CN101832921A - Method for on-linly detecting and controlling two-dimensional mixing homogeneous degree of traditional Chinese medicine powder by near infrared - Google Patents
Method for on-linly detecting and controlling two-dimensional mixing homogeneous degree of traditional Chinese medicine powder by near infrared Download PDFInfo
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Abstract
The invention discloses a method for on-linly detecting and controlling homogeneous degree of two-dimensional mixing process of traditional Chinese medicine powder by a near infrared spectrum analyzer, comprising the following steps: (1) presetting the on-line detection time span of an near infrared spectrum analyzer in the two-dimensional mixing process of the traditional Chinese medicine powder; (2) in the two-dimensional mixing process of the traditional Chinese medicine powder, utilizing the near infrared spectrum analyzer to on-liny measure the mixing of the traditional Chinese medicine powder at preset wavelength within the preset time span to obtain a spectrum, and displaying the spectrum graph in a computer screen wirelessly connected with the near infrared spectrum analyzer; and (3) according to the difference of the near infrared spectrum at different time points within the preset time span in the mixing process, judging whether materials are evenly mixed; if the difference of the near infrared spectrum at different time points is smaller than certain threshold value within certain time, proving that the traditional Chinese medicine powder is evenly mixed, otherwise, continuing on-linly detecting the two-dimensional mixing of the traditional Chinese medicine powder. Preferably, the near infrared spectrum difference is judged according to the standard deviation of the absorbance of multiple continuous spectrums on each point of multiple wavelength points at different time points.
Description
Technical field
The present invention relates to the method for Chinese medicine, relate in particular to and adopt near infrared online detection to control the method for the uniformity coefficient of Yaotongning capsules mixed process in the online detection and control of the uniformity coefficient of mixed process.
Background technology
At present, Chinese medicine at the Chinese medicine production field mixes the one dimensions mixing of adopting more, promptly adopt the flip-flop movement mixer to carry out the mixing of Chinese medicine medicinal powder, it is made up of barrel, kinematic train, support etc., cylindrical shell rotatablely moves as average rate under the drive of motor, material moves as hoop along barrel, form the motion of material above-below direction, go up the remaining space of reservation in the barrel and the reasonable rotational speed of barrel in addition, make the different component of participating in mixing can do relative motion most possibly, thereby reach the purpose of mixing.The motion of barrel very simple (motion in one dimension), this method mixed process is simple to operate, however have certain shortcoming: 1. owing to be simple motion in one dimension, its coefficient is lower, only is 50%, has seriously restricted the batch mixing amount, has limited mixing efficiency.2. in mixed process, only rely on simple one-way movement to reach the purpose that mixes, the dead angle appears mixing in its mixed process easily, causes and mixes uneven phenomenon, and its mixture homogeneity only can reach about 95%.
Shortcoming at the one dimension mixing, the Chinese medicine production field adopts the method for two-dimentional hybrid motion that Chinese medicine medicinal powder is mixed, promptly adopt compound mixer, it is by barrel, two cover barrel motions and the parts such as upper and lower frame that this two covers barrel motion uses are installed are formed.Wherein, barrel is fixed on the upper spider, and the barrel motion is respectively that barrel is made circular motion and barrel is done oscillating motion.Its tempering tank is made circular motion in the drive of circular motion gear train around its axis of symmetry on the one hand, and promptly batch mixer rotates with 9rpm; Under the swinging transmission mechanism transmission, do oscillating motion again on the other hand around a transverse axis with its axis of symmetry quadrature, it is the swing that batch mixer carries out 5spm, thereby barrel is obtained simultaneously by rotation and swing, and these two kinds of separate synergy make material do the motion of two-dimensional directional.Simultaneously, the staving inwall is welded with flight in addition, material is shed to the space, thereby made mixing of materials more abundant, makes material increase moving radially again, thereby becomes the motion of three-dimensional, and material is fully mixed.Because the rock and roll process can make material produce powerful axially pulse, thereby hybrid motion each moment is mixed and convection current conglomeration effect by diffusion.
