CN112903508B - On-line detection method of dripping pill preparation - Google Patents

On-line detection method of dripping pill preparation Download PDF

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CN112903508B
CN112903508B CN202110320246.7A CN202110320246A CN112903508B CN 112903508 B CN112903508 B CN 112903508B CN 202110320246 A CN202110320246 A CN 202110320246A CN 112903508 B CN112903508 B CN 112903508B
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dripping
pill
dropping
width
drop
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瞿海斌
王小平
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Zhejiang University ZJU
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness

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Abstract

The invention belongs to the technical field of drop size characterization and laser measurement in a dropping process of dropping pills, and particularly relates to an online detection method of a dropping pill preparation. The method comprises the following steps: measuring the width of the liquid drop in the dropping process of the dropping pill by using a detection system; after data processing, the width of the liquid drop is correlated with the weight of the dripping pill, and a model is established; and then, according to the measured liquid drop width, predicting the pill weight of the dropping pill by using a model, and realizing the online detection of the dropping process. The detection system is simple and convenient to operate, stable in measurement, suitable for industrial production and good in economic benefit, social benefit and environmental benefit.

Description

On-line detection method of dripping pill preparation
Technical Field
The invention belongs to the technical field of drop width characterization and laser measurement in a dropping process of dropping pills, and particularly relates to an online detection method of a dropping pill preparation.
Background
The dripping pill is a novel medicament form and has the advantages of improving the medicament dissolution, increasing the medicament stability, improving the bioavailability and the like. The preparation process is complicated, wherein the key process influencing the quality of finished dripping pills is a dripping process, namely, a mixed liquid medicine prepared by uniformly mixing raw and auxiliary materials is dripped into a matrix at a certain temperature. The property difference of the raw and auxiliary materials and the parameter change of the dripping process are all key factors causing the quality difference of finished products. The weight of the dripping pill is an important index for evaluating the quality of the dripping pill, and the difference between batches and in batches caused by the weight of the dripping pill is directly related to the dosage of the dripping pill, thereby influencing the drug effect.
At present, no literature reports a measuring and characterizing method of a dripping process of the dripping pills, enterprises mostly judge the dripping state manually according to production experience, and the weight of the dripping pills mostly adopt a traditional balance weighing method. In addition, chinese utility model patent CN 202027925U discloses a full-automatic pill dropping machine with on-line measuring function, this pill dropping machine includes quick-witted case, drip irrigation equipment, the pill dropping host computer of pill device is received in the cooling and is used for in time catching and the high-speed camera on-line measuring system who gathers the instantaneous phenomenon to the whole process of complete shaping from the twinkling of an eye of dripping to the dripping pill system in-process, a pill dropping machine control system for heating, stirring, refrigeration or the circulation part carries out control in the pill dropping host computer according to the information realization pill dropping system process that high-speed camera on-line measuring system provided, and can carry out the condensation post of length adjustment. Compared with the traditional balance weighing method, the pill weight of the dripping pill has certain hysteresis.
The invention aims to provide a laser detection technology based on a laser micrometer, which is used for collecting the width of a dripping liquid drop form in the dripping process of a dripping pill, carrying out data processing on the width value and carrying out correlation analysis on the width value and the weight of the dripping pill to establish an online detection method for dripping the dripping pill.
Disclosure of Invention
In order to overcome the technical problems, the invention provides an online detection method of a dripping pill preparation. The method has the advantages of reasonable design, simple operation, good measurement stability, and good realization of on-line detection of dripping pill.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
an on-line detection method of a dripping pill preparation comprises the following steps:
(1) melting and mixing the dripping pill raw materials and the auxiliary materials uniformly, placing the mixture into a material storage tank of a dripping device, and dripping when the temperature of the material liquid is constant; measuring the width of the liquid drop in the dropping process of the dropping pill by using a detection system;
(2) after data processing, the width of the liquid drop is correlated with the weight of the dripping pill, and a model is established;
(3) and predicting the pill weight of the dropping pill by using a model according to the measured width of the dropping liquid, thereby realizing the on-line detection of the dropping process.
