectrum data of product and the Sodium Danshensu content measured according to standard method are associated, and establish calibration model;Best
Regression algorithm refers to selecting smooth no Pretreated spectra, convolution, convolution derivation, polynary scattered color school for different property models
Just, a kind of method of standard normal variable transformation and its methods of intercombination mode is calculated.
Wherein, near infrared spectrum region, the spectral absorption information of different wave length is for the calibration model finally established
Contributed value is different, at specific wave-length coverage, for specific components absorption intensity be likely less than impurity absorption or
Disturbing factor influences, and is difficult to extract and effectively be extracted to characteristic information.Using chemometrics method especially partially minimum two
Multiplication can be handled full modal data information, but in order to improve the performance of calibration model, improve calculating speed, it should
The wave-length coverage of spectrum is carried out in modeling process preferred.Different-waveband selection method such as all-wave length, correlation can be used in the present invention
Any one in Y-factor method Y, Related Component method, 3 method of iteration optimization 1, iteration optimization 2 or iteration optimization or at least two
Combination spectrum is optimized.
In the present invention, the input, calculating, output of spectroscopic data are realized by computer and its software kit, entire mistake
The journey time is short, speed is fast, accuracy is high.
As a kind of preferred embodiment of the present invention, in step (a), the test sample method of original near infrared spectra collection:
Transmission/transflector measures, and resolution ratio is 1nm or 8cm-1, scanning times 1~64 time, light path 1,2,5,10mm, scanning range:
Wave-length coverage is 800~2500nm.
By acquiring the specific restriction of test sample method to original near infrared spectrum data, sample can be fast and accurately determined
The original near infrared spectrum data of product.
As a kind of preferred embodiment of the present invention, Sodium Danshensu extracting solution elution process includes the following steps:
By Sodium Danshensu extracting solution through macroreticular resin loading absorption after, be rinsed with purified water, from start collect Radix Salviae Miltiorrhizae
While plain sodium efflux, sample collection is carried out to Sodium Danshensu efflux every 1~10min, separation obtains different batches
Sodium Danshensu efflux.
Since Sodium Danshensu extracting solution is soluble easily in water, purified water can be used to elution, at this time obtained Sodium Danshensu stream
Go out liquid and is alternatively referred to as Sodium Danshensu water lotion.Wherein, the typical but non-limiting time interval of sample collection be 1min, 2min,
3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min.
A kind of preferred embodiment as the present invention carries Sodium Danshensu in Sodium Danshensu extracting solution elution process
Liquid is taken to be rinsed with 3BV~15BV purified waters after the absorption of macroreticular resin loading, flow velocity is 3BV/h~15BV/h;
And/or separation, preferably 0.45 μm -0.8 μm of miillpore filter are filtered using miillpore filter, it is further excellent
It is selected as 0.45 μm of miillpore filter.
When being rinsed to macroreticular resin, the dosage of typical but non-limiting purified water is 3BV, 4BV, 5BV, 6BV,
8BV, 10BV, 12BV, 14BV or 15BV.Typical but non-limiting flow velocity be 3BV/h, 4BV/h, 5BV/h, 6BV/h, 8BV/h,
10BV/h, 12BV/h, 14BV/h or 15BV/h.
As a kind of preferred embodiment of the present invention, at room temperature by the Sodium Danshensu efflux of obtained different batches
It is sealed;
And/or Sodium Danshensu extracting solution is extracted by salvia piece and is made.
It is 15-25 DEG C that room temperature, which typically refers to temperature,.
