CN103808665A - Method for determining content of multi-index components in purification process of Chinese buckeye seed extractive - Google Patents
Method for determining content of multi-index components in purification process of Chinese buckeye seed extractive Download PDFInfo
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- CN103808665A CN103808665A CN201310516594.7A CN201310516594A CN103808665A CN 103808665 A CN103808665 A CN 103808665A CN 201310516594 A CN201310516594 A CN 201310516594A CN 103808665 A CN103808665 A CN 103808665A
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- near infrared
- sodium aescinate
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Abstract
The invention discloses a method for rapidly determining the content of multi-index components in a sample feeding and eluting process of a Chinese buckeye seed extractive, namely sodium aescinate, in macro-porous resin and rapidly judging an eluting terminal point. The method comprises the following steps: (1) scanning near infrared spectrums and collecting a macro-porous effluent liquid sample; (2) determining the content of the multi-index components in a sample by using a reference method; (3) establishing a near-infrared multi-element correction model in a macro-porous purification process; (4) carrying out model evaluation; and (5) rapidly judging the eluting terminal point. The method provided by the invention has the advantages of rapidness, no loss, capability of simultaneously detecting a plurality of components and the like, can be used for an online analysis of a traditional Chinese medicine production process, and provides a novel thought for production and quality control of traditional Chinese medicines.
Description
Technical field
The invention belongs to the quality determining method of Chinese Traditional Medicine, relate to the detection method of multi-target ingredient content in a kind of Near Infrared Spectroscopy for Rapid Horse chest Nut P.E macroporous resin purification process.
Background technology
In recent years, safety of Chinese medicine injection event takes place frequently, and the quantity of bad reaction report also increases to some extent.The reason such as unstable and manual operation difference of operating mode in traditional Chinese medicine production run, usually cause traditional Chinese medicine quality unstable, Product Safety cannot be guaranteed, therefore the quality testing of, strengthening traditional Chinese medicine production run to improve traditional Chinese medicine security, ensure that patient's vital interests are significant.
Aescin for injection can be used for the treatment of the swelling causing after encephaledema wound and operation, and also for venous return obstacle disease, its crude drug is the dry mature fruit (buckeye) of Hippocastanaceae plant Aesculus.Buckeye complex chemical composition, comprises saponins, flavonoids, Coumarins, organic acid, phytosterin compound and other amino acid etc., and main pharmacodynamics composition is α-Sodium Aescinate and beta-aescin sodium.Pharmacological research shows, Sodium Aescinate has very strong anti-inflammatory, the impervious effect that goes out, eliminates swelling and increase intravenous tension and promote lymphatic return.Sodium Aescinate is as the main pharmacodynamics composition of buckeye, and its content has larger impact to final products drug effect, and macroporous resin purification technique is the critical process that affects otoginsenoside sodium content.In addition, due on Sodium Aescinate with two glycosyls, due to the fluctuation of technique, may bring glycosidic bond fracture and sugared generation, the variation that detects sugared content in macroporous resin purification process contributes to understand product quality variation.Solid content also to a certain extent can significant reaction Chinese Traditional Medicine mass change.Therefore, in macroporous resin purification technique, the online detection of multi-target ingredient content is very necessary for aescin for injection constant product quality Journal of Sex Research.
At present, traditional assay method is as HPLC, sample preparation process complexity, and complex operation and analysis time are long, are difficult to realize online detection.Near-infrared spectral analysis technology is a kind of modern analytical technique of quick nondestructive, its integrated use the newest research results of multiple subjects such as computer technology, spectral technique and Chemical Measurement, obtained increasingly extensive application with its unique advantage in multiple fields such as petrochemical complex, agricultural food product, tobacco industry and pharmaceuticals industries.Compared with traditional analysis, near-infrared spectrum technique has the features such as express-analysis, sample preparation be simple, and near infrared light has good transport property in optical fiber, therefore can be for the fast detecting of sample, be suitable for very much on-line analysis and the remote monitoring of Chinese Traditional Medicine." a kind of method of measuring content of tannin in red sage root extracting solution by near infrared spectrum " (number of patent application: 201010125515.6) calculate fast content of tannin in red sage root extract by building near infrared spectrum quantitative correction model, can effectively solve content of tannin monitoring problem in red sage root extract, guarantee danshen injections quality.But also rarely near-infrared spectrum technique is applied in the fast detecting of macroporous resin purification process at present, the present invention is applied to near-infrared spectrum technique in the online detection of Sodium Aescinate macroporous resin purification process.Document had been reported the content that adopts Sodium Aescinate A and B in high effective liquid chromatography for measuring aescin for injection; in aescin for injection product, mainly contain Sodium Aescinate A, B, C, D; also contain catabolite and other impurity of a small amount of glycogen, aglycon, deacylated tRNA base; the present invention utilizes near-infrared spectrum technique to monitor Sodium Aescinate A, B, C, D and sugar content and solid content in Sodium Aescinate macroporous resin purification process simultaneously, can evaluate more all sidedly Sodium Aescinate active constituent content.In addition, high performance liquid chromatography length consuming time, each analysis needs 20min, be difficult to reach the effect of Real-Time Monitoring, near infrared can obtain the content results of each index components in 1min, can really accomplish Real-Time Monitoring production run mass change, therefore, otherness between can more effectively reducing batch, contributes to improve stability, security and the validity of product.
In addition, macroreticular resin wash-out terminal is a key point of macroporous resin purification process, and the quick judgement of wash-out terminal can make macroporous resin purification process operation more reasonable, significant to realizing macroreticular resin on-line monitoring.Elution process terminal refers to sampling spot when active constituent content relative concentration rate of change RRCR is tending towards setting threshold.Movable block standard deviation (MBSD method) is a kind of conventional endpoint method, and existing bibliographical information adopts MBSD method to judge fast traditional Chinese medicine extraction terminal, but yet there are no in the quick judgement of using it for macroreticular resin elution process terminal.MBSD method ultimate principle is: when the standard deviation rate of change between the spectral signal gathering several times is continuously less than certain value, can think that oneself is through arriving extraction process terminal.Concrete operation step: be first identified for calculating the continuous spectrum number n of standard deviation, determine and then calculate the standard deviation between the n bar spectrum recording when endpoint starts by movable block window width
then calculate S
imean value
wherein X
ijbe the absorbance of j article of spectrum at wave number i place,
for n bar spectrum in window is at the mean value of the absorbance at wave number i place, m is the wave number sum of choosing.Reject in chronological order that spectrum the earliest in former n bar spectrum, and add next spectrum of last that spectrum, recalculate S
i, S.Repeat successively to reject, add and calculating operation, finally to deviation mean value S mapping, and whether arrive according to the rate of change judgement extraction terminal of S.The present invention in Sodium Aescinate macroporous resin purification process, can realize the quick judgement of wash-out terminal by MBSD method endpoint application of principle.
Summary of the invention
The object of this invention is to provide many indexes component content in a kind of Fast Measurement macroporous resin purification process and judge fast the method for macroreticular resin elution process terminal; This method utilizes Chemical Measurement software to set up the near infrared correction of many indexes component content in macroporous resin purification process, with the multi-target ingredient content in fast prediction purge process, and adopt MBSD method to judge fast macroreticular resin elution process terminal, thereby realize the on-line analysis to macroporous resin purification process, for the quality control of process of producing product lays the foundation.
The object of this programme is to be achieved through the following technical solutions:
(1) collection of macroreticular resin loading and elution process calibration set sample: in macroreticular resin loading and elution process interval 0.5h sampling.
(2) mensuration of calibration set sample multi-target ingredient content reference point:
A) content of total Sodium Aescinate and Sodium Aescinate A, B, C, D in HPLC method mensuration sample;
Chromatographic condition: chromatographic column is Phanomenex, C
18(100mm × 4.6mm, 2.6 μ are m); Mobile phase: A is 0.5% phosphoric acid solution, and B is acetonitrile, gradient elution; Detect wavelength: 220nm; Column temperature: 30 ℃; Flow velocity: 1ml/min.
B) measure the sugar content of efflux in macroreticular resin loading and elution process with compound microcapsule;
C) measure the solid content of efflux in macroreticular resin loading and elution process by weight method;
(3) calibration set sample near infrared spectrum data gathers:
Use near infrared spectrometer scanning calibration set sample, spectral range is 4000～12000cm
-1, obtain calibration set sample near infrared spectrum data.
(4) foundation of calibration model:
Adopt Chemical Measurement software and partial least square method to set up many indexs content Multivariate Correction model in macroporous resin purification process.First calibration set spectrum is carried out to abnormity point differentiation, removes abnormity point, simultaneously to spectroscopic data carry out smoothly, the pre-service such as differential, and select suitable wave band to carry out modeling.Differential can be eliminated baseline wander, and can introduce high frequency noise simultaneously, smoothly can effectively remove the impact of high frequency noise on signal.In addition, band selection can avoid introducing too much redundant information, improves model performance.