Yet because the method for the two-dimentional hybrid motion of employing is mixed Chinese medicine medicinal powder, in the past technology that are used for one dimension mixing and liquid preparation on-line monitoring are difficult to be applicable to the mixing of employing two dimension more.In the present invention, be that two dimension is mixed because Yaotongning capsules adopts in mixed process, this has proposed a difficult problem for again near infrared online detection.
Summary of the invention
According to the present invention, provide a kind of near-infrared spectrometers that adopts to carry out the method that the uniformity coefficient of Chinese medicine medicinal powder two dimension mixed process is controlled in online detection, comprising:
(1) sets in advance the online detection time length of near-infrared spectrometers in the two-dimentional mixed process of Chinese medicine medicinal powder;
(2) in Chinese medicine medicinal powder two dimension mixed process and in the time span that is setting in advance, utilize near-infrared spectrometers that the mixing of Chinese medicine medicinal powder is carried out on-line measurement and obtained spectrum with presetted wavelength, and with the computer screen of near infrared spectrometer wireless connections in spectrogram shape;
(3) judge according to the near infrared spectrum difference of the different time points in preset time length in the batch mixing process whether the batch mixing of Chinese medicine medicinal powder is even, if in the near infrared spectrum difference of different time points within a certain period of time less than certain threshold value, then the mixing of Chinese medicine medicinal powder is even, otherwise proceeds the online detection to the two dimension mixing of Chinese medicine medicinal powder.
Wherein, whether judge that less than certain threshold value whether near infrared spectrum difference in different time points is within a certain period of time less than certain threshold value within a certain period of time according to the standard deviation of the absorbance of a plurality of continuous spectrum at each place of a plurality of wavelength points in the predetermined wavelength of different time points.
According to the present invention, step (3) further comprises:
(4) very first time point in the length is at the fixed time selected piece of spectral composition of n bar continuous acquisition from the spectrum that described near-infrared spectrometers obtained, according to n bar spectrum in formula (1) computing block in wavelength points i place absorbance A
IjStandard deviation S
i
Wherein, A
IjBeing the absorbance of the wavelength points i j of place bar spectrum, is to utilize near infrared spectrometer that the one dimension mixing of Chinese medicine medicinal powder is carried out on-line monitoring with above-mentioned predetermined wavelength to measure in advance,
It is the mean light absorbency of n bar spectrum in the wavelength points i place piece;
(5) calculate the mean standard deviation S of m wavelength according to formula (2), and S is presented in the described computer screen;
Wherein, m is the wavelength points sum of choosing, and is positive number;
(6) second time point in the time span that sets in advance respectively repeats steps (4)-(5) up to t time point, and wherein t is an integer;
(7) if when continuously the S value of k time point is less than threshold value L in the time span that sets in advance, finish online detection; Otherwise, continue execution in step (4)-(6), wherein k is the integer less than t.
According to the present invention, described near-infrared spectrometers is the online near infrared spectrometer of Luminar4030 type that BRIMROSE company produces.
According to the present invention, described predetermined wavelength is 1300～2000nm, and each wavelength points is 1300nm, 1302nm, and 1304nm ..., 1998nm, 2000nm, n=20, m=351.
Wherein, the described time span that sets in advance is 60 minutes.
Wherein, described threshold value is 0.000045.
Wherein said Chinese medicine medicinal powder is the medicinal powder of Yaotongning capsules.
Description of drawings
Fig. 1 two dimension Chinese medicine medicinal powder mixing arrangement synoptic diagram.
Fig. 2 a and 2b are the method for the uniformity coefficient of online detection and control Chinese medicine medicinal powder two dimension mixed process of the present invention.
The spectrum of the one dimension batch mixing process that Fig. 3 gathers near infrared spectrometer of the present invention.
The uniformity coefficient trend map of the Chinese medicine medicinal powder of Fig. 4-8 when determining piece big or small in the movable block standard deviation algorithm.
The uniformity coefficient trend map of Yaotongning capsules two dimension batch mixing process when Fig. 9-13 is Block Size=20.
Figure 14-15 is the uniformity coefficient trend map of Yaotongning capsules two dimension batch mixing process in the preferred embodiment of the present invention.
Figure 16-17 is the uniformity coefficient trend map of the different spectrum average times of Yaotongning capsules two dimension batch mixing process in the preferred embodiment of the present invention.
Embodiment
According to the present invention, in the two-dimentional batch mixing process of Chinese medicine medicinal powder such as Yaotongning capsules, adopt the near infrared detection uniformity coefficient to carry out on-line monitoring.At first, set in advance the online detection time length (step 202) of near-infrared spectrometers in Yaotongning capsules mixed process.Next, in Chinese medicine medicinal powder two dimension mixed process and in the time span that is setting in advance, utilize the near-infrared spectrometers detection technique that the two-dimentional batch mixing process of Yaotongning capsules is carried out on-line measurement and obtained spectrum with predetermined wavelength, and in the corresponding window of near-infrared spectrometers spectrogram shape (step 204).Judge batch mixing whether evenly (step 206) according to the near infrared spectrum difference of the different time points in preset time length in the batch mixing process.Batch mixing is inhomogeneous, and the each spectrum of gathering of near infrared is just variant, inhomogeneous more, and then the SPECTRAL DIVERSITY in different time points is big more; Batch mixing is even, and material all forms an integral body, and the composition of every part all is the same, then in the near infrared spectrum difference of different time points just very little (as less than certain threshold value).
Preferably, the measurement index of SPECTRAL DIVERSITY can occur with the movable block standard deviation, promptly with the pretreated data of spectrum differential the spectrum of front and back is asked for standard deviation, forms a MBSD value.The MBSD value is big and variation is big, and then SPECTRAL DIVERSITY is big, and batch mixing is inhomogeneous; The MBSD value is little and tend towards stability, and then SPECTRAL DIVERSITY is little, and batch mixing is even.In the spectrum real-time analysis to the batch mixing process, the change procedure of this value is that the form with the MBSD Trendline provides.
Preferably, the present invention adopts movable block standard deviation method (moving block of standarddeviation, MBSD) difference of analyzing near infrared spectrum is judged with the two-dimentional mixed process terminal point that carries out Yaotongning capsules.Particularly, from the spectrum that near infrared spectrometer obtains, select piece of spectral composition of n bar continuous acquisition, calculate in this piece n bar spectrum in wavelength points i place absorbance A according to following formula (1) and (2)
IjStandard deviation S
i, calculate the mean standard deviation S (step 402,404) of m wavelength again:
In the formula, n forms a piece n absorbance spectrum continuously, and m is that the wavelength of choosing is always counted, and is positive integer.A
IjBe the absorbance of the wavelength points i j of place bar spectrum, can utilize near infrared spectrometer that the one dimension mixing of Yaotongning capsules is carried out on-line monitoring with above-mentioned predetermined wavelength and measure in advance,
It is the mean light absorbency of n bar spectrum in the wavelength points i place piece.Si is the variance that wavelength points i place amounts to the absorbance of n bar spectrum.
A time point will be moved behind the piece, promptly reject in the former n bar spectrum time point spectrum the earliest as the 1st spectrum, replenish a new spectrum as n+1 bar spectrum, the 2nd spectrum is recomputated standard deviation S to second piece of n+1 bar spectral composition according to above-mentioned formula, by that analogy, t time point in the schedule time had a rest.
In the two-dimentional mixed process of Yaotongning capsules, the S value changes in time, and when the mixing of Yaotongning capsules was even gradually, the S value diminished gradually.When S amplitude of variation during, as the S value of a continuous k time point during less than threshold value L (step 406), then think the mixing evenly (step 408) of Yaotongning capsules less than a predetermined threshold.If the S amplitude of variation is not less than a predetermined threshold in regular hour length, think that then the mixing of Yaotongning capsules is uneven as yet, then continue to utilize near infrared spectrometer that the two-dimentional mixed process of Yaotongning capsules is carried out on-line monitoring.
