Quality control equipment and method for multivitamins for injection

Abstract

The invention discloses a quality control device and method for multivitamins for injection, and relates to the technical field of vitamin preparation, the technical key points are as follows: the quality control device comprises a sample collection mechanism, a liquid guide tube, an electromagnetic metering valve and a test tube transfer assembly; the sample pretreatment mechanism is provided with a stirring assembly and an automatic dilution assembly, and the automatic dilution assembly comprises a high-precision capacity metering device and a flow control valve; the high performance liquid chromatography detection mechanism is provided with a plurality of chromatographic columns, a mobile phase conveying system containing a high-pressure pump, a detection wavelength adjusting device, an automatic sample injector and a data processing system; the atomic absorption spectrometry detection mechanism is provided with a hollow cathode lamp; the infrared spectroscopy detection mechanism is provided with an interferometer and a detector; the quality control process management system is constructed based on a programmable logic controller and an industrial computer and is provided with a state indicator lamp and an alarm device; the online quality monitoring system comprises a data processing unit and a network communication unit; according to the invention, convenience can be ensured, and efficiency and automation degree are improved.

Description

Technical Field

[0001] This invention relates to the field of vitamin preparation technology, and in particular to a quality control device and method for injectable multivitamins. Background Technology

[0002] Injectable multivitamins (12) play an irreplaceable and important role in clinical nutritional support as an intravenous parenteral nutrition solution. Its scientifically formulated composition covers nine water-soluble vitamins (including vitamins B1, B2, B6, B12, vitamin C, nicotinamide, dextropanthenol, biotin, and folic acid) and three fat-soluble vitamins (vitamins A, D, and E) essential for metabolism in adults and children over 11 years of age, excluding vitamin K. This provides comprehensive and balanced vitamin support, meeting the vitamin needs of patients under different physiological and pathological conditions. The market demand for parenteral nutrition drugs is enormous, and injectable multivitamins (12), as an important parenteral nutrition supplement, has broad market application prospects.

[0003] Injectable multivitamins (12) have many significant advantages that make them stand out in the market competition. First, they are highly stable. As a powder injection preparation, they have a long shelf life and can maintain excellent stability when added to binary or ternary mixtures of parenteral nutrition solutions, ensuring the quality and longevity of the product's efficacy. Second, they are highly safe. They do not contain VK1, which avoids interference with anticoagulation therapy during clinical use. At the same time, they contain fewer excipients, reducing some safety hazards caused by excipients and providing strong protection for patients' medication safety. Compared with ordinary fat-soluble and water-soluble vitamins, its biggest feature is that fat-soluble vitamins and water-soluble vitamins can be dissolved in the same container, which can maintain their injectability in the final preparation while being preserved, better meeting different clinical needs. At present, the main products that directly compete with this product are water-soluble vitamins for injection, fat-soluble vitamins for injection, and multivitamins for injection (13), but the market share of this product has been increasing year by year, and it has gradually replaced the former two, occupying an important position in the field of intravenous vitamin supplements.

[0004] Market sales data shows that injectable multivitamins (12) are performing strongly. Internationally, this product was first launched in Germany in 1992, and the original manufacturer was imported into China on October 29, 1999. The licensee was Baxter SA, and the specification was 5ml / vial, with the trade name Cernevit®. However, the existing technical solutions for quality control of injectable multivitamins are not convenient enough, and the degree of automation and efficiency need to be improved. Summary of the Invention

[0005] In order to at least solve one of the above-mentioned technical problems, the present invention aims to provide a quality control device and method for injectable multivitamins, which ensures convenience and improves efficiency and automation.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A quality control device for injectable multivitamins, comprising:

[0008] The sample collection mechanism includes a liquid guide tube for guiding the finished multivitamin injection solution, the liquid guide tube being equipped with an electromagnetic metering valve, and a test tube transfer assembly for fixing and moving the sample tube.

[0009] The sample pretreatment mechanism includes a stirring assembly and an automatic dilution assembly, wherein the automatic dilution assembly is equipped with a high-precision volume metering device and a flow control valve;

[0010] A high-performance liquid chromatography (HPLC) detection system includes various chromatographic columns, a mobile phase delivery system, a detection wavelength adjustment device, an automated sampler, and a data processing system, wherein the mobile phase delivery system includes a high-pressure pump.

[0011] Atomic absorption spectrometry detection equipment, including hollow cathode lamps;

[0012] Infrared spectroscopy detection equipment includes interferometers and detectors;

[0013] The quality control process management system is built on a programmable logic controller and an industrial computer, and is equipped with status indicator lights and alarm devices.