As a kind of preferred embodiment of the present invention, the quick judgement Sodium Danshensu extracting solution macroporous resin adsorption point
Method from elution beginning and end in the process includes the following steps:
(a) foundation of calibration model
In Sodium Danshensu extracting solution elution process, Sodium Danshensu extracting solution is used into 3BV after the absorption of macroreticular resin loading
~15BV purified waters are rinsed, and flow velocity is 3BV/h~15BV/h, and sample is carried out to Sodium Danshensu efflux every 1~10min
Acquisition crosses 0.45 μm of miillpore filter, the Sodium Danshensu efflux for obtaining different batches is sealed;
The Sodium Danshensu efflux for the different batches that Sodium Danshensu extracting solution elution process obtains is chosen as sample, is constituted
Calibration samples collection;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method, meanwhile, using close red
External spectrum instrument concentrates the original near infrared spectrum data of each sample to be acquired calibration samples, the original near infrared light that will be obtained
Modal data is selected by Pretreated spectra and wave-length coverage, the characteristic spectrum data of each sample is obtained, using Chemical Measurement side
Calibration samples are concentrated the characteristic spectrum data of each sample to establish corresponding calibration model with Sodium Danshensu content by method, and using ginseng
Number examines the calibration model, filters out optimal calibration model;
(b) content of Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted using optimal calibration model
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, danshensu to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through optimal correction by the characteristic spectrum data of sodium efflux
Model, which calculates, obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, so judge the elution starting point of elution process with
Terminal.
Pass through the specific limit of the method to quickly judging to elute beginning and end in Radix Salviae Miltiorrhizae macroporous resin adsorption separation process
It is fixed so that the judgment method more rapidly, efficiently, accurately.
According to another aspect of the present invention, it additionally provides one kind and quickly judging Sodium Danshensu extracting solution macroporous resin adsorption
Application of the method for beginning and end in Radix Salviae Miltiorrhizae production is eluted in separation process.
In view of advantage possessed by above-mentioned judgment method so that the quick judgment method has good in Radix Salviae Miltiorrhizae production process
Good application.
With reference to specific embodiment, the invention will be further described.
Embodiment 1
One kind provided in this embodiment quickly judges to elute in Sodium Danshensu extracting solution macroporous resin adsorption separation process
The method of point and terminal, includes the following steps:
(1) feedstock processing:By 300kg red rooted salvias, using physics mode, its medicine materical crude slice is obtained;
(2) process:Salvia piece is required according to actual production, produces and be made Sodium Danshensu extracting solution, it will be red
The plain sodium extracting solution of ginseng is rinsed, flow velocity 6BV/h, every 2min to pellet after the absorption of macroreticular resin loading with 6BV purified waters
The plain sodium efflux of ginseng carries out sample collection, crosses 0.45 μm of miillpore filter, and the Sodium Danshensu efflux for obtaining different batches is sealed
It preserves;
(3) foundation of calibration model:Choose the Sodium Danshensu for the different batches that Sodium Danshensu extracting solution elution process obtains
Efflux constitutes calibration samples collection as sample;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method;
Meanwhile in 800~2500nm of wavelength (wave-length coverage can be replaced according to specific spectrometer) range, utilizing near-infrared
Spectrometer (German Bruker companies Matrix-F near infrared spectrometers, resolution ratio:2nm, scanning times:32 times, scanning optical spectrum model
It encloses:800~2500nm, light path:2mm) in acquisition correction sample set each sample original near infrared spectrum data;
Using no Pretreated spectra, convolution is smooth, convolution derivation, polynary scattered color correction, standard normal variable transformation and its
The methods of intercombination mode pre-processes collected original near infrared spectrum data, then selects suitable wavelength zone
Between, with best regression algorithm such as Partial Least Squares, artificial neural network, support vector machines etc., to obtaining the spy of each sample
Sign spectroscopic data and the data of Sodium Danshensu content are associated, and establish corresponding calibration model, and use parametric test (model
Evaluation parameter SECV, SEC etc.) compare calibration model, filter out optimal calibration model;
(4) content of Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted using optimal calibration model
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, danshensu to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through optimal correction by the characteristic spectrum data of sodium efflux
Model, which calculates, obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, so judge the elution starting point of elution process with
Terminal.