Example:
1, two-dimentional Chinese medicine medicinal powder mixing apparatus is introduced
According to a preferred embodiment of the invention, the two-dimentional Chinese medicine mixing apparatus of employing is as follows:
The important technological parameters of EYH-1500A rock and roll formula (two dimension) Wen Heji:
Sample: 10 kinds of starting material of Yaotongning capsules, sample state are 80 purpose powder.
2, the type selecting of near-infrared spectrometers, installation and equipment operation
According to the present invention, as long as nir instrument can guarantee to stablize in the two-dimentional hybrid motion process of complexity, be not afraid of vibrations, have higher sensitivity, also can realize the real-time detection of various batch mixers, just can be used for online detection to control the uniformity coefficient of Yaotongning capsules mixed process.Certainly, because the instrument of different model, may there be small difference in the setting of its parameter when carrying out online the detection, but still can use method of the present invention.
Preferably, the present invention adopts the Luminar 4030 free space formula AOTF technology near infrared spectrometers of U.S. Brimrose company.
The formation of this product is shown in 5.1 tables:
The configuration of table 5.1AOTF/ (NIR) Luminar4030 free style near infrared process analyzer
Luminar 4030 free space formula AOTF technology near infrared spectrometer mounting meanss are as shown in Figure 2:
According to the present invention, it is as follows to utilize the U.S.'s Luminar4030AOTF-NIR of BRIMROSE company spectrometer to control the operation of uniformity coefficient of the two-dimentional mixed process of Chinese medicine medicinal powder (as Yaotongning capsules):
(1) preliminary work
1. the U.S.'s Luminar4030AOTF-NIR of BRIMROSE company spectrometer correctly is installed on the two-dimentional mixer, hold-down nut is screwed.
2. battery is loaded onto, turned on the power switch pre-thermal instrument in preceding 5 minutes in monitoring.
3. open computer work, in open mode, workstation will be finished the wireless connections with instrument automatically as if the spectrometer power switch.
(2) working procedure
1. double-click the pred32 icon, start the Predictor32 program, the input username and password enters main window.
2. click Setup Parameters at main window coefficient is set, the instrument parameter of employing is: spectral range 1300～2000nm, time-delay 350ms, Block size=20, MBSD limit=0.000045,100 spectrum are average, 1450nm place absorbance 〉=0.51,1800nm place absorbance 〉=0.52.In program schema, click On-line Automatic (on-line automatic), click " ok " and determine.
3. in main window, click Load Profile/Select INI File and the SessionDefinition dialog box occurs, clicking Browse browses, load the configuration file set (D: test.bpp), click " ok " and determine that software systems are ready.
When 4. beginning batch mixing, determine workstation, click Run MeasurementSession operation on-line measurement, begin monitoring with on spectrometer is connected.Monitoring system is obtained spectrum automatically continuously, shows to predict the outcome spectrum figure and trend chart in corresponding window.
If 5. stop, only needing to click Stop Measurement Session and stop measuring phases in the process any stage.
6. continue previous measuring phases if desired, click Run Measurement Session operating measurement process once more, and in ejecting dialog box, select " yes " to determine to continue to go up subtask.
7. mix and finish on-line monitoring trend map grabgraf and preservation.
8. spectrogram be kept at automatically computer D: in the test.dat file, every batch detect finish after, this document is moved in the corresponding document folder, and renames with drug batch number.
9. after monitoring finishes, close main window, close instrument power source, take off battery.
(3) result judges
The curve tendency of MBSD in the online observation trend chart changes up and down not quite when curve is stabilized in certain numerical value, and kept more than 30 minutes stabilization time, and incorporation time reaches more than 1 hour, and it is even to can be considered mixing of materials.
In the Luminar4030AOTF-NIR spectrometer, Load Profile/Select INI File opens the dialog box that loading parameters is provided with file, On-line Automatic carries out spectral scan and data processing automatically for the parameter that is provided with in the file according to the parameter that loads, D: test.bpp be that parameter is provided with file.All the other parameters specify as follows:
On-line Manual is online manually, and program begins circulation, allows the user to accept or abandon the spectrum that each obtains, and shows to predict the outcome spectrum figure and trend chart in corresponding window.Online manual mode: online manual mode allows the number of times of a sample duplicate measurements of instruction manual, selects one from three Sample Name Change Options sample name changing options
Off-line Automatic off-line is automatic, and program begins circulation, is kept at the spectrogram that is scanned and collects in the spectroscopic data file with showing continuously automatically.In corresponding window, show and predict the outcome spectrum figure and trend chart.
Off-line Manual off-line is manual, and program begins circulation, allows the user to accept or abandon each to be kept at the spectrum that is scanned and collects in the spectroscopic data file, shows to predict the outcome spectrum figure and trend chart in corresponding window.
Don ' t Change does not change, and the spectrum title of acquiescence generates in spectrum is collected: the previous spectrum that is scanned becomes the default name that the next one is scanned spectrum.
Clear removes, and the spectrum title of acquiescence generates in spectrum is collected: will be eliminated (neutral gear) after scanning default name at every turn.
Increment Trailing increment, the spectrum title of acquiescence generates in spectrum is collected: if the title of the previous spectrum that is scanned finishes with numerical value, then the default name of next spectrum will add up with N numerical value.
For example, as n=5, continuous acquiescence spectrum title is as follows:
Sample 1, sample 6 and sample 11.
Show Classification Results Detailed shows that detailed classification results selects frame, shows the exhaustive division result.
Show all Results show that all results select frame, show all results that measure.
Show All Selected Spectra shows that all selecteed spectrum select frame, shows all selecteed spectroscopic datas in the measurement.The display result option spectrum that will slow down is collected.
General routine (dd.dddd ...), the definition resulting schema is: dd.dddd
Scientific science counting (dd ... E+dd), the definition resulting schema is: d.dd ... E+dd.
Decimal Digits decimal place, the definition resulting schema is the decimal place of measurement result, default value: 4, tolerance interval: 1-10.
Method for the uniformity coefficient of the employed U.S. Luminar4030AOTF-NIR of BRIMROSE company spectrometer and near infrared online detection of the present invention control Chinese medicine medicinal powder two dimension mixed process among the present invention, Block size is the parameter n in the formula 1, presetted wavelength is 1300～2000nm, and predetermined threshold is that MBSD limit is 0.000045.Above-mentioned parameter is determined according to experiment once.
2.1 determine the size of piece
Utilize the U.S. Luminar4030AOTF-NIR of BRIMROSE company spectrometer, carry out the two dimensional motion batch mixing with 1300～2000nm, time-delay 350ms, 10 spectrum average out to parameters, behind every batch mixing 5min, stop motion turns to the bottom with instrument, begin to gather spectrum, till the Yaotongning capsules sample mixes fully.Can guarantee that like this spectrum that collects all is effective spectrum.Then the spectrum that collects is carried out MBSD movable block number experiment,, carry out the trend analysis of batch mixing uniformity coefficient, to determine best Block Size as Block Size=3,5,10,15 or 20 the time.When Block Size=3,5,10,15, uniformity coefficient trend 20 time shown in Fig. 4-8.
Here the spectrum that is used for doing the uniformity coefficient trend analysis all is effective spectrum.Can find that by changing BlockSize as Block Size=3,5 or 10 the time, the trend of uniformity coefficient all compare confusion, does not have tangible trend, as Fig. 4～shown in Figure 6; When Block Size=15 or 20, the trend of uniformity coefficient is just apparent in view, as Fig. 7, shown in Figure 8.Here we determine with Block Size=20 to be the experiment parameter of the best.
2.2 one dimension batch mixing experiment
Utilize the U.S. Luminar4030AOTF-NIR of BRIMROSE company spectrometer, carry out the one dimension batch mixing spectra collection of omnidistance Yaotongning capsules with 1300～2000nm, time-delay 350ms, 10 spectrum average out to parameters.
" time-delay 350ms " refer in mixed process, when medicinal powder arrives active position under the near infrared spectrometer form for the spectrum that makes collection more accurately and the response delay time of setting.Have only when medicinal powder under the near infrared spectrometer form during upright position, the spectrum that collect this moment is only more accurately and is reliable, therefore set delay time, i.e. moment when medicinal powder has just arrived the near infrared spectrometer form, do not carry out spectra collection immediately, but treat to carry out spectra collection again behind the 350ms, this moment medicinal powder and near infrared spectrometer form position the best, the effect of spectra collection is also best.
Batch mixing is rocked to minimum point with the instrument end of batch mixer when 10min, rely on the gravity sensor of instrument itself to trigger automatically.According to the present invention, the one dimension batch mixing process of Yaotongning capsules is carried out spectrogram that spectra collection obtains as shown in Figure 3.Spectral absorbance to the one dimension batch mixing is analyzed, and finally obtains best absorbance scope, and promptly 1450nm place absorbance scope is 0.588～0.606.
Simultaneously, according to the experiment of one dimension batch mixing, determine absorbance A
Ij, A
IjBe the absorbance of j bar spectrum at i wavelength points place.In sweep parameter, the wavelength coverage of setting is: 1300～2000nm, wavelength increment is 2nm, determines A
IjEach wavelength points in 1300～2000nm scope is 1300,1302 ... 1998,2000 absorbances that amount to 351 wavelength points places.
According to the present invention, the m in the formula (1) is a wavelength increment.In m value deterministic process, compare wavelength increment respectively and be respectively 1,2,3,5 situation, when wavelength increment is 1, when being m=701, cause sweep velocity slow excessively too much owing to counting at the scanning process medium wavelength, the invalid spectrum number that collects in the on-line monitoring process increases considerably, and has had a strong impact on the judgement of mixing resultant; When wavelength increment is 3 and 5, promptly m is respectively 234 and at 141 o'clock, minimizings because wavelength is counted, and its sweep velocity raising is convenient to obtain rational spectrum, but S
iValue is unstable in experiment, can't set the exact value of MBSD limit; Only when m=351, the speed of its scanning and stability are all best, therefore determine with m=351 to be optimum value.
Therefore, according to the present invention, the size of movable block is 20, and each wavelength points in 1300～2000nm scope is 1300,1302 ... 1998,2000 amount to 351 wavelength points, then are being used for basis of calculation mean deviation formula, m=351, n=20.In other words, according to embodiments of the invention, the method of near infrared detection uniformity coefficient that finally is used for the two-dimentional batch mixing process of Chinese medicine medicinal powder such as Yaotongning capsules, Si is that 20 spectrum are respectively 1300,1302 ... 1998, the standard deviation of 2000 each wave point place absorbance log value, S is the mean value of the standard deviation of 351 wavelength points.
2.3 two-dimentional batch mixing uniformity coefficient trend analysis
Carried out the spectra collection of 3 two-dimentional batch mixings of whole process with 1300～2000nm, time-delay 350ms, 10 spectrum average out to parameters.During the two dimension batch mixing, adopt the definite absorbance scope (1450nm place absorbance scope is 0.588～0.606) of one dimension batch mixing spectrum of Block Size=20 and Yaotongning capsules that two-dimentional batch mixing spectrum is carried out the analysis of uniformity coefficient trend.Set MBSD limit=0.000045.
2.3.1 the omnidistance data analysis of two-dimentional batch mixing
On February 28th, 2008, utilization utilizes the method for the uniformity coefficient of the U.S.'s Luminar4030AOTF-NIR of BRIMROSE company spectrometer and near infrared online detection of the present invention control Chinese medicine medicinal powder two dimension mixed process, gather the Yaotongning capsules two dimension and mix the near infrared spectrum of overall process, situation to mixed process is analyzed, it is as follows to impose a condition: with 1300～2000nm, time-delay 350ms, 10 times spectrum is average, the absorbance scope (1450nm place absorbance scope is 0.588～0.606) that adopts Block Size=20 and Yaotongning capsules one dimension batch mixing spectrum to determine, the result shows: batch mixing is after 1 hour, and spectrum is all in setting range.Trend shows shown in Fig. 9-13:
2.3.2 omnidistance data analysis of two-dimentional batch mixing and chemical content are measured checking
On March 3rd, 2008, utilization utilizes the U.S. Luminar4030AOTF-NIR of BRIMROSE company spectrometer, adopts the parameter of method of the present invention and above-mentioned setting, again Continuous Tracking the two-dimentional mixed process of 2 batch samples, the near infrared spectrum of gathering is analyzed, and the result is all consistent.
Validity for the method for the uniformity coefficient that confirms near infrared online detection control Chinese medicine medicinal powder two dimension mixed process, adopt the chemical content method for measuring that the different incorporation times of material in above 3 batches of Tongning capsules two dimension mixed process are analyzed, based on each index content wherein, the result is as shown in the table, experimental data shows that after the two dimension of Yaotongning capsules is mixed 1 hour each index content does not have significant change in the sample, illustrate and mix, this is consistent with the near infrared spectrum trend map, shows the purpose of utilizing method of the present invention and each parameter setting can reach online detection substantially.
Table 1: content results in the sample of different incorporation times (080228) (unit: mg/0.3g)
Table 2: content results in the sample of different incorporation times (080229) (unit: mg/0.3g)
Table 3: content results in the sample of different incorporation times (080330) (unit: mg/0.3g)
2.4 adjust the parameter analysis
By all experimental spectrum are carried out analysis-by-synthesis, experiment parameter made partly adjusted, promptly average with 1300～2000nm wave band, 100 spectrum, time-delay 350ms, 1450nm absorbance 〉=0.51,1800nm absorbance 〉=0.52, Block size=20 are the analysis that parameter is carried out two-dimentional batch mixing spectrum uniformity coefficient trend.Have carried out the collection of omnidistance Yaotongning capsules two dimension batch mixing spectrum on March 11st, 2008 and on March 12nd, 2008 according to above parameter.Set MBSD limit=0.000045.The result shows that this parameter satisfies condition.Simultaneously, find out that mix after 1 hour, sample near infrared curve does not have significant change, show to mix from the spectrogram trend of Figure 14-15.
3. conclusion
Comprehensive above the analysis, adopt method of the present invention and utilization to utilize the U.S. Luminar4030AOTF-NIR of BRIMROSE company spectrometer, discovery two-dimension spectrum in 1 hour of initial batch mixing has demonstrated the trend of tangible uniformity coefficient, and Trendline is just in the fluctuation of doing among a small circle the time afterwards.
For the adjustment of the Luminar4030AOTF-NIR of BRIMROSE company instrument parameter, carried out twice analysis, parameter is provided with as follows:
(1) 10 spectrum is average, 1450nm place absorbance scope is 0.588～0.606;
(2) 100 spectrum is average, 1450nm place absorbance 〉=0.51,1800nm place absorbance 〉=0.52.
More than Shi Yan wavelength coverage is 1300～2000nm, time-delay 350ms, Block size=20, MBSD limit=0.000045.
Find by analyzing, when selecting 10 spectrum mean times, the undulatory property of the mixing trend curve that obtains is bigger, when the undulatory property of the mixing trend curve of selecting 100 spectrum mean times to obtain smaller, and its fluctuation range all below preset threshold, can reflect the situation of change of mixed process traditional Chinese medicine powder uniformity coefficient more accurately.This is because 100 spectrum have on average adopted two absorbance scopes, and only be provided with the lower limit of scope, filter effect to spectrum is more remarkable, therefore adopts 100 average uniformity coefficient Trendline more remarkable than adopting 10 average uniformity coefficient, and Trendline is more level and smooth.Shown in Figure 16-17.
The method according to this invention, utilize the Luminar4030AOTF-NIR of BRIMROSE company spectrometer, Yaotongning capsules mixed the two dimension in the batch mixing process carry out separate analysis, to triggering time-delay, the scanning average time, analysis is groped and debugged to parameters such as the absorbance scope of characteristic wavelength point, and final definite Luminar4030AOTF-NIR spectrometer instrument parameter that adopts is: spectral range 1300～2000nm, time-delay 350ms, Block size=20, MBSD limit=0.000045,100 times spectrum is average, 1450nm place absorbance 〉=0.51,1800nm place absorbance 〉=0.52.
In the embodiments of the invention, mix to describe with the two dimension of Yaotongning capsules.Yet method of the present invention is not restricted to the control of the uniformity coefficient that the two dimension of Yaotongning capsules mixes, and the present invention is equally applicable to the control of the uniformity coefficient that the two dimension of other Chinese medicine medicinal powder mixes.Under the condition that does not deviate from principle of the present invention and spirit, can make amendment and change the present invention.
Claims (8)
1. one kind is adopted near-infrared spectrometers to carry out the method that the uniformity coefficient of Chinese medicine medicinal powder two dimension mixed process is controlled in online detection, comprising:
(1) sets in advance the online detection time length of near-infrared spectrometers in the two-dimentional mixed process of Chinese medicine medicinal powder;
(2) in Chinese medicine medicinal powder two dimension mixed process and in the time span that is setting in advance, utilize near-infrared spectrometers that the mixing of Chinese medicine medicinal powder is carried out on-line measurement and obtained spectrum with presetted wavelength, and with the computer screen of near infrared spectrometer wireless connections in spectrogram shape;
(3) judge according to the near infrared spectrum difference of the different time points in preset time length in the batch mixing process whether the batch mixing of Chinese medicine medicinal powder is even, if in the near infrared spectrum difference of different time points within a certain period of time less than certain threshold value, then the mixing of Chinese medicine medicinal powder is even, otherwise proceeds the online detection to the two dimension mixing of Chinese medicine medicinal powder.
2. described method as claimed in claim 1, wherein, whether judge that less than certain threshold value whether near infrared spectrum difference in different time points is within a certain period of time less than certain threshold value within a certain period of time according to the standard deviation of the absorbance of a plurality of continuous spectrum at each place of a plurality of wavelength points in the predetermined wavelength of different time points.
3. described method as claimed in claim 2, wherein, step (3) further comprises:
(4) very first time point in the length is at the fixed time selected module of spectral composition of n bar continuous acquisition from the spectrum that described near-infrared spectrometers obtained, calculate in this module n bar spectrum in wavelength points i place absorbance A according to formula (1)
IjStandard deviation S
i
Wherein, A
IjBeing the absorbance of the wavelength points i j of place bar spectrum, is to utilize near infrared spectrometer that the one dimension mixing of Chinese medicine medicinal powder is carried out on-line monitoring with above-mentioned predetermined wavelength to measure in advance,
It is the mean light absorbency of n bar spectrum in the wavelength points i place piece;
(5) calculate the mean standard deviation S of m wavelength according to formula (2), and S is presented in the described computer screen;
Wherein, m is the wavelength points sum of choosing, and is positive number;
(6) second time point in the time span that sets in advance respectively repeats steps (4)-(5) up to t time point, and wherein, t is an integer;
(7) if when continuously the S value of k time point is less than threshold value L in the time span that sets in advance, finish online detection; Otherwise, continue execution in step (4)-(6), wherein k is the integer less than t.
4. described method as claimed in claim 3, wherein, described near-infrared spectrometers is the online near infrared spectrometer of Luminar 4030 types that BRIMROSE company produces.
5. described method as claimed in claim 4, wherein, described predetermined wavelength is 1300～2000nm, each wavelength points is 1300nm, 1302nm, 1304nm ..., 1998nm, 2000nm, n=20, m=351.
6. described method as claimed in claim 5, wherein, the described time span that sets in advance is 60 minutes.
7. described method as claimed in claim 6, wherein, described threshold value is 0.000045.
8. the method one of any as claim 1-7, wherein said Chinese medicine medicinal powder is the medicinal powder of Yaotongning capsules.
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