[0014] The online quality monitoring system includes a data processing unit, which is signal-connected to the high-performance liquid chromatography detection mechanism, the atomic absorption spectrometry detection mechanism, and the infrared spectroscopy detection mechanism. The data processing unit is also signal-connected to a network communication unit.

[0015] Preferably, the stirring assembly uses a Teflon-material magnetic stir bar in conjunction with an external magnetic drive device; the flow control valve is an electromagnetic proportional valve; the external magnetic drive device of the stirring assembly uses a brushless motor; and the flow control valve of the automatic dilution assembly is a piezoelectric-driven electromagnetic proportional valve.

[0016] Preferably, the brushless motor speed is adjustable from 0 to 2000 rpm, and the radius of the stir bar rotation trajectory is adjustable from 5 to 30 mm; the piezoelectric driven electromagnetic proportional valve has a response time ≤20 ms and a repeatability of ±5%; a reversed-phase chromatography column is used for the detection of water-soluble vitamins, and the reversed-phase chromatography column packing is C18 bonded silica with a particle size of 5 μm; a normal-phase chromatography column or a special-function chromatography column is used for the detection of fat-soluble vitamins, and the normal-phase chromatography column packing is silica with a particle size of 3 to 10 μm.

[0017] Preferably, the high-pressure pump has a pressure range of 0-40 MPa; the detection wavelength adjustment device adopts grating spectral dispersion technology; the automated sampler adopts a robotic arm-type sample introduction structure; and the data processing system is built based on hardware circuits and embedded chips.

[0018] Preferably, the sample collection mechanism's liquid guide tube is made of medical-grade silicone material, and the inner wall is treated with an anti-adsorption coating; the electromagnetic metering valve has a flow control accuracy of ±1μL and a response time of ≤50ms; the test tube transfer assembly uses a six-axis robotic arm and a vision positioning system, with a positioning accuracy of ≤0.5mm and a gripping force adjustment range of 10-500g.

[0019] Preferably, the hollow cathode lamp adopts a pulse power supply mode, the lamp current is adjustable from 1 to 10mA, and the stability is ≤5%; the infrared spectroscopy detection mechanism adopts a Michelson interferometer and a mercury cadmium telluride cooled detector, with ≥32 scans, resolution ≤4cm⁻¹, and signal-to-noise ratio ≥5000:1.

[0020] Preferably, the quality control process management system adopts a PLC and industrial computer architecture, the status indicator is a three-color LED, the alarm device supports sound and light synchronization, and the response time is ≤2s; the online monitoring system network communication unit adopts the industrial Ethernet protocol, the transmission rate is ≥100Mbps, and it supports remote control.

[0021] A quality control method for injectable multivitamins includes the following steps:

[0022] Sample collection and pretreatment steps: The sample collection mechanism is activated, and the multivitamin injection solution is introduced into the sample tube through the liquid delivery tube. The volume of the collected injection solution is precisely controlled using an electromagnetic metering valve. The sample tube transfer assembly fixes and moves the sample tube, transferring the sample tube containing the injection solution to the sample pretreatment mechanism. In the sample pretreatment mechanism, the stirring assembly is activated to thoroughly stir the injection solution. The automatic dilution assembly is activated, using a high-precision volumetric metering device to determine the volume of the diluent, and the flow rate of the diluent is precisely controlled using a flow control valve to add the diluent to the injection solution for dilution.

[0023] High-performance liquid chromatography (HPLC) detection steps: Select an appropriate chromatographic column according to the type of vitamin to be detected. For water-soluble vitamins, use a reversed-phase column; for fat-soluble vitamins, use a normal-phase column or a special-function column. Start the mobile phase delivery system and use a high-pressure pump to deliver the mobile phase to the column. Adjust the detection wavelength to a suitable range using the detection wavelength adjustment device. Inject the pretreated sample into the column using an automated sampler. After separation in the column, the sample enters the detector. The data processing system processes and analyzes the detection signal to obtain relevant data on vitamin composition.