Preferably, the detection system consists of a laser micrometer, a voltage input module and a data recording computer end.
Preferably, the laser micrometer consists of a laser transmitter, a laser receiver and a sensor amplifier.
Preferably, the laser transmitter and the laser receiver are both connected with the sensor amplifier, and transmit and record data to the computer end after passing through the voltage input module.
Preferably, when the detection system is installed, the horizontal positions of the laser transmitter and the laser receiver at the two ends of the dripper are met, and the vertical distance between the laser transmitter and the laser receiver is 5.0-30 mm downward from the dripper after the laser transmitter and the laser receiver are fixed by a mechanical support.
Preferably, the dropping process of the dropping pill is as follows: when the dripping pill is prepared, the mixed liquid medicine is dripped into the condensate through the dripper.
Preferably, the droplet width is all width values that pass through the laser micrometer during the droplet falling process.
Preferably, the data processing method is as follows: dividing the width value according to the drop period of the liquid drop, taking the width value of the liquid drop as the spherical diameter, calculating the volume, and summing all volume values calculated in one drop period, wherein the calculation method comprises the following steps:
Figure BDA0002992558700000021
wherein Dn is the measured drop width, n is the number of all data points with a width value greater than 0.1 in a drop period, and a drop period is the complete process of dropping a drop from a dripper.
During measurement, the position of the laser micrometer is fixed, liquid drops drop from the dripper, and data collected by the micrometer are all data points passing through the micrometer in the dropping process of the liquid drops. Since there is also a baseline noise level when no drop passes, the threshold 0.1 is set to remove the baseline data from the data.
Preferably, the droplet landing period dividing method is to divide the droplet period by setting the threshold value to 0.1 according to the width variation trend detected during the droplet landing.
Preferably, the correlation between the droplet volume and the pill weight of the dropping pill is a linear correlation between the droplet volume and the pill weight of the dropping pill.
Preferably, the online detection is to realize the online detection of the dropping process of the dropping pill by establishing a linear relation between the volume of the dropping pill and the weight of the dropping pill, and predicting the weight of the dropping pill according to the measured width and the calculated volume of the dropping pill.
Compared with the prior art, the invention has the technical advantages that:
1. the invention uses the laser micrometer to measure the width value of the liquid drop in the dropping process of the dropping pill, the established detection system has good stability, the horizontal and vertical distances of the laser micrometer can be adjusted, the method has accurate measurement result and wide applicability, can measure the width change in the dropping process of the liquid drop in real time, and has flexible and simple operation.
2. The method analyzes and processes the measured liquid drop width value, combines the fitted liquid drop volume with the dropping process, establishes the correlation between the liquid drop size and the dropping pill weight, can realize the online detection of the dropping process of the dropping pill, is simple and clear, is economic and practical, is green and environment-friendly, and has certain economic value and research significance.
Drawings
FIG. 1 is a schematic view of a laser detection device in a dropping process of a dropping pill;
FIG. 2 is a schematic view of the laser micrometer installed in a position opposite to the dripper;
FIG. 3 is a graph showing the correlation between the drop volume and the drop weight in the dropping process of the dropping pill in example 1;
FIG. 4 is a graph showing the correlation between the drop volume and the drop weight in the dropping process of a dropping pill in example 2;
FIG. 5 is a graph showing the correlation between the drop volume and the drop weight in the dropping process of a dropping pill in example 3;
FIG. 6 is a graph showing the correlation between the drop volume and the drop weight in the dropping process of a dropping pill in example 4;
FIG. 7 is a graph showing the correlation between the drop volume and the drop weight in the dropping process of a dropping pill in example 5;
FIG. 8 is a graph showing the correlation between the drop volume and the drop weight in the dropping process of a dropping pill in example 6;
FIG. 9 is a graph showing the correlation between the volume of a drop and the weight of a drop obtained in the dropping process of a dropping pill in example 7;
FIG. 10 is a graph showing the correlation between the predicted pill weight and the actual pill weight in the process of dropping the dropping pill in example 8;
FIG. 11 is a graph showing the correlation between the predicted pill weight and the actual pill weight in the process of dropping the dropping pill in example 9;
FIG. 12 is a graph showing the correlation between the predicted pill weight and the actual pill weight in the process of dropping a dripping pill in example 10;
FIG. 13 is a flow chart of on-line detection of dripping pill preparation.
The invention will now be further described with reference to the accompanying drawings and examples:
Detailed Description
The present invention will be described below with reference to specific examples to make the technical aspects of the present invention easier to understand and grasp, but the present invention is not limited thereto. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The following examples are further illustrative of the present invention, but the present invention is not limited thereto.
The detection system is arranged on two sides of the dripping device, and the relative position of the laser micrometer and the dripper is adjusted to select a proper position to measure the width of liquid drops in the dripping process of the dripping pill.
In the embodiment of the invention, the vertical distance between the laser micrometer and the dripper is 5-30 mm.
Example 1
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 80 ℃, after the temperature is kept balanced, adjusting the opening of a valve by a laser micrometer to enable the vertical distance between the laser micrometer and a dripper to be 10mm, carrying out dripping, simultaneously collecting the width value of the dripping pill by the laser micrometer, after the dripping is finished, collecting the dripping pill, weighing and recording the weight of the dripping pill in the dripping process, carrying out data processing on the width value of the dripping pill, and carrying out correlation analysis on the volume of the fitted dripping pill and the weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000041
where Dn is the measured drop width and n is the number of data points with a width value greater than 0.1 in a drop period.
(2) The weight of the dripping pills collected in the experiment in the dripping process is shown in table 1.
TABLE 1
Figure BDA0002992558700000042
(3) Carrying out correlation analysis on the volume of the liquid drop and the pill weight of the dropping pill, and drawing a correlation curveFigure (a). As shown in fig. 3. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is better, R2All are more than 0.95, which shows that the volume value of the selected liquid drop can well represent the change condition of the pill weight of the dropping pill.
Example 2
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 80 ℃, after the temperature is kept balanced, enabling the vertical distance between a laser micrometer and a dripping head to be 15mm, carrying out dripping, simultaneously adopting the laser micrometer to carry out droplet width value acquisition, after dripping is finished, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, carrying out data processing on the droplet width value, and carrying out correlation analysis on the volume of the fitted droplet and the pill weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000051
wherein D isnFor measured drop widths, n is the number of data points for which the width value is greater than 0.1 within a drop period.
(2) The weight of the dripping pills collected in the experiment during the dripping process is shown in table 2.
TABLE 2
Figure BDA0002992558700000052
(3) And (4) carrying out correlation analysis on the volume of the liquid drop and the weight of the dripping pill, and drawing a correlation curve chart. As shown in fig. 4. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is good, and R2 is greater than 0.95, which indicates that the selected drop volume value can well represent the change condition of the drop pill weight.
Example 3
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 80 ℃, after the temperature is kept balanced, enabling the vertical distance between a laser micrometer and a dripper to be 20mm, carrying out dripping, simultaneously adopting the laser micrometer to carry out droplet width value acquisition, after dripping is finished, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, carrying out data processing on the droplet width value, and carrying out correlation analysis on the fitted droplet volume and the pill weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000053
wherein D isnFor measured drop widths, n is the number of data points for which the width value is greater than 0.1 within a drop period.
(2) The weight of the dripping pills collected in the experiment during the dripping process is shown in table 3.
TABLE 3
Figure BDA0002992558700000054
(3) And (4) carrying out correlation analysis on the volume of the liquid drop and the weight of the dripping pill, and drawing a correlation curve chart. As shown in fig. 5. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is better, R2All are more than 0.98, which shows that the volume value of the selected liquid drop can well represent the change condition of the pill weight of the dropping pill.
Example 4
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 80 ℃, after the temperature is kept balanced, enabling the vertical distance between a laser micrometer and a dripping head to be 25mm, carrying out dripping, simultaneously adopting the laser micrometer to carry out droplet width value acquisition, after dripping is finished, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, carrying out data processing on the droplet width value, and carrying out correlation analysis on the volume of the fitted droplet and the pill weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000061
wherein D isnFor measured drop widths, n is the number of data points for which the width value is greater than 0.1 within a drop period.
(2) The weights of the pills collected in the experiment during the dripping process are shown in Table 4.
TABLE 4
Figure BDA0002992558700000062
(3) And (4) carrying out correlation analysis on the volume of the liquid drop and the weight of the dripping pill, and drawing a correlation curve chart. As shown in fig. 6. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is better, R2All are more than 0.98, which shows that the volume value of the selected liquid drop can well represent the change condition of the pill weight of the dropping pill.
Example 5
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 70 ℃, after the temperature is kept balanced, enabling the vertical distance between a laser micrometer and a dripper to be 20mm, carrying out dripping, simultaneously adopting the laser micrometer to carry out droplet width value acquisition, after dripping is finished, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, carrying out data processing on the droplet width value, and carrying out correlation analysis on the fitted droplet volume and the pill weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000063
wherein D isnFor measured drop widths, n is the number of data points for which the width value is greater than 0.1 within a drop period.
(2) The weight of the dripping pills collected in the experiment during the dripping process is shown in table 5.
TABLE 5
Figure BDA0002992558700000071
(3) And (4) carrying out correlation analysis on the volume of the liquid drop and the weight of the dripping pill, and drawing a correlation curve chart. As shown in fig. 7. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is better, R2All are more than 0.99, which shows that the volume value of the selected liquid drop can well represent the change condition of the pill weight of the dropping pill.
Example 6
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 90 ℃, after the temperature is kept balanced, enabling the vertical distance between a laser micrometer and a dripper to be 20mm, carrying out dripping, simultaneously adopting the laser micrometer to carry out droplet width value acquisition, after dripping is finished, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, carrying out data processing on the droplet width value, and carrying out correlation analysis on the fitted droplet volume and the pill weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000072
wherein D isnFor measured drop widths, n is the number of data points for which the width value is greater than 0.1 within a drop period.
(2) The weight of the dripping pills collected in the experiment during the dripping process is shown in table 6.
TABLE 6
Figure BDA0002992558700000073
(3) And (4) carrying out correlation analysis on the volume of the liquid drop and the weight of the dripping pill, and drawing a correlation curve chart. As shown in fig. 8. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is better, R2Are all greater than 0.98, indicating selected drop volume valuesCan well represent the change condition of the pill weight of the dropping pill.
Example 7
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 100 ℃, after the temperature is kept balanced, enabling the vertical distance between a laser micrometer and a dripper to be 20mm, carrying out dripping, simultaneously adopting the laser micrometer to carry out droplet width value acquisition, after dripping is finished, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, carrying out data processing on the droplet width value, and carrying out correlation analysis on the fitted droplet volume and the pill weight of the dripping pill. The method comprises the following specific steps:
(1) and (3) carrying out volume fitting on the width of the collected liquid drop according to a formula:
Figure BDA0002992558700000081
wherein D isnFor measured drop widths, n is the number of data points for which the width value is greater than 0.1 within a drop period.
(2) The weight of the dripping pills collected in the experiment during the dripping process is shown in table 7.
TABLE 7
Figure BDA0002992558700000082
(3) And (4) carrying out correlation analysis on the volume of the liquid drop and the weight of the dripping pill, and drawing a correlation curve chart. As shown in fig. 9. As can be seen from the figure, the correlation between the fitted drop volume and the drop pill weight is better, R2All are more than 0.99, which shows that the volume value of the selected liquid drop can well represent the change condition of the pill weight of the dropping pill.
Example 8
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 80 ℃, after the temperature is kept balanced, continuously dripping, simultaneously collecting the width value of a liquid drop by using a laser micrometer, calculating the change trend of the weight of the dripping pill in the dripping process according to the correlation between the volume of the liquid drop established at 80 ℃ and the weight of the pill, after the dripping is finished, collecting the dripping pill, weighing and recording the weight of the dripping pill in the dripping process, and comparing the predicted weight of the dripping pill with the actual weight of the dripping pill, as shown in figure 10.
Example 9
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 90 ℃, after the temperature is kept balanced, continuously dripping with a laser micrometer with the vertical distance of 20mm from a dripper, simultaneously collecting the width value of the dripping by adopting the laser micrometer, calculating the change trend of the pill weight in the dripping process according to the correlation between the volume of the dripping and the pill weight, after finishing dripping, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, and comparing the predicted pill weight of the dripping pill with the actual pill weight, as shown in figure 11.
Example 10
Adding the uniformly mixed dripping pill raw and auxiliary materials into a liquid storage tank of a dripping device, heating to 100 ℃, after the temperature is kept balanced, continuously dripping with a laser micrometer with the vertical distance of 20mm from a dripper, simultaneously collecting the width value of the dripping by adopting the laser micrometer, calculating the change trend of the pill weight in the dripping process according to the correlation between the volume of the dripping and the pill weight, after finishing dripping, collecting the dripping pill, weighing and recording the pill weight in the dripping process of the dripping pill, and comparing the predicted pill weight of the dripping pill with the actual pill weight, as shown in figure 12.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.

Claims (2)

1. An on-line detection method of a dripping pill preparation comprises the following steps:
(1) melting and mixing the dripping pill raw materials and the auxiliary materials uniformly, placing the mixture into a material storage tank of a dripping device, and dripping when the temperature of the material liquid is constant; measuring the width of the liquid drop in the dropping process of the dropping pill by using a detection system;
(2) after the width of the liquid drop is processed by data, establishing a model, and establishing a linear relation between the V value obtained by the model and the weight of the dripping pill;
(3) calculating the V value by using a model according to the measured liquid drop width through the established linear relation between the V value and the weight of the dripping pills, predicting the weight of the dripping pills and realizing the on-line detection in the dripping process;
the detection system consists of a laser micrometer, a voltage input module and a data recording computer end; the laser micrometer consists of a laser transmitter, a laser receiver and a sensor amplifier;
when the detection system is installed, the horizontal positions of the laser transmitter and the laser receiver are positioned at two ends of the dripper, and the vertical distance between the laser transmitter and the laser receiver is 5.0-30.0 mm downward from the dripper after the laser transmitter and the laser receiver are fixed by the mechanical support;
the dripping process of the dripping pill comprises the following steps: when the dripping pill is prepared, the mixed liquid medicine is dripped into the condensate through a dripper;
the width of the liquid drop is all width values of the liquid drop passing through a laser micrometer in the falling process;
the data processing method comprises the following steps: dividing the width value according to the drop period of the liquid drop, fitting the width value of the liquid drop as a spherical diameter, calculating the volume, and summing all volume values calculated in one drop period, wherein the calculation method comprises the following steps:
Figure 112301DEST_PATH_IMAGE001
wherein D isiFor the measured width of the liquid drop, n is all data points with the width value larger than 0.1mm in one liquid drop period, and the one liquid drop period refers to the complete process of the liquid drop falling from the water dropper;
the method for dividing the dropping period of the liquid drops is to divide the dropping period by setting the threshold value to be 0.1mm according to the width variation trend detected in the dropping process of the liquid drops.
2. The method for on-line detection of dripping pill preparation of claim 1, wherein the laser transmitter and laser receiver are connected to the sensor amplifier, and after passing through the voltage input module, the data is transmitted and recorded to the data recording computer.
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