Pass through screening and the wave-length coverage of preprocess method in the original near infrared spectrum data to Sodium Danshensu efflux
Selection when, it should be noted that problems with:
(a) influence of the different preprocessing procedures to calibration model
In the gatherer process of original near infrared spectrum data, using following different preprocessing procedures to spectrum into
Row optimization, is specifically shown in Table 1:
The calibration model parameter of the different preprocessing procedures of table 1
| Serial number | Preprocessing procedures | Main cause subnumber | R2 | SECV |
| 1 | Convolution is smooth | 5 | 0.8251 | 0.1847 |
| 2 | Single order convolution derivation | 3 | 0.8120 | 0.1953 |
| 3 | Second Order Convolution derivation | 6 | 0.8473 | 0.1776 |
| 4 | Multiplicative scatter correction | 6 | 0.8305 | 0.1948 |
| 5 | Standard normal variable converts | 6 | 0.8304 | 0.1951 |
| 6 | Normalization method | 3 | 0.7728 | 0.1973 |
| 7 | Single order convolution derivation+multiplicative scatter correction | 4 | 0.7428 | 0.2473 |
(b) influence of the different wave length selection method to calibration model
Using Tsinghua University's chemometrics application system (THUNIR V3.0) to the preprocess method and wave of different size
The selection of long range carries out matrix form calculating, filters out the optimal preprocessing procedures under a certain Wavelength selecting method,
As shown in table 2.
The calibration model parameter of 2 different wave length range of choice of table
(c) selection of partial least squares regression (PLS) model main cause subnumber
The selection of PLS model main cause subnumbers is directly related to the actual prediction ability of calibration model.In calibration set sample number
In the case that amount is certain, atlas of near infrared spectra, using different main cause subnumbers, can obtain difference in specific wave-length coverage
RMSECV values, optimal RMSECV values are obtained by THUNIR V3.0 Automatic Optimals, to avoid " over-fitting " and " poor fitting "
The generation of phenomenon.
(d) screening of optimal model
By comparing the related coefficient and SECV values under various algorithms in Tables 1 and 2, the considerations such as comprehensive main cause subnumber, most
The optimal model selected eventually establish parameter for:Band selection method is iteration optimization 1, and chosen wavelength range is:833~
1165nm and 1498~1890nm, preprocessing procedures are Second Order Convolution derivation, and main cause subnumber is 6, is returned using PLS
Obtain model to the end, SECV 0.1776, the coefficient of determination 0.8281.
(e) the Sodium Danshensu content in Sodium Danshensu efflux to be measured is predicted with the optimal calibration model after screening
The content that Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted with the optimal calibration model after screening, for be measured
Sodium Danshensu efflux, it is only necessary to take appropriate abjection liquid stoste, scan its original atlas of near infrared spectra, be then input to
Chemometrics application software is calculated by calibration model and obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured.
The predicted value for calculating Sodium Danshensu in each Sodium Danshensu efflux to be measured, predicted value and measured value are compared,
As shown in table 3.
3 near-infrared model of table collects prediction result to verification
The predicted value and actual value of initial 8 samples and final 8 samples is opposite it can be seen from the data in table 3
Deviation is more than 10%, and the relative deviation of remaining sample is all smaller.In conjunction with Fig. 1 as can be seen that from left number, the 9th point is to elute
Starting point, from right number, the 9th point is the terminal eluted.