[0024] Atomic absorption spectrometry detection steps: Start the atomic absorption spectrometry detection mechanism, and the hollow cathode lamp emits characteristic spectral lines; introduce the pretreated sample into the atomic absorption spectrometry detection area, and the atomic vapor in the sample absorbs the characteristic spectral lines; the detector detects the intensity of the absorbed spectral lines, and the data processing system processes and analyzes the detection data to obtain the content information of relevant elements in the sample;

[0025] Infrared spectroscopy detection steps: Start the infrared spectroscopy detection mechanism; place the pretreated sample in the detection area, and the interferometer modulates the infrared light emitted by the sample; the detector receives the infrared light signal after interference; the data processing system processes the signal received by the detector to obtain the infrared spectrum of the sample and analyze information such as functional groups in the sample;

[0026] Quality control process management and online monitoring steps: The quality control process management system operates, displaying the equipment's operating status in real time through status indicator lights. When an abnormality occurs, an alarm device sounds. The data processing unit of the online quality monitoring system receives real-time detection data from high-performance liquid chromatography (HPLC), atomic absorption spectrometry (AAS), and infrared spectroscopy (IR) testing institutions. The data processing unit comprehensively analyzes and processes the received data, transmitting the detection results to the remote control terminal via network communication, while also supporting remote control of equipment operation and parameter adjustments.

[0027] Results Judgment and Recording Steps: Based on the preset quality standards, analyze and judge the various data obtained from the testing steps to determine whether the quality of the injectable multivitamins is up to standard; record all data and judgment results of the testing process in detail.

[0028] Preferably, in the sample collection and pretreatment step, the sample collection mechanism includes a liquid guide tube, a sample tube, an electromagnetic metering valve, and a test tube transfer assembly, and the sample pretreatment mechanism includes a stirring assembly, an automatic dilution assembly, a high-precision volumetric metering device, and a flow control valve.

[0029] Preferably, in the high-performance liquid chromatography detection step, the mobile phase delivery system includes a high-pressure pump; in the quality control process management and online monitoring step, the online quality monitoring system includes a data processing unit and a network communication unit.

[0030] The present invention has the following beneficial effects:

[0031] I. Significantly Enhanced Convenience: The quality control equipment of this invention features a sophisticated design in the sample collection and pretreatment stages, greatly improving operational convenience. In the sample collection mechanism, the liquid guide tube, made of medical-grade silicone with an anti-adsorption coating on its inner wall, guides the multivitamin injection solution, ensuring the sample remains uncontaminated during collection and guaranteeing its purity. The electromagnetic metering valve achieves a flow control accuracy of ±1μL and a response time ≤50ms, precisely controlling the collected injection volume and avoiding errors caused by manual operation. The test tube transfer assembly utilizes a six-axis robotic arm and a vision positioning system, achieving a positioning accuracy ≤0.05mm and a gripping force adjustment range of 10-500g. This allows for accurate fixation and movement of the sample tubes, quickly transferring the sample tubes containing the injection solution to the sample pretreatment mechanism, reducing the tedious manual handling process and improving the convenience of sample collection and transfer. For sample pretreatment, the stirring assembly uses a Teflon magnetic stir bar in conjunction with an external magnetic drive device. The external magnetic drive device uses a brushless motor with an adjustable speed of 0-2000 rpm, and the stir bar's rotation radius is adjustable from 5-30 mm. The stirring parameters can be flexibly adjusted according to the characteristics of different samples to achieve thorough mixing of the injection solution. The automatic dilution assembly is equipped with a high-precision volumetric metering device and a flow control valve. The flow control valve is a piezoelectric-driven electromagnetic proportional valve with a response time ≤20ms and a repeatability of ±5%, accurately controlling the diluent flow rate and precisely adding the diluent to the injection solution for dilution. The entire pretreatment process is highly automated and easy to operate.

[0032] II. Significantly Improved Efficiency: This invention improves the efficiency of quality control for injectable multivitamins in several aspects. In the detection stage, the high-performance liquid chromatography (HPLC), atomic absorption spectrometry (AAS), and infrared spectroscopy (IR) detection mechanisms work collaboratively to simultaneously detect different components in the sample. In the HPLC detection mechanism, the high-pressure pump of the mobile phase delivery system operates within a pressure range of 0-40 MPa, rapidly delivering the mobile phase to the chromatographic column and improving sample separation speed. The detection wavelength adjustment device employs grating spectrophotometry technology, enabling rapid and accurate adjustment of the detection wavelength to the appropriate range. The automated sampler uses a robotic arm-type injection structure, automatically injecting pretreated samples into the chromatographic column, reducing the time consumed by manual sample injection. In the AAS detection mechanism, the hollow cathode lamp uses a pulsed power supply mode with an adjustable lamp current of 1-10 mA and a stability of ≤5%, rapidly emitting stable characteristic spectral lines and improving detection efficiency. The infrared spectroscopy detection unit employs a Michelson interferometer and a mercury cadmium telluride cooled detector, performing ≥32 scans with a resolution ≤4cm⁻¹ and a signal-to-noise ratio ≥5000:1. This allows for rapid acquisition of the infrared spectrum of samples and analysis of functional groups and other information. Furthermore, the quality control process management system, built on a programmable logic controller and an industrial computer, monitors equipment operation in real time. In case of abnormalities, the alarm response time is ≤2 seconds, promptly notifying operators to handle the situation and preventing detection delays caused by equipment malfunctions. The online quality monitoring system's data processing unit receives and comprehensively analyzes the detection data from each testing unit. Through a network communication unit (using industrial Ethernet protocol, transmission rate ≥100Mbps), the detection results are rapidly transmitted to the remote control terminal. This also supports remote control of equipment operation and parameter adjustments, further improving the efficiency of quality control.