(5) evaluation of calibration model:
Adopt the indexs such as coefficient R, cross validation mean square deviation (RMSECV), relative analytical error (RPD) to evaluate respectively the calibration model of set up each index components.
(6) prediction of calibration model:
The near infrared spectrum of scanning forecast set sample, the Fast Measurement by set up calibration model for forecast set sample active constituent content.
(7) the quick judgement of wash-out terminal:
Adopting movable block standard deviation (MBSD method) to carry out wash-out terminal judges fast.
Embodiment
The method of near infrared spectrum fast detecting Sodium Aescinate macroporous resin purification process effective constituent, its detecting step is as follows:
(1) collection of macroreticular resin loading and elution process calibration set sample:
80, sample in collection different batches macroreticular resin loading and elution process
(2) mensuration of calibration set sample multi-target ingredient content reference point
The content of total Sodium Aescinate and Sodium Aescinate A, B, C, D in A.HPLC method mensuration sample:
Chromatographic condition: chromatographic column is Phanomenex, C
18(100mm × 4.6mm, 2.6 μ are m); Mobile phase: A is 0.5% phosphoric acid solution, and B is acetonitrile, carries out gradient elution by table 1; Detect wavelength: 220nm; Column temperature: 30 ℃; Flow velocity: 1ml/min.
Specification Curve of Increasing: precision takes Sodium Aescinate reference substance 124.08mg and is placed in 25mL measuring bottle, using methyl alcohol dissolve and constant volume as storing solution.Storing solution is diluted by gradient, be made into the working fluid of 5 variable concentrations, sample introduction analysis, and record peak area separately.With chromatographic peak area Y, sample introduction concentration X is carried out to linear regression.The regression equation of Sodium Aescinate A is: Y=2225.5X-4.242, R
2=0.9999; The regression equation of Sodium Aescinate B is: Y=1867.7X-17.386, R
2=0.9999, result shows that Sodium Aescinate A is good in 140.5～1123.7 μ g scope internal linear relations at 192.6～1540.6 μ g, Sodium Aescinate B.
Sample determination: the Sample Dilution of obtaining, to corresponding multiple, is carried out to assay according to above-mentioned chromatographic condition.
B. measure the sugar content of efflux in macroreticular resin loading and elution process with compound microcapsule:
Dip 2～3 of sample liquids, drip in the Abbe refractometer prism facets central authorities of having proofreaied and correct, closed prism, leaves standstill 1min.Tune and make terminator clear, and make its separatrix just on the right-angled intersection point of objective lens.Read the sugar content percentage in the eyepiece visual field.
C. measure the solid content of efflux in macroreticular resin loading and elution process by weight method:
Weighed cillin bottle (after twice oven dry, weight is less than 5mg) X of drying to constant weight
0, the about 2mL of sample thief is to flat bottle, and X weighs
1, water bath method, 105 ℃ are dried 18h, take out and put cooling 30min in exsiccator, and X weighs rapidly
2.
Solid content=(X
2-X
0)/(X
1-X
0)
(3) calibration set sample near infrared spectrum data gathers
Use near infrared spectrometer scanning calibration set sample, spectral range is 4000～12000cm
-1, scanning times 32 times, resolution 8cm
-1, obtain calibration set sample near infrared spectrum data.
(4) foundation of calibration model
Adopt Chemical Measurement software and partial least square method to set up many indexs content Multivariate Correction model in Sodium Aescinate macroporous resin purification process.First calibration set spectrum is carried out to abnormity point differentiation, remove abnormity point, select suitable wave band simultaneously, and employing is level and smooth, first order derivative is carried out pre-service to spectroscopic data, then adopts partial least square method to carry out the foundation of quantitative correction model.
(5) evaluation of calibration model
Adopt the indexs such as coefficient R, cross validation mean square deviation (RMSECV), relative analytical error (RPD) to evaluate respectively the calibration model of set up each index components.Macroreticular resin loading and elution process model evaluation result are respectively in table 1 and table 2.
Table 1 macroreticular resin loading process near-infrared model is evaluated
Table 2 macroreticular resin elution process near-infrared model is evaluated
Result shows, the quantitative correction model of the multi-target ingredient that macroporous resin purification process is set up all has higher related coefficient and less RMSECV, and RPD value >3, show that this model performance is good, be applicable to the online detection of Sodium Aescinate macroreticular resin elution process multi-target ingredient.
(6) prediction of calibration model: the near infrared spectrum of scanning forecast set sample, the Fast Measurement by set up calibration model for forecast set sample active constituent content.
(7) the quick judgement of wash-out terminal:
Adopting movable block standard deviation (MBSD method) to carry out wash-out terminal judges fast.Measure the total Sodium Aescinate content of elution process by HPLC method, the wash-out terminal that quick MBSD method judgement is obtained and effective constituent actual content change the wash-out terminal obtaining and contrast.Found that both basically identical, illustrate and adopt MBSD method to judge that fast macroreticular resin wash-out terminal is practicable.
Claims (6)
1. a method for multi-target ingredient content near infrared spectrum quick test Sodium Aescinate macroreticular resin loading and elution process, is characterized in that, realizes by following steps:
(1) collection of calibration set sample: collect 80, different batches Sodium Aescinate macroreticular resin loading and elution process efflux sample;
(2) mensuration of calibration set sample multi-target ingredient content:
A) with total Sodium Aescinate, Sodium Aescinate A, Sodium Aescinate B, Sodium Aescinate C and Sodium Aescinate D content in high effective liquid chromatography for measuring sample;
B) measure sugar content in sample with compound microcapsule;
C) measure solid content in sample by weight method;
(3) near infrared spectra collection of calibration set sample: use near infrared spectrometer scanned samples, obtain near infrared spectrum data;
(4) foundation of calibration model: select suitable spectral band and preprocess method, obtain characteristic spectrum data, use multivariate calibration methods, build the calibration model between the above-mentioned each index component content of calibration set sample and near infrared characteristic spectrum, for the prediction of sample index's property component content;
(5) evaluation of calibration model: adopt the indexs such as coefficient R, cross validation mean square deviation (RMSECV), relative analytical error (RPD) to evaluate respectively the calibration model of set up each index components;
(6) prediction of calibration model: the near infrared spectrum of scanning forecast set sample, the Fast Measurement by set up calibration model for forecast set sample active constituent content;
(7) the quick judgement of wash-out terminal: adopt movable block standard deviation (MBSD method) to carry out wash-out terminal and judge fast.
2. according to the method for multi-target ingredient content in a kind of near infrared spectrum quick test Sodium Aescinate macroreticular resin loading described in claims 1 and elution process, it is characterized in that, adopt total Sodium Aescinate, Sodium Aescinate A, Sodium Aescinate B, Sodium Aescinate C and Sodium Aescinate D, sugar content, solid content as quantitative target.
3. according to the method for multi-target ingredient content in a kind of near infrared spectrum quick test Sodium Aescinate macroreticular resin loading described in claims 1 and elution process, it is characterized in that, near infrared spectra collection mode and condition are: use transmission beam method to gather near infrared spectrum, correlation parameter is: scanning optical spectrum wavelength coverage is 4000～12000cm
-1, scanning times 32 times, resolution 8cm
-1.
4. according to the method for multi-target ingredient content in a kind of near infrared spectrum quick test Sodium Aescinate macroreticular resin loading described in claims 1 and elution process, it is characterized in that, select suitable modeling wave band by wave band optimization, and adopt first order derivative and smoothly near infrared spectrum carried out to pre-service.
5. according to the method for multi-target ingredient content in a kind of near infrared spectrum quick test Sodium Aescinate macroreticular resin loading described in claims 1 and elution process, it is characterized in that, application partial least square method is set up Multivariate Correction model.
6. according to the method for the quick judgement wash-out terminal described in claims 1, it is characterized in that, adopt movable block standard deviation to judge fast wash-out terminal in conjunction with near infrared spectrum.
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| CN107153048A (en) * | 2017-06-12 | 2017-09-12 | 浙江大学 | The near infrared spectrum on-line detecting system and method for a kind of arasaponin column chromatography procedure |
| CN107917895A (en) * | 2017-11-14 | 2018-04-17 | 广州中大南沙科技创新产业园有限公司 | The quality determining method of otoginsenoside C in a kind of buckeye |
| CN107976407A (en) * | 2017-11-14 | 2018-05-01 | 广州中大南沙科技创新产业园有限公司 | The quality determining method of otoginsenoside D in a kind of buckeye |
| CN108008030A (en) * | 2017-11-14 | 2018-05-08 | 广州中大南沙科技创新产业园有限公司 | The quality determining method of Aescinate A in a kind of buckeye |
| CN107655853A (en) * | 2017-11-14 | 2018-02-02 | 广州中大南沙科技创新产业园有限公司 | The quality determining method of Aescinate B in a kind of buckeye |
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