Embodiment 2
One kind provided in this embodiment quickly judges to elute in Sodium Danshensu extracting solution macroporous resin adsorption separation process
The method of point and terminal, includes the following steps:
(1) feedstock processing:By 300kg red rooted salvias, using physics mode, its medicine materical crude slice is obtained;
(2) process:Salvia piece is required according to actual production, produces and be made Sodium Danshensu extracting solution, it will be red
The plain sodium extracting solution of ginseng is rinsed, flow velocity 12BV/h, every 8min couples after the absorption of macroreticular resin loading with 12BV purified waters
Sodium Danshensu efflux carries out sample collection, crosses 0.45 μm of miillpore filter, and the Sodium Danshensu outflow for obtaining different batches is liquid-tight
Envelope preserves;
(3) foundation of calibration model:Choose the Sodium Danshensu for the different batches that Sodium Danshensu extracting solution elution process obtains
Efflux constitutes calibration samples collection as sample;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method;
Meanwhile in 800~2500nm of wavelength (wave-length coverage can be replaced according to specific spectrometer) range, utilizing near-infrared
Spectrometer (German Bruker companies Matrix-F near infrared spectrometers, resolution ratio:2nm, scanning times:32 times, scanning optical spectrum model
It encloses:800~2500nm, light path:2mm) in acquisition correction sample set each sample original near infrared spectrum data;
Using no Pretreated spectra, convolution is smooth, convolution derivation, polynary scattered color correction, standard normal variable transformation and its
The methods of intercombination mode pre-processes collected original near infrared spectrum data, then selects suitable wavelength zone
Between, with best regression algorithm such as Partial Least Squares, artificial neural network, support vector machines etc., to obtaining the spy of each sample
Sign spectroscopic data and the data of Sodium Danshensu content are associated, and establish corresponding calibration model, and use parametric test (model
Evaluation parameter SECV, SEC etc.) compare calibration model, filter out optimal calibration model;
(4) content of Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted using optimal calibration model
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, danshensu to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through optimal correction by the characteristic spectrum data of sodium efflux
Model, which calculates, obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, so judge the elution starting point of elution process with
Terminal.
It should be noted that in the sieve for passing through preprocess method to the original near infrared spectrum data of Sodium Danshensu efflux
When choosing and the selection of wave-length coverage, it should be noted that problems with:
(a) influence of the different preprocessing procedures to calibration model
In the gatherer process of original near infrared spectrum data, using following different preprocessing procedures to spectrum into
Row optimization, is specifically shown in Table 4:
The calibration model parameter of the different preprocessing procedures of table 4
| Serial number | Preprocessing procedures | Main cause subnumber | R2 | SECV |
| 1 | Convolution is smooth | 5 | 0.8251 | 0.1847 |
| 2 | Single order convolution derivation | 3 | 0.8120 | 0.1953 |
| 3 | Second Order Convolution derivation | 6 | 0.8473 | 0.1776 |
| 4 | Multiplicative scatter correction | 6 | 0.8305 | 0.1948 |
| 5 | Standard normal variable converts | 6 | 0.8304 | 0.1951 |
| 6 | Normalization method | 3 | 0.7728 | 0.1973 |
| 7 | Single order convolution derivation+multiplicative scatter correction | 4 | 0.7428 | 0.2473 |
(b) influence of the different wave length selection method to calibration model
Using Tsinghua University's chemometrics application system (THUNIR V3.0) to the preprocess method and wave of different size
The selection of long range carries out matrix form calculating, filters out the optimal preprocessing procedures under a certain Wavelength selecting method,
As shown in table 5.
The calibration model parameter of 5 different wave length range of choice of table
(c) selection of partial least squares regression (PLS) model main cause subnumber
The selection of PLS model main cause subnumbers is directly related to the actual prediction ability of calibration model.In calibration set sample number
In the case that amount is certain, atlas of near infrared spectra, using different main cause subnumbers, can obtain difference in specific wave-length coverage
RMSECV values, optimal RMSECV values are obtained by THUNIR V3.0 Automatic Optimals, to avoid " over-fitting " and " poor fitting "
The generation of phenomenon.
(d) screening of optimal model
By comparing the RMSECV values and SEC values under various algorithms in table 4 and table 5, the considerations such as comprehensive main cause subnumber, finally
The optimal model selected establish parameter for:Waveband selection is ranging from:833~1165nm and 1498~1890nm, spectrum are pre-
Processing method is Second Order Convolution derivation, and main cause subnumber is 6, using PLS return model, SECV are to the end
0.1776, the coefficient of determination 0.8281.
(e) the Sodium Danshensu content in Sodium Danshensu efflux to be measured is predicted with the optimal calibration model after screening
The content that Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted with the optimal calibration model after screening, for be measured
Sodium Danshensu efflux, it is only necessary to take appropriate efflux stoste, scan its original atlas of near infrared spectra, be then input to
Chemometrics application software is calculated by calibration model and obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured.
The predicted value for calculating Sodium Danshensu in each Sodium Danshensu efflux to be measured, predicted value and measured value are compared,
As shown in table 6.
6 near-infrared model of table collects prediction result to verification
The predicted value and actual value of initial 8 samples and final 8 samples is opposite it can be seen from the data in table 6
Deviation is more than 10%, and the relative deviation of remaining sample is all smaller.In conjunction with Fig. 2 as can be seen that from left number, the 9th point is to elute
Starting point, from right number, the 9th point is the terminal eluted.
In conclusion the present invention establishes during quickly judging Sodium Danshensu extracting solution macroporous resin adsorption separation phase
The method that water-wash section elutes starting point and elutes terminal.The result shows that the near infrared spectrum established judges that column chromatography elutes
The analysis method of point and terminal is suitable in the big production of Radix Salviae Miltiorrhizae.Judgment method provided by the invention is advanced, science, finding speed
It soon, can be to carrying out the judgement of elution beginning and end, Sodium Danshensu in Accurate Prediction efflux in Sodium Danshensu elution process
Content, it can be ensured that drug quality and production efficiency, and testing cost is low.Compared with the conventional method through reality, minute
It shortens dramatically, usually each sample is completed within 1min, and accuracy of detection also approaches standard method, is Chinese Traditional Medicine
A big innovation on active constituent content measuring, has huge economic and social benefit.
Finally it should be noted that:The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that:Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement;And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of method that beginning and end is eluted in quick judgement Sodium Danshensu extracting solution macroporous resin adsorption separation process,
It is characterized in that, includes the following steps:
(a) foundation of calibration model
Choose the Sodium Danshensu efflux conduct for the different batches that Sodium Danshensu extracting solution is obtained using macroreticular resin elution process
Sample constitutes calibration samples collection;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method, meanwhile, and to calibration samples
It concentrates the original near infrared spectrum data of each sample to be acquired, handle, the characteristic spectrum data of each sample is obtained, using chemistry
Calibration samples are concentrated the characteristic spectrum data of each sample to establish corresponding calibration model with Sodium Danshensu content by metrology method;
(b) calibration model is used to predict the content of Sodium Danshensu in Sodium Danshensu efflux to be measured
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, Sodium Danshensu stream to be measured is obtained
Characteristic spectrum data are input to chemometrics application software by the characteristic spectrum data for going out liquid, are by calibration model calculating
The content of Sodium Danshensu in Sodium Danshensu efflux to be measured is obtained, and then judges the elution beginning and end of elution process.
2. according to the method described in claim 1, it is characterized in that, in step (a), in the spy that calibration samples are concentrated to each sample
Further include using parametric test and filtering out optimal after sign spectroscopic data establishes corresponding calibration model with Sodium Danshensu content
Calibration model the step of.
3. according to the method described in claim 1, it is characterized in that, in step (a), using near infrared spectrometer to calibration samples
It concentrates the original near infrared spectrum data of each sample to be acquired, obtained original near infrared spectrum data is located in advance by spectrum
Reason and wave-length coverage selection, obtain the characteristic spectrum data of each sample, are concentrated calibration samples respectively using chemometrics method
The characteristic spectrum data of sample establish corresponding calibration model with Sodium Danshensu content, and use the parametric test calibration model,
Filter out optimal calibration model.