[0033] III. Enhanced Automation: The quality control equipment and method of this invention achieve a high degree of automation. The sample collection mechanism automatically controls the injection volume through an electromagnetic metering valve, and the test tube transfer assembly automatically fixes and moves the sample tubes. In the sample pretreatment mechanism, the stirring assembly and automatic dilution assembly automatically stir and dilute the samples without manual intervention. The high-performance liquid chromatography (HPLC) detection mechanism automatically selects the appropriate chromatographic column according to the type of vitamin to be detected. The mobile phase delivery system, detection wavelength adjustment device, and automatic sample injector all operate automatically, achieving automatic sample separation and detection. The atomic absorption spectrometry (AAS) and infrared spectroscopy (IR) detection mechanisms can also automatically complete the detection process. The data processing system automatically processes and analyzes the detection signals to obtain relevant data and information. The quality control process management system operates automatically, displaying the equipment operating status in real time through status indicator lights and automatically alarming when abnormalities occur. The online quality monitoring system automatically receives the detection data from each detection mechanism, performs comprehensive analysis and processing, and transmits the detection results to the remote control terminal, supporting remote control of equipment operation and parameter adjustment. The entire quality control process, from sample collection and pretreatment to testing, result analysis, and transmission, is automated, reducing the workload and errors of manual operations and improving the accuracy and reliability of quality control.

[0034] IV. Unique Combined Effects: The quality control equipment of this invention integrates multiple advanced detection technologies (high-performance liquid chromatography, atomic absorption spectrometry, and infrared spectroscopy) into a comprehensive quality control system. High-performance liquid chromatography can accurately separate and detect vitamin components in samples, atomic absorption spectrometry can accurately determine the content of relevant elements in samples, and infrared spectroscopy can analyze information such as functional groups in samples. These three detection technologies complement each other, enabling a comprehensive evaluation of the quality of injectable multivitamins from different perspectives, improving the accuracy and comprehensiveness of quality testing. Simultaneously, the addition of a quality control process management system and an online quality monitoring system enables real-time monitoring and management of the entire quality control process, allowing for timely detection and handling of anomalies, ensuring the smooth operation of quality control. This unique combination of multiple detection technologies and management systems gives this invention significant advantages in the quality control of injectable multivitamins, better meeting the market demand for high-quality vitamin products. Attached Figure Description

[0035] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0036] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the present invention.

[0037] Figure 2 This is a flowchart of an embodiment of the present invention.

[0038] In the diagram: 101, liquid guide tube; 102, electromagnetic metering valve; 2, test tube transfer assembly; 201, stirring assembly; 202, automatic dilution assembly; 301, mobile phase delivery system; 302, detection wavelength adjustment device; 303, automatic sampler; 4, hollow cathode lamp; 5, interferometer; 601, industrial computer; 602, status indicator light; 603, alarm device. Detailed Implementation

[0039] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0040] like Figure 1 As shown, a quality control device for injectable multivitamins includes:

[0041] The sample collection mechanism includes a liquid guide tube 101 for guiding the finished multivitamin injection solution, an electromagnetic metering valve 102 is provided on the liquid guide tube 101, and a test tube transfer assembly 2 for fixing and moving the sample tube.

[0042] The sample pretreatment mechanism includes a stirring assembly 201 and an automatic dilution assembly 202. The automatic dilution assembly 202 is equipped with a high-precision volume metering device and a flow control valve.

[0043] The high-performance liquid chromatography detection system includes multiple chromatographic columns, a mobile phase delivery system 301, a detection wavelength adjustment device 302, an automated sampler 303, and a data processing system. The mobile phase delivery system 301 includes a high-pressure pump.

[0044] Atomic absorption spectrometry detection apparatus, including a hollow cathode lamp 4;

[0045] The infrared spectroscopy detection mechanism includes an interferometer 5 and a detector;

[0046] The quality control process management system is built on a programmable logic controller and an industrial computer 601, and is equipped with status indicator lights 602 and alarm devices 603.

[0047] The online quality monitoring system includes a data processing unit, which is connected to the high-performance liquid chromatography (HPLC) detection mechanism, the atomic absorption spectrometry (AAS) detection mechanism, and the infrared spectroscopy (IR) detection mechanism. The data processing unit is also connected to a network communication unit.

[0048] like Figure 1 As shown, the multivitamin injection solution is guided by the liquid guide tube 101, the electromagnetic metering valve 102 precisely controls the amount of sample collected, and the test tube transfer assembly 2 fixes and moves the sample tube containing the sample, accurately delivering the sample to the subsequent processing stage. The stirring assembly 201 stirs the collected sample to ensure uniform distribution of sample components; the automatic dilution assembly 202 uses a high-precision volumetric metering device to accurately measure the amount of diluent, and controls the addition rate of diluent through a flow control valve to achieve accurate dilution of the sample to meet the requirements of subsequent detection. Multiple chromatographic columns separate the different vitamin components according to their characteristics; the high-pressure pump delivers the mobile phase in the mobile phase delivery system 301 at high pressure, carrying the sample through the chromatographic column. Different components separate at different rates in the chromatographic column, thus achieving separation; the automatic sampler 303 accurately injects the pretreated sample into the mobile phase; the detection wavelength adjustment device 302 adjusts the detection wavelength according to the absorption characteristics of different vitamins, the detector detects the absorption of each component after separation by the chromatographic column at a specific wavelength, and transmits the signal to the data processing system. The data processing system analyzes and processes the signal to obtain the content information of each vitamin component.

[0049] A hollow cathode lamp 4 emits characteristic spectral lines of specific elements. The atomic vapor of the element to be measured in the sample absorbs these characteristic spectral lines, and the content of the corresponding element in the sample is determined by measuring the degree of absorption. An interferometer 5 splits the light emitted by the infrared light source into two beams, forming interference light. After the interference light illuminates the sample, the sample molecules absorb infrared light of a specific frequency, producing an interference pattern. The detector detects the interference pattern and converts it into an electrical signal. After processing, the infrared spectrum of the sample is obtained, and the structural information of each component in the sample is determined by analyzing the infrared spectrum. A programmable logic controller (PLC) and an industrial computer 601 control and manage the entire quality control process. A status indicator 602 displays the equipment's operating status, and an alarm device 603 issues an alarm in case of abnormalities, reminding operators to handle the situation promptly. The data processing unit receives signals from the high-performance liquid chromatography (HPLC), atomic absorption spectrometry (AAS), and infrared spectroscopy (IR) detection mechanisms, performs comprehensive analysis and processing of the data, and determines whether the sample quality is up to standard. The network communication unit transmits the monitoring results to a remote terminal for remote monitoring.

[0050] like Figure 1As shown, the stirring assembly 201 uses a Teflon magnetic stir bar in conjunction with an external magnetic drive device. The external brushless motor, as the core component of the magnetic drive device, generates a rotating magnetic field when energized. This rotating magnetic field acts on the Teflon magnetic stir bar, causing it to rotate synchronously with the magnetic field. During sample pretreatment, the stir bar rotates within the sample tube, stirring the multivitamin injection sample and ensuring uniform distribution of components, providing favorable sample conditions for subsequent accurate detection. The automatic dilution assembly 202 employs a piezoelectric-driven electromagnetic proportional valve, achieving precise flow control through the inverse piezoelectric effect of the piezoelectric element. When a voltage is applied to the piezoelectric element, it deforms, driving the valve core to move and thus changing the valve opening. By adjusting the magnitude and frequency of the voltage applied to the piezoelectric element, the movement distance and speed of the valve core can be precisely controlled, thereby precisely controlling the flow rate of the diluent. The electromagnetic proportional valve has a response time of ≤20ms, enabling it to respond quickly to control signals and has a repeatability of ±5%, ensuring the accuracy and consistency of the amount of diluent added each time, thus achieving accurate dilution of various vitamin injection samples.

[0051] like Figure 1 As shown, for the detection of water-soluble vitamins, a reