CN105203496A - Near-infrared online detecting method for lame impediment tablet concentration process - Google Patents
Near-infrared online detecting method for lame impediment tablet concentration process Download PDFInfo
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- CN105203496A CN105203496A CN201510609287.2A CN201510609287A CN105203496A CN 105203496 A CN105203496 A CN 105203496A CN 201510609287 A CN201510609287 A CN 201510609287A CN 105203496 A CN105203496 A CN 105203496A
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Abstract
A near-infrared online detecting method for the lame impediment tablet concentration process comprises online detection on water extract concentration in the lame impediment tablet production process, alcohol precipitation supernate concentration and the water extract and alcohol precipitate mixed liquid concentration process. A near-infrared online detecting device is adopted and comprises a first valve, a second valve, a third valve, a fourth valve, a fifth valve, a sixth valve, an evaporation chamber, a heating chamber, a variable frequency pump, a sampling valve, a flow cell, a fiber probe, a near-infrared spectrometer, a branch circuit and a circulation manifold bypass. A transillumination method is adopted in collection of a near-infrared spectrum, the spectral range is 4,000 cm<-1> to 12,000 cm<-1>, and air is adopted as a reference. Online detection of the three concentration processes in lame impediment tablet production is mainly achieved. According to the detecting target of the method, the three concentration processes of lame impediment tablets are monitored in real time, the change conditions of effective ingredients and the solid content in a concentrated solution are fed back in time, then the production process is guided, and product quality stability is guaranteed.
Description
Technical field
The invention belongs near infrared online detection technical field, be specifically related to Costumes numbness sheet 3 concentration process near infrared online detection methods.
Background technology
Costumes numbness sheet is by the compound preparation of 17 kinds of drug matchings such as barrenwort, the root of herbaceous peony, and it is extracted by modern extraction technique, forms through alcohol precipitation, the series of process means compressing tablet such as concentrated.Its effect is filling liver kidney, strengthening the bones and muscles, wines used as antirheumatic, stimulate the menstrual flow network, sees there is above-mentioned disease person etc. for kidney deficiency and liver, for a long time numbness body void, arthralgia, locally enlargement, stiff deformity, joint stuffiness and rheumatoid arthritis.
Concentration process is the key link in Costumes numbness sheet production technology, and fundamental purpose is that the concentration improving effective constituent in liquid reduces medicine liquid volume simultaneously, is beneficial to the refining further of later stage and purifying.Presently, concentration process is mainly by building vacuum environment for liquid, improve temperature to make liquid density reach predetermined value with the evaporation of accelerated solvent to realize simultaneously, in different batches liquid, the fluctuation of active constituent content, total solvent volume all can affect the carrying out of technological process therebetween, otherwise the variation of the key process parameter such as vacuum tightness, temperature also easily causes the quality fluctuation of final concentrate.Now concentration technology quality control mainly relies on experience and conventional mass analysis method (HPLC etc.), time and effort consuming, analysis result is delayed, active constituent content information in concentrate can not be reflected in time, be difficult to Instructing manufacture process, the stable uniform of concentrate quality cannot be guaranteed, and then cause the batch wise differences of product quality.
Near-infrared spectrum analysis is the material information utilizing near infrared spectrum district to comprise, and for a kind of analytical approach of material qualitative and quantitative analysis, having quick, pollution-free, sample does not need pre-service and can detect the advantages such as Multiple components simultaneously.From research in recent years progress, near-infrared spectral analysis technology is hopeful one of process analysis technique realizing on-line checkingi and quality control at Chinese Traditional Medicine most.Control and production application field at traditional Chinese medicine quality, the mensuration that near infrared spectrum is applied to index components as a kind of online measuring technique has Patents document, as patent (CN201410135322.7, CN201410135324.6 and CN200410090617.3) etc.But patent or the document of near infrared online detection Costumes numbness sheet concentration process also do not have report.
Near-infrared spectrum technique is introduced in the concentration technology of Costumes numbness sheet, just can utilize near-infrared spectral analysis technology fast, harmless, without the need to the advantage of sample pretreatment, concentration process is monitored in real time, in timely feedback concentrate, effective constituent and solid content situation of change, ensure product quality stability further.
Summary of the invention
The object of this invention is to provide a kind of Costumes numbness sheet concentration process near infrared online detection method, the method mainly realizes the on-line checkingi of three concentration processs in the production of Costumes numbness sheet.The detection target of the method is monitor Costumes numbness sheet 3 concentration processs in real time, in time effective constituent and solid content situation of change in feedback concentrate, and then Instructing manufacture process, ensures product quality stability.
The present invention is achieved by the following technical solutions:
A kind of Costumes numbness sheet concentration process near infrared online detection method, comprises that aqueous extract in Costumes numbness sheet production run concentrates, the on-line checkingi of alcohol precipitation supernatant concentration and water extract-alcohol precipitation amalgamation liquid concentration process, it is characterized in that:
The checkout equipment adopted is near infrared online detection device.
Near infrared online detection device comprises the first valve 1, second valve 2, the 3rd valve 3, the 4th valve 4, the 5th valve 5, the 6th valve 6, vaporization chamber 7, heating chamber 8, variable frequency pump 11, sample valve 12, flow cell 13, fibre-optical probe 14, near infrared spectrometer 15, branch road 16 and circulation house steward bypass.
Circulation house steward bypass is connected and composed by the first bypass branch 17, second bypass branch 18 and the 3rd bypass branch 19, and the upper end of the first bypass branch 17 is connected with circulation house steward 9, and the first valve 1 is installed in the first bypass branch 17.The lower end of the first bypass branch 17 is connected with the charging aperture of variable frequency pump 11, the discharging opening of variable frequency pump 11 is connected with one end of the second bypass branch 18, second bypass branch 18 is equiped with the 3rd valve 3, the other end of the second bypass branch 18 is connected with the charging aperture of sample valve 12, the discharging opening of sample valve 12 is connected with the charging aperture of flow cell 13 by the first line segments 22 of the 3rd bypass branch 19, the discharging opening of flow cell 13 is connected with the second line segments 10 of the 3rd bypass branch 19, 4th valve 4 and the second valve 2 are installed in the 3rd bypass branch 19, the other end of the 3rd bypass branch 19 is connected with circulation house steward 9.5th valve 5 is installed on arm 20, and one end of arm 20 is connected with the second bypass branch 18, and tie point is positioned on the pipeline in the middle of variable frequency pump 11 and the 3rd valve 3, forms the 5th valve 5 in parallel with the 3rd valve 3 and the 4th valve 4.Flow cell 13 is equiped with fibre-optical probe 14, fibre-optical probe 14 is connected with near infrared spectrometer 15 by optical fiber 21.6th valve is connected with one end of branch road 16, in the second line segments 10 of another termination the 3rd bypass branch 19 of branch road 16.
One end of circulation house steward 9 is connected with the outlet of vaporization chamber 7, and the other end of circulation house steward 9 is connected with the import of heating chamber 8, and the upper end outlet of heating chamber 8 is connected with vaporization chamber 7 by pipeline 23.
Costumes numbness sheet concentration process on-line checkingi, comprises the steps:
Detect and adopt above-mentioned near infrared online detection device, carry out online acquisition and concentrate sample and near infrared spectrum:
1, tank to be concentrated brings into operation, and the first valve 1, second valve 2, the 3rd valve 3, the 4th valve 4 is opened, opens variable frequency pump 11, concentrate is circulated at pipeline.During spectra collection, open the 5th valve 5, close the 3rd valve 3 and the 4th valve 4 simultaneously, gather spectrum; After collection spectrum terminates, open the 6th valve 6, destroy system vacuum environment, sample valve 12 from below samples.
The collection of near infrared spectrum adopts transmission beam method, and spectral range is 4000cm
-1-12000cm
-1, scanning times is 16 times, and resolution is 8cm
-1, take air as reference.
Near infrared spectrum and concentrating sample online acquisition divide 3 stages:
(1), extract enriching stage: 2 and a half hours after from producing, gather near infrared spectrum every 15 minutes online acquisition by the concentrate of flow cell and get concentrating sample simultaneously, gather infrared spectrum every 5 minutes afterwards, get concentrating sample simultaneously;
(2), the alcohol precipitation supernatant concentration stage: every 2 minutes online acquisition by the concentrate near infrared spectrum of flow cell, simultaneously gather concentrating sample sample;
(3) alcohol precipitation amalgamation liquid enriching stage, is extracted: in 2 hours that calculate from producing, every 15 minutes online acquisition concentrate near infrared spectrum by flow cell, gather concentrated sample simultaneously, afterwards every 5 minutes online acquisition concentrate near infrared spectrum by flow cell, gather concentrated sample simultaneously.
(4), traditional chemical analysis method measures each quality control index content in concentrated sample:
A () high effective liquid chromatography for measuring Costumes numbness sheet concentrates Paeoniflorin in sample and Icariin content
Chromatographic condition: chromatographic column is LichrospherC18 (4.6*250mm); Mobile phase A is 0.1% glacial acetic acid mutually, and B phase is acetonitrile; Gradient is set to 0-15min, 15%B; 15-20min, 15%-30%B; 20-35min, 30%B; Determined wavelength is 240nm, and temperature is 25 DEG C, and flow velocity is 1ml/min, and sample size is 10 μ l.
B () oven drying method mensuration Costumes numbness sheet concentrates the solid content in sample
Dry to the measuring cup (after twice oven dry, weight is less than 5mg) of constant weight that weigh X
0; Sample centrifugal (13000rpm) is after 10 minutes, and get supernatant 10ml to flat bottle, weigh X
1, water bath method, 105 DEG C are dried 5 hours, take out to put in exsiccator to cool 30 minutes, and weigh rapidly X
2.
Calculate solid content: SSC (%)=(X
2-X
0)/(X
1-X
0) × 100%
(5), the Establishment and evaluation of near infrared quantitative model
Concentrated 3 concentration processs of, alcohol precipitation supernatant concentration, water extract-alcohol precipitation amalgamation liquid concentrated for Aqueous extracts, each process chooses 10 lot data respectively for modeling, and 1 lot sample is originally used for checking.1. extract enriching stage: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively and deducts straight line, eliminates constant offset and first order derivative; Modeling wave band is respectively 5449.9-6101.8,5449.9-6101.8 and 4601.4-4246.5,5449.9-6101.8cm
-1; 2. the alcohol precipitation supernatant concentration stage: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively without Pretreated spectra, eliminates constant offset, eliminates constant offset; Modeling wave band is respectively 5449.9-6475.9,5773.9-6101.8 and 7498-9403.3,5449.9-6475.9cm
-1; 3. alcohol precipitation amalgamation liquid enriching stage is extracted: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively without Pretreated spectra, vector normalization, second derivative; Modeling wave band is respectively 5449.9-6475.9,5773.9-6101.8,5449.9-6101.8cm
-1.Partial least squares regression (PLSR) is adopted to set up the quantitative calibration models of near infrared spectrum and icariin, Paeoniflorin and solid content.Integrate mean square deviation (RMSEP) and relative deviation (RSEP) as index optimization modeling parameters with related coefficient (R), calibration set mean square deviation (RMSEC), checking, investigation model performance.Close to 1, R more represents that the correlativity between the predicted value of model and standard control methods analyst value is better; The size of RMSEC with RMSEP is relevant to sample chemical value, and these two parameters are more little more close, then show that model performance is better, precision of prediction is higher; According to actual mass control overflow, when RSEP value lower than 20% time, think that the precision of prediction of institute's established model is in tolerance interval.
(6) variation tendency of each quality control index in built model on-line prediction concentration process, is applied
The near infrared spectrum of online acquisition concentrate, uses the correlation model built up to detect the variation tendency of each quality control index in concentration process.
The present invention nearly infrared on line analysis technology is incorporated into 3 concentration processs of Costumes numbness sheet, the quality control index content (Paeoniflorin, icariin and solid content) of Real-Time Monitoring concentrate, be conducive to the quality information feeding back product in time, ensure the consistance of product batches.
Accompanying drawing explanation
Fig. 1 is concentration process near infrared online detection device sketch.
Fig. 2 is the related coefficient figure of extract concentration process each quality control index calibration set measured value and predicted value.
Fig. 3 is that each quality control index measured value of extract concentration process PLSR model on-line analysis contrasts figure with predicted value trend.
Fig. 4 is the related coefficient figure of alcohol precipitation supernatant concentration process each quality control index calibration set measured value and predicted value.
Fig. 5 is that each quality control index measured value of alcohol precipitation supernatant concentration process PLSR model on-line analysis contrasts figure with predicted value trend.
Fig. 6 is the related coefficient figure extracting alcohol precipitation amalgamation liquid concentration process each quality control index calibration set measured value and predicted value.
Fig. 7 extracts each quality control index measured value of alcohol precipitation amalgamation liquid concentration process PLSR model on-line analysis to contrast figure with predicted value trend.
Embodiment
Be described further below in conjunction with drawings and Examples.
Embodiment 1:
A kind of Costumes numbness sheet concentration process near infrared online detection method, the checkout equipment of employing is above-mentioned near infrared online detection device.
Near infrared spectrum and extract concentrate the online acquisition of sample
1, tank to be concentrated brings into operation, and the first valve 1, second valve 2, the 3rd valve 3, the 4th valve 4 is opened, opens variable frequency pump 11, concentrate is circulated at pipeline.During spectra collection, open the 5th valve 5, close the 3rd valve 3 and the 4th valve 4 simultaneously, gather spectrum; After collection spectrum terminates, open the 6th valve 6, destroy system vacuum environment, sample valve 12 from below samples.
Adopt transmission beam method to gather near infrared spectrum, spectral range is 4000cm
-1-12000cm
-1, scanning times is 16 times, and resolution is 8cm
-1, take air as reference.2 and a half hours after from producing, sampled by the concentrate near infrared spectrum of flow cell every 15 minutes online acquisition simultaneously, gathered spectrum every 5 minutes afterwards and sample simultaneously.Sample the mensuration being originally respectively used to Paeoniflorin, icariin and solid content.Repeat 11 batches of Costumes numbness sheet extract concentration processs, the experiment of every batch is carried out sampling and gathering spectrum all in the same manner.2, each quality control index content measures
2, each quality control index content measures
High effective liquid chromatography for measuring Costumes numbness sheet concentrates Paeoniflorin in sample and Icariin content; Oven drying method mensuration Costumes numbness sheet concentrates the solid content in sample.
3, the Establishment and evaluation of near infrared quantitative model
For Aqueous extracts concentration process, choose 10 lot data for modeling, 1 lot sample is originally used for checking.The PLSR model parameter of Paeoniflorin, icariin and solid content is in table 1.In calibration set, the measured value of Paeoniflorin, icariin and solid content and the related coefficient figure of predicted value are shown in Fig. 2.Can find out, calibration set and the checking collection related coefficient of PLSR model are all greater than 0.94, RMSEC and RMSEP value is less and close to each other.Illustrate that the stability of model is high, generalization ability is good.
The parameter of table 1 each quality control index PLSR model gathers
4, each quality control index variation tendency in on-line analysis extract concentration process
Built PLSR established model is used for on-line analysis wherein Paeoniflorin, icariin and solid content in 1 batch of complete concentration process sample.Fig. 3 is that quality control index index prediction value contrasts figure with actual measured value trend.As can be seen from the figure, the anticipation trend of Paeoniflorin, icariin, solid content and the variation tendency of practical measurement value basically identical.RSEP value is respectively 8.20%, 13.80%, 10.44%, describes PLSR model and has higher prediction accuracy, substantially meet the accuracy requirement of Chinese Traditional Medicine real-time analysis.
Embodiment 2:
According to the method for embodiment 1, difference part is that the process of near infrared online analysis is alcohol precipitation supernatant concentration process.
1. near infrared online detection device is installed
Adopt the near infrared online detection device identical with embodiment 1.
2. the online acquisition of near infrared spectrum and alcohol precipitation supernatant concentration sample
Tank to be concentrated brings into operation, and the first valve 1, second valve 2, the 3rd valve 3, the 4th valve 4 is opened, opens variable frequency pump 11, concentrate is circulated at pipeline.During spectra collection, open the 5th valve 5, close the 3rd valve 3 and the 4th valve 4 simultaneously, gather spectrum; After collection spectrum terminates, open the 6th valve 6, destroy system vacuum environment, sample valve 12 from below samples.
Adopt transmission beam method to gather near infrared spectrum, spectral range is 4000cm
-1-12000cm
-1, scanning times is 16 times, and resolution is 8cm
-1, take air as reference.Collecting sample every 2 minutes online acquisition pass through the concentrate near infrared spectrum of flow cell while.Sample the mensuration being originally respectively used to Paeoniflorin, icariin and solid content.Repeat 11 batches of Costumes numbness sheet alcohol precipitation supernatant concentration processes, the experiment of every batch is carried out sampling and gathering spectrum all in the same manner.
3. each quality control index content measures
Adopt the analytical approach identical with embodiment 1.
4. the Establishment and evaluation of near infrared quantitative model
For alcohol precipitation supernatant concentration process, choose 10 lot data for modeling, 1 lot sample is originally used for checking.The PLSR model parameter of Paeoniflorin, icariin and solid content is in table 2.In calibration set, the measured value of Paeoniflorin, icariin and solid content and the related coefficient figure of predicted value are shown in Fig. 4.Can find out, calibration set and the checking collection related coefficient of PLSR model are all greater than 0.97, RMSEC and RMSEP value is less and close to each other.Illustrate that the stability of model is high, generalization ability is good.
The parameter of table 2 each quality control index PLSR model gathers
5. each quality control index variation tendency in on-line analysis extract concentration process
Built PLSR established model is used for on-line analysis wherein Paeoniflorin, icariin and solid content in 1 batch of complete concentration process sample.Fig. 5 is that quality control index predicted value contrasts figure with actual measured value trend.As can be seen from the figure, the variation tendency of Paeoniflorin, icariin and solid content anticipation trend and practical measurement value is basically identical.RSEP value is respectively 13.62%, 14.77% and 4.59%, describes NIR and to predict the outcome the result basic simlarity obtained with standard method.According to actual mass demand for control, think that the precision of prediction of institute's established model is in tolerance interval.
Embodiment 3:
According to the method for embodiment 1, difference part is that the process of near infrared online analysis extracts alcohol precipitation amalgamation liquid concentration process.
1. near infrared online detection device is installed
Adopt the near infrared online detection device identical with embodiment 1.
2. the online acquisition of near infrared spectrum and alcohol precipitation supernatant concentration sample
Tank to be concentrated brings into operation, and the first valve 1, second valve 2, the 3rd valve 3, the 4th valve 4 is opened, opens variable frequency pump 11, concentrate is circulated at pipeline.During spectra collection, open the 5th valve 5, close the 3rd valve 3 and the 4th valve 4 simultaneously, gather spectrum; After collection spectrum terminates, open the 6th valve 6, destroy system vacuum environment, sample valve 12 from below samples.
Adopt transmission beam method to gather near infrared spectrum, spectral range is 4000cm
-1-12000cm
-1, scanning times is 16 times, and resolution is 8cm
-1, take air as reference.Every 15 minutes online acquisition concentrate near infrared spectrum collecting sample simultaneously by flow cell in 2 hours that calculate from producing; Collecting sample every 5 minutes online acquisition pass through the concentrate near infrared spectrum of flow cell while afterwards.Sample the mensuration being originally respectively used to Paeoniflorin, icariin and solid content.Repeat 11 batches of Costumes numbness sheet alcohol precipitation supernatant concentration processes, the experiment of every batch is carried out sampling and gathering spectrum all in the same manner.
3. each quality control index content measures
Adopt the analytical approach identical with embodiment 1.
4. the Establishment and evaluation of near infrared quantitative model
For water extract-alcohol precipitation amalgamation liquid concentration process, choose 10 lot data for modeling, 1 lot sample is originally used for checking.The PLSR model parameter of Paeoniflorin, icariin and solid content is in table 3.In calibration set, the measured value of Paeoniflorin, icariin and solid content and the related coefficient figure of predicted value are shown in Fig. 6.Can find out, calibration set and the checking collection related coefficient of PLSR model are all greater than 0.93, RMSEC and RMSEP value is less and close to each other.Illustrate that the stability of model is high, generalization ability is good.
The parameter of table 3 each quality control index PLSR model gathers
5. each quality control index variation tendency in on-line analysis extract concentration process
Built PLSR established model is used for on-line analysis wherein Paeoniflorin, icariin and solid content in 1 batch of complete concentration process sample.Fig. 7 is that quality control index predicted value contrasts figure with actual measured value trend.As can be seen from the figure, the variation tendency of Paeoniflorin, icariin and solid content anticipation trend and practical measurement value is basically identical.RSEP value is respectively 8.09%, 1.32% and 9.98%, describes NIR and to predict the outcome the result basic simlarity obtained with standard method.According to actual mass demand for control, think that the precision of prediction of institute's established model is in tolerance interval.
Claims (4)
1. a Costumes numbness sheet concentration process near infrared online detection method, comprises that aqueous extract in Costumes numbness sheet production run concentrates, the on-line checkingi of alcohol precipitation supernatant concentration and water extract-alcohol precipitation amalgamation liquid concentration process, it is characterized in that:
The checkout equipment adopted is near infrared online detection device;
Near infrared online detection device comprises the first valve (1), the second valve (2), the 3rd valve (3), the 4th valve (4), the 5th valve (5), the 6th valve (6), vaporization chamber (7), heating chamber (8), variable frequency pump (11), sample valve (12), flow cell (13), fibre-optical probe (14), near infrared spectrometer (15), branch road (16) and circulation house steward bypass;
Circulation house steward bypass is connected and composed by the first bypass branch (17), the second bypass branch (18) and the 3rd bypass branch (19), the upper end of the first bypass branch (17) is connected with circulation house steward (9), and the first valve (1) is installed in the first bypass branch (17), the lower end of the first bypass branch (17) is connected with the charging aperture of variable frequency pump (11), the discharging opening of variable frequency pump (11) is connected with one end of the second bypass branch (18), second bypass branch (18) is equiped with the 3rd valve (3), the other end of the second bypass branch (18) is connected with the charging aperture of sample valve (12), the discharging opening of sample valve (12) is connected with the charging aperture of flow cell (13) by first line segments (22) of the 3rd bypass branch (19), the discharging opening of flow cell (13) is connected with second line segments (10) of the 3rd bypass branch (19), 4th valve (4) and the second valve (2) are installed in the 3rd bypass branch (19), the other end of the 3rd bypass branch (19) is connected with circulation house steward (9), 5th valve (5) is installed on arm (20), one end of arm (20) is connected with the second bypass branch (18), tie point is positioned on the pipeline in the middle of variable frequency pump (11) and the 3rd valve (3), forms the 5th valve (5) in parallel with the 3rd valve (3) and the 4th valve (4), flow cell (13) is equiped with fibre-optical probe (14), fibre-optical probe (14) is connected with near infrared spectrometer (15) by optical fiber (21), being connected with one end of branch road (16) of 6th valve, in second line segments (10) of another termination the 3rd bypass branch (19) of branch road (16),
One end of circulation house steward (9) is connected with the outlet of vaporization chamber (7), the other end of circulation house steward (9) is connected with the import of heating chamber (8), and the upper end outlet of heating chamber (8) is connected with vaporization chamber (7) by pipeline (23);
Costumes numbness sheet concentration process on-line checkingi, comprises the steps:
Detect and adopt above-mentioned near infrared online detection device, carry out online acquisition and concentrate sample and near infrared spectrum:
A, tank to be concentrated bring into operation, and the first valve (1), the second valve (2), the 3rd valve (3), the 4th valve (4) are opened, open variable frequency pump (11), concentrate is circulated at pipeline; During spectra collection, open the 5th valve (5), close the 3rd valve (3) and the 4th valve (4) simultaneously, gather spectrum; After collection spectrum terminates, open the 6th valve (6), destroy system vacuum environment, sample valve (12) sampling from below;
The collection of near infrared spectrum adopts transmission beam method, and spectral range is 4000cm
-1-12000cm
-1, scanning times is 16 times, and resolution is 8cm
-1, take air as reference;
B, use traditional chemical analysis method measure each quality control index content in concentrated sample:
A, high effective liquid chromatography for measuring Costumes numbness sheet concentrate Paeoniflorin in sample and Icariin content;
Chromatographic condition: chromatographic column is LichrospherC18 (4.6*250mm); Mobile phase A is 0.1% glacial acetic acid mutually, and B phase is acetonitrile; Gradient is set to 0-15min, 15%B; 15-20min, 15%-30%B; 20-35min, 30%B; Determined wavelength is 240nm, and temperature is 25 DEG C, and flow velocity is 1ml/min, and sample size is 10 μ l;
B, oven drying method mensuration Costumes numbness sheet concentrates the solid content in sample;
Dry to the measuring cup (after twice oven dry, weight is less than 5mg) of constant weight that weigh X
0; Sample centrifugal (13000rpm) is after 10 minutes, and get supernatant 10ml to flat bottle, weigh X
1, water bath method, 105 DEG C are dried 5 hours, take out to put in exsiccator to cool 30 minutes, and weigh rapidly X
2;
Calculate solid content: SSC (%)=(X
2-X
0)/(X
1-X
0) × 100%.
2. a kind of Costumes numbness sheet concentration process near infrared online detection method according to claim 1, is characterized in that near infrared spectrum and concentrating sample online acquisition divide 3 stages:
1., extract enriching stage: 2 and a half hours after from producing, gather near infrared spectrum every 15 minutes online acquisition by the concentrate of flow cell and get concentrating sample simultaneously, gathered infrared spectrum every 5 minutes afterwards, get concentrating sample simultaneously;
2., the alcohol precipitation supernatant concentration stage: every 2 minutes online acquisition by the concentrate near infrared spectrum of flow cell, simultaneously gather concentrating sample sample;
3. alcohol precipitation amalgamation liquid enriching stage, is extracted: in 2 hours that calculate from producing, every 15 minutes online acquisition concentrate near infrared spectrum by flow cell, gather concentrated sample simultaneously, afterwards every 5 minutes online acquisition concentrate near infrared spectrum by flow cell, gather concentrated sample simultaneously.
3. a kind of Costumes numbness sheet concentration process near infrared online detection method according to claim 1, is characterized in that the Establishment and evaluation setting up three enriching stage concentrate near infrared quantitative models;
Concentrated 3 concentration processs of, alcohol precipitation supernatant concentration, water extract-alcohol precipitation amalgamation liquid concentrated for Aqueous extracts, each process chooses 10 lot data respectively for modeling, and 1 lot sample is originally used for checking; 1. extract enriching stage: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively and deducts straight line, eliminates constant offset and first order derivative; Modeling wave band is respectively 5449.9-6101.8,5449.9-6101.8 and 4601.4-4246.5,5449.9-6101.8cm
-1; 2. the alcohol precipitation supernatant concentration stage: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively without Pretreated spectra, eliminates constant offset, eliminates constant offset; Modeling wave band is respectively 5449.9-6475.9,5773.9-6101.8 and 7498-9403.3,5449.9-6475.9cm
-1; 3. alcohol precipitation amalgamation liquid enriching stage is extracted: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively without Pretreated spectra, vector normalization, second derivative; Modeling wave band is respectively 5449.9-6475.9,5773.9-6101.8,5449.9-6101.8cm
-1; Partial least squares regression (PLSR) is adopted to set up the quantitative calibration models of near infrared spectrum and icariin, Paeoniflorin and solid content; Mean square deviation (RMSEP) and relative deviation (RSEP) is integrated as index optimization modeling parameters with related coefficient (R), calibration set mean square deviation (RMSEC), checking, investigate model performance, close to 1, R more represents that the correlativity between the predicted value of model and standard control methods analyst value is better; The size of RMSEC with RMSEP is relevant to sample chemical value, and these two parameters are more little more close, then show that model performance is better, precision of prediction is higher; According to actual mass control overflow, when RSEP value lower than 20% time, think that the precision of prediction of institute's established model is in tolerance interval;
Apply the variation tendency of each quality control index in built model on-line prediction concentration process;
The near infrared spectrum of online acquisition concentrate, uses the correlation model built up to detect the variation tendency of each quality control index in concentration process.
4. Costumes numbness sheet concentration process near infrared online detection method according to claim 3, is characterized in that: quantitative model divides 3 stages to set up: 1. extract enriching stage: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively and deducts straight line, eliminates constant offset and first order derivative; Modeling wave band is respectively 5449.9-6101.8,5449.9-6101.8 and 4601.4-4246.5,5449.9-6101.8cm
-1; 2. the alcohol precipitation supernatant concentration stage: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively without Pretreated spectra, eliminates constant offset, eliminates constant offset; Modeling wave band is respectively 5449.9-6475.9,5773.9-6101.8 and 7498-9403.3,5449.9-6475.9cm
-1; 3. alcohol precipitation amalgamation liquid enriching stage is extracted: the preprocessing procedures of Paeoniflorin, icariin and solid content is respectively without Pretreated spectra, vector normalization, second derivative; Modeling wave band is respectively 5449.9-6475.9,5773.9-6101.8,5449.9-6101.8cm
-1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105784778A (en) * | 2016-05-25 | 2016-07-20 | 安徽华润金蟾药业股份有限公司 | System and method for judging terminal point of cinobufagin ethanol recycling section |
| CN108195969A (en) * | 2018-01-26 | 2018-06-22 | 吉林省现代中药工程研究中心有限公司 | Chinese Traditional Medicine component content detection method and relevant device |
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| CN112924411A (en) * | 2019-12-06 | 2021-06-08 | 九芝堂股份有限公司 | Detection system and detection method for concentration process of Liuwei Dihuang pills |
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