4. according to the method described in claim 1, it is characterized in that, in step (a), using near infrared spectrometer to calibration samples
The original near infrared spectrum data of each sample is concentrated to be acquired, each Sample Scan is primary, soft using chemometrics application
Part is pre-processed to original near infrared spectrum data and wavelength band selection, and it is dry to remove background interference, spectral drift and other noises
It disturbs, obtains the characteristic spectrum data of each sample, calibration samples are concentrated to the characteristic spectrum number of sample using chemometrics method
Corresponding calibration model is established according to Sodium Danshensu content, and using the parametric test calibration model, filters out optimal correction
Model.
5. according to the method described in claim 1, it is characterized in that, in step (a), the test sample side of original near infrared spectra collection
Method:Transmission/transflector measures, and resolution ratio is 1nm or 8cm-1, scanning times 1~64 time, light path 1,2,5,10mm, scanning model
It encloses:Wave-length coverage is 800~2500nm.
6. according to the method described in claim 1-5 any one, which is characterized in that Sodium Danshensu extracting solution elution process includes
Following steps:
By Sodium Danshensu extracting solution through macroreticular resin loading absorption after, be rinsed with purified water, from start collect Sodium Danshensu
While efflux, sample collection is carried out to Sodium Danshensu efflux every 1~10min, separation obtains the Radix Salviae Miltiorrhizae of different batches
Plain sodium efflux.
7. according to the method described in claim 1-5 any one, which is characterized in that in Sodium Danshensu extracting solution elution process
In, Sodium Danshensu extracting solution is rinsed after the absorption of macroreticular resin loading with 3BV~15BV purified waters, flow velocity 3BV/h
~15BV/h;
And/or separation, preferably 0.45 μm -0.8 μm of miillpore filter are filtered using miillpore filter, further preferably
0.45 μm of miillpore filter.
8. according to the method described in claim 1-5 any one, which is characterized in that by the Sodium Danshensu of obtained different batches
Efflux is sealed at room temperature;
And/or Sodium Danshensu extracting solution is extracted by salvia piece and is made.
9. according to the method described in claim 1-5 any one, which is characterized in that include the following steps:
(a) foundation of calibration model
In Sodium Danshensu extracting solution elution process, by Sodium Danshensu extracting solution through macroreticular resin loading absorption after with 3BV~
15BV purified waters are rinsed, and flow velocity is 3BV/h~15BV/h, and carrying out sample to Sodium Danshensu efflux every 1~10min adopts
Collection crosses 0.45 μm of miillpore filter, the Sodium Danshensu efflux for obtaining different batches is sealed;
The Sodium Danshensu efflux for the different batches that Sodium Danshensu extracting solution elution process obtains is chosen as sample, constitutes correction
Sample set;
The Sodium Danshensu content of each sample is concentrated to be measured calibration samples according to standard method, meanwhile, utilize near infrared light
Spectrometer concentrates the original near infrared spectrum data of each sample to be acquired calibration samples, the original near infrared spectrum number that will be obtained
It is selected according to by Pretreated spectra and wave-length coverage, obtains the characteristic spectrum data of each sample, it will using chemometrics method
Calibration samples concentrate the characteristic spectrum data of each sample to establish corresponding calibration model with Sodium Danshensu content, and are examined using parameter
The calibration model is tested, optimal calibration model is filtered out;
(b) content of Sodium Danshensu in Sodium Danshensu efflux to be measured is predicted using optimal calibration model
The original near infrared spectrum data of Sodium Danshensu efflux to be measured is acquired, is handled, Sodium Danshensu stream to be measured is obtained
Characteristic spectrum data are input to chemometrics application software, pass through optimal calibration model by the characteristic spectrum data for going out liquid
It calculates and obtains the content of Sodium Danshensu in Sodium Danshensu efflux to be measured, and then judge elution starting point and the end of elution process
Point.
10. in quick judgement Sodium Danshensu extracting solution macroporous resin adsorption separation process described in any one of claim 1-9
Elute application of the method for beginning and end in Radix Salviae Miltiorrhizae production.
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