CN103335960A - Rapid detection method of key indicators in cinobufagin extraction and concentration processes - Google Patents
Rapid detection method of key indicators in cinobufagin extraction and concentration processes Download PDFInfo
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- CN103335960A CN103335960A CN2013102206362A CN201310220636A CN103335960A CN 103335960 A CN103335960 A CN 103335960A CN 2013102206362 A CN2013102206362 A CN 2013102206362A CN 201310220636 A CN201310220636 A CN 201310220636A CN 103335960 A CN103335960 A CN 103335960A
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Abstract
The invention relates to a rapid detection method of key indicators in cinobufagin extraction and concentration processes. The rapid detection method comprises the following steps of: (1) collecting cinobufagin extracting concentrates obtained in the extraction and concentration processes in different batches as calibration set samples; (2) respectively determining the key indicators of concentrate samples by adopting a conventional analysis method, including the indole alkaloids concentration, moisture content and density; (3) collecting near infrared spectrograms of the calibration set samples; (4) selecting an appropriate spectrum band and a pre-processing method to obtain spectrum information of cinobufagin concentrate characteristics, and establishing calibration models between the near infrared spectrums and the corresponding key indicators; (5) collecting near infrared spectrograms under the same conditions by taking the concentrate samples with the known key indicator values as a validation set, and leading the collected near infrared spectrograms in the established calibration models, wherein the requirement on the measurement error value is less than 20%; (6) leading near infrared spectrum data of unknown samples into the established calibration models to obtain forecasting information of all the key indicators.
Description
Technical field
The invention belongs near infrared fast detecting field, be specifically related to the method for quick that a kind of cinobufagin extracts the concentration process key index.
Background technology
Cinobufagin injection is the sterile water solution that dry maxima skin is made through extraction, effect with detumescence, pain relieving, detoxifcation, be mainly used in the treatment in, late tumor, diseases such as chronic hepatitis B can also be broadcast type pulmonary tuberculosis, Hemorrhagic fever, intractable hiccup and children's for acute blood and flow diseases such as the concurrent meningitis of the cheek.Because cinobufagin injection has the good anticancer effect, be listed in national basic medical insurance medicine Class A and national Chinese medicine protection kind at present.
The technological process of production of cinobufagin injection by extract, concentrate, a plurality of technologies such as alcohol precipitation form.Concentration process is one of important procedure of producing of Chinese medicine, is the workshop section of not only having consumed energy but also being difficult to realize quality control in the herbal pharmaceutical production run.Conventional Concentrating Process Control lacks on-line monitoring method fast and effectively based on empirical method, and the uncontrollability that striking point is determined becomes the inhomogenous important factor in order of traditional Chinese medicine quality, directly influences follow-up refining or dry run.Therefore to improve the tcm product quality, press for the On-line Control that realizes the Chinese medicine concentration process.In concentration process, parameters such as density, solvent and effective constituent concentration are the crucial evaluation indexes of concentration process quality.Concentrating back medicinal extract density is the follow-up refining or key factor of dry run of influence, also is the important indicator that commercial production is passed judgment on the medicinal extract quality.Solvent content affects solvent residual in the final products.Effective constituent keeps height directly influences drug effect.Therefore, research can realize the on-line monitoring method of these parameters simultaneously, thereby realizes the FEEDBACK CONTROL to technological parameter, will optimize concentration technology to a great extent, thereby improve the Chinese patent drug product quality.
Near-infrared spectrum technique has been successfully applied to different analysis fields as a kind of process analysis technique fast, as food, medicine, oil etc.Being extensive use of of near infrared technology mainly have benefited from its have express-analysis, sample preparation simple, need not to consume characteristics such as reagent, be a kind of green analytical technology of quick nondestructive.In recent years, near infrared technology more and more has been applied to traditional Chinese medicine research, comprises online detection and the monitoring of the discriminating of the medicinal material place of production, active principle assay and pharmacy procedure.It seems that from progress situation in recent years near-infrared spectral analysis technology is to be hopeful one of process analysis technique that realizes in the Chinese medicine production run online detection and quality control most.
The present invention is incorporated into the concentration process that Chinese medicine is produced with near-infrared spectral analysis technology, and extracting concentration process with cinobufagin is example, realizes cinobufagin is extracted the quick mensuration of indoles alkaloid concentration, water percentage and density in the concentration process.The present invention is conducive to improve the quality control level that cinobufagin extracts concentration process, fully guarantees constant product quality, reliable.
Summary of the invention
The object of the present invention is to provide a kind of cinobufagin to extract the method for quick of concentration process key index, can solve the difficult point that cinobufagin extracts concentration process key index fast quantification effectively, with the accurate control of raising process unit, thereby guarantee end product quality.
The objective of the invention is to be achieved through the following technical solutions:
1. the collection of calibration set sample
Collect the different batches cinobufagin and extract the concentrate sample that obtains in the concentration process, the sample number is no less than 50 parts.
2. the mensuration of each key index of calibration set sample
Use ultraviolet-spectrophotometric method, weight method and oven drying method respectively, be respectively applied to measure indoles alkaloid concentration in the concentrate sample (in the serotonin hydrochloride), density and water percentage.
3. the calibration set sample spectral data is gathered
Use transmission beam method to gather near infrared spectrum, wavelength band is 4000 ~ 10000 cm
-1, scanning times is 32 times, resolution is 8 cm
-1Each sample is made 3 parallel sweeps, is averaged spectroscopic data as the near infrared spectrum data of sample.
4. the foundation of calibration model
Use the Chemical Measurement software data processing, adopt partial least square method (PLS) to set up the near infrared Quantitative Analysis Model of each key index of concentrate sample.Before model is set up to original near infrared spectrum carry out smoothly, appropriate pretreatment such as differential is in order to eliminate instrumental background or to drift about to the influence of signal.Select suitable spectral band in order to extract effective information, reduce calculated amount, shorten the modeling time.
5. the checking of calibration model
Get the concentrate sample of known key index value, as the checking collection, gather the near infrared light spectrogram under the same conditions, import the calibration model of having built, the requirement forecast error amount is less than 20%.
6. the quick mensuration of each key index of unknown sample
The near infrared light spectrogram of scanning unknown sample is input to spectroscopic data in the calibration model, through calculating the information that can learn each key index in the unknown sample.
The near-infrared spectrum technique that the present invention adopts is measured the method that cinobufagin extracts each key index of concentration process fast, and is easy, accurate, quick.Compare with traditional analytical approach, minute foreshortened to 20 seconds by original 40 minutes even 8 hours, and did not need sample is carried out pre-service, had saved manpower and materials.The present invention is expected to solve cinobufagin and extracts traditional offline inspection cost height, length consuming time, an inefficient difficult problem in the concentration process, reduces final products batch differences, for the quality of cinobufagin injection and related preparations thereof provides safeguard.
Description of drawings
The present invention is further described below in conjunction with accompanying drawing and embodiment.
Accompanying drawing 1 is that cinobufagin extracts concentration process sampling sketch (single-action concentrates)
Accompanying drawing 2 is concentration process indoles alkaloid concentration change dynamic curves
Accompanying drawing 3 is that the concentration process water percentage changes dynamic curve
Accompanying drawing 4 is concentration process variable density dynamic curves
Accompanying drawing 5 is original near infrared spectrums of calibration set sample
Accompanying drawing 6 is calibration set sample near infrared original spectrum first order derivative processing figure
Accompanying drawing 7 is calibration set and the predicted value of checking collection sample and the correlogram (indoles alkaloid) of reference value
Accompanying drawing 9 is calibration set and the predicted value of checking collection sample and the correlogram (density) of reference value
The prediction of accompanying drawing 10 concentration process near infrareds is schemed (indoles alkaloid) with the trend contrast of reference value
The prediction of accompanying drawing 11 concentration process near infrareds is schemed (water percentage) with the trend contrast of reference value
The prediction of accompanying drawing 12 concentration process near infrareds is schemed (density) with the trend contrast of reference value.
Embodiment
Be described further below in conjunction with accompanying drawing and embodiment, but the present invention is not limited to this.
Embodiment
1. the collection of calibration set sample
Toad skin medicinal material adds the immersion of 8 times of amount purified water and decocted 1 hour after 1 hour, and the dregs of a decoction add 4 times of amount purified water, decoct 45 minutes, merge extracted twice liquid.The cinobufagin extract imported the single-action concentration tank fully and arrive suitable thickening temperature and during pressure (0.04-0.08 Mpa) as timing zero point, every sampling in ten minutes.Eliminate the influence of vacuum to obtain concentrated sample, referring to Fig. 1 by the folding of two hand valves (connecting pipe between heating chamber and vaporization chamber) up and down.Hand valve 1 and hand valve 2 are in closed condition simultaneously in the concentration process.Open earlier during sampling the hand valve after 1, ten second concentrate fill full liquid storage pipe, open hand valve 2 when closing hand valve 1, gather the concentrate sample.Concentrated production run is striking point with the relative density arrival 1.1-1.2 of concentrate, and thickening temperature remains on 60 ℃-80 ℃.Repeat five times concentration process, obtain 54 samples altogether, participate in modeling as the calibration set sample.
2. the mensuration of each key index of calibration set sample
1) indoles alkaloid (in the serotonin hydrochloride) concentration determination
Precision takes by weighing serotonin hydrochloride reference substance 15 mg, puts in the 100 mL measuring bottles, and the water dissolving also is diluted to scale, shakes up, and precision is measured 15 mL, puts in the 50 mL measuring bottles, adds water to scale, shakes up, namely.Precision is measured reference substance solution 1.0,2.0,3.0,4.0,5.0 mL, putting 10 mL respectively puts in the bottle, add 15% paradime thylaminobenzaldehyde hydrochloric acid (2 → 3) solution, 5 mL, add water to scale and shake up, room temperature was placed 35 minutes, according to spectrophotometric method (appendix VB), being blank with water, measuring absorbance log at the wavelength place of 555 nm, is ordinate with the absorbance log, concentration is horizontal ordinate, the drawing standard curve map.Precision is measured concentrate 1 mL, dilution, draw 5 mL, put in the 10 mL measuring bottles, by " preparation of a typical curve " method of stipulating down, rise from " adding 15% paradime thylaminobenzaldehyde hydrochloric acid (2 → 3) solution ... ", measure absorbance log in accordance with the law, from the amount that typical curve is read serotonin hydrochloride the need testing solution, calculate, namely.
2) density and measurement of water-content coefficient
Precision pipettes 5 mL(v from every increment basis) solution, weigh (m), by formula ρ=m/v calculates, and should be worth as the sample rate value.
Claim to dry surely flat bottle (weight is less than 5 mg after the twice oven dry) X0 to constant weight, measure concentrate 3 mL to the flat bottle, the X1 that weighs, water bath method, 105 ℃ were dried by the fire 8 hours, took out and put cooling 30 min in the exsiccator, and X2 weighs rapidly.
Water percentage=(X2-X1)/(X1-X0)
Indoles alkaloid concentration, water percentage and the density value of the calibration set sample that records is respectively referring to Fig. 2, Fig. 3 and Fig. 4.
3. the calibration set sample spectral data is gathered
Use the near-infrared transmission spectrogram of ANTARIS ft-nir spectrometer (U.S. Thermo Nicolet company) acquisition correction collection sample, wavelength band is 4000 ~ 10000 cm
-1, scanning times is 32 times, resolution is 8 cm
-1Each sample is made 3 parallel sweeps, is averaged spectroscopic data as the near infrared spectrum data of sample.The original near infrared light spectrogram of calibration set sample is referring to Fig. 5.
4. the foundation of calibration model
Before setting up calibration model, use Chemical Measurement software (U.S. Thermo Nicolet company's T Q Analyst software) to optimize spectral band and preprocess method, and handle raw data to extract spectral signature information with this wavelength band and preprocess method.Utilize partial least square method (PLS) to set up the near infrared Quantitative Analysis Model of each key index in the concentrate sample, adopt and stay a cross validation method to carry out internal verification.
(1) optimum band selection
Remove absorbance log when selecting spectral band and be higher than 1.5 SPECTRAL REGION.In addition, concentrate is at 9000-10000 cm
-1Significantly do not absorb, removed equally.Absorbance log according to the spectroscopic data after the first order derivative processing changes, and adopts 5500-6500 cm
-1With 8500-9000 cm
-1These two wave bands are set up quantitative model, referring to Fig. 6.
(2) optimum preprocessing procedures is selected
Select 5500-6500 cm
-1With 8500-9000 cm
-1The near infrared spectrum data of these two wave bands, adopt first order derivative, second derivative respectively, Savitzky-Golay is level and smooth, Norris is level and smooth and the near infrared raw data of this wave band of average centralization disposal methods, and set up the quantitative model of each key index with the PLS method, poor according to RMSECV(cross validation error mean square), R(calibration set related coefficient) and main Composition Factor count the judgment models performance, see Table 2.The result shows, for the indoles alkaloid model, the model performance that adopts original spectrum, Savitzky-Golay smoothing processing and " Savitzky-Golay level and smooth+average center processing " to build is suitable; For water percentage and density model, the model performance that uses " Savitzky-Golay level and smooth+average center processing " to build obviously is better than other preprocess methods.According to the RMSECV value, three models all select " Savitzky-Golay level and smooth+average center processing " as the preprocess method of spectroscopic data.
The different preprocessing procedures of table 1 are to the influence of each parameter of PLS calibration model
(3) foundation of calibration model
According to above preferred result, select 5500-6500 cm
-1With 8500-9000 cm
-1These two wave bands and " Savitzky-Golay level and smooth+average center processing " method are set up the near infrared correction of cinobufagin extraction concentration process indoles alkaloid, water percentage and density with the PLS method.
5. the checking of calibration model
Get 11 parts of concentrate samples of known key index value, as the checking collection, press the calibration set identical parameters and gather the near infrared light spectrogram, import the calibration model of having built, calculate each key index predicted value of checking collection sample.The near infrared predicted value of three models and the correlogram of classic method assay value are respectively referring to Fig. 7, Fig. 8 and Fig. 9.Correlativity is good between concentrate near infrared characteristic spectrum and each key index, and prediction error value is all less than 17%.
6. the quick mensuration of each key index of unknown sample
Repeating cinobufagin extracts concentration process and obtains new unknown concentrate sample, obtain near-infrared transmission spectrum according to step 3 in the present embodiment, spectroscopic data is directed into the calibration model of setting up in the step 4 in the present embodiment respectively, calculates the predicted value of each key index in the sample solution.Adopt step 2 in the present embodiment to record the reference value of each key index of unknown sample then.The near infrared predicted value of the indoles alkaloid of unknown sample, water percentage and density and reference value are respectively referring to Figure 10, Figure 11 and Figure 12.Match is good between model predication value and the reference value as seen from the figure, and three models all have good estimated performance.
The present invention proposes the near infrared method for quick that cinobufagin extracts indoles alkaloid, water percentage and density in the concentration process, result of study shows, set up PLS quantitative correction model by chemometrics method, near-infrared spectral analysis technology can carry out express-analysis to each key index in the concentrate.This method saves time, harmless, enhance productivity, reflection concentration process composition changes, for the quality control of tcm manufacturing process provides new method.
Claims (8)
1. the method for quick of a cinobufagin extraction concentration process key index is characterized in that, realizes by following steps:
(1) collects the cinobufagin that obtains in the different batches concentration process and extract concentrate as the calibration set sample;
(2) adopt the traditional analysis method to measure the key index of concentrate sample respectively, comprise indoles alkaloid concentration, water percentage and density;
(3) the near infrared light spectrogram of acquisition correction collection sample;
(4) select suitable spectral band and preprocess method to obtain cinobufagin and extract concentrate characteristic spectrum information, set up the calibration model between near infrared spectrum and each key index;
(5) get the concentrate sample of known key index value, as the checking collection, gather the near infrared light spectrogram under the same conditions, import the calibration model of having built, require measurement error value less than 20%;
(6) near infrared spectrum data with unknown sample imports the calibration model of having built, obtains the information of forecasting of each key index.
2. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that: the cinobufagin of calibration set sample collection extracts concentration process and is: toad skin medicinal material adds the immersion of 8 times of amount purified water and decocted 1 hour after 1 hour, the dregs of a decoction add 4 times of amount purified water, decocted 45 minutes, twice decoction all carried out under 100 ℃ of conditions, merges extracted twice liquid; The cinobufagin extract imported the single-action concentration tank fully and arrive suitable thickening temperature and during pressure (0.04-0.08 Mpa) as timing zero point, every sampling in ten minutes; Concentrated production run is striking point with the relative density arrival 1.1-1.2 of concentrate; Thickening temperature remains on 60 ℃-80 ℃.
3. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that: eliminate the influence of vacuum to obtain the concentrate sample by the folding of two hand valves (connecting pipe between heating chamber and vaporization chamber) up and down; Hand valve 1 and hand valve 2 are in closed condition simultaneously in the concentration process; Open earlier during sampling the hand valve after 1, ten second concentrate fill full liquid storage pipe, open hand valve 2 when closing hand valve 1, gather the concentrate sample.
4. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that: described traditional analysis method comprises ultraviolet-spectrophotometric method, weight method and oven drying method, is respectively applied to measure indoles alkaloid concentration in the concentrate sample (in the serotonin hydrochloride), water percentage and density.
5. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that: use transmission beam method to gather near infrared spectrum, wavelength band is 4000 ~ 10000 cm
-1, scanning times is 32 times, resolution is 8 cm
-1Each sample is made 3 parallel sweeps, is averaged spectroscopic data as the near infrared spectrum data of sample.
6. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that: remove absorbance log when selecting spectral band and be higher than 1.5 SPECTRAL REGION; In addition, concentrate is at 9000-10000 cm
-1Significantly do not absorb, removed equally; Therefore adopt 5500-6500 cm
-1With 8500-9000 cm
-1These two wave bands are set up quantitative model.
7. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that described preprocessing procedures comprises: one-level derivative method, secondary derivative method, Norris convolution smoothing method, Savitzky-Golay convolution smoothing method, average centralization method etc.
8. a kind of cinobufagin according to claim 1 extracts the method for quick of concentration process key index, it is characterized in that: the partial least square method in the utilization Chemical Measurement software is set up the Quantitative Analysis Model of each key index in the concentrate sample.
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Application publication date: 20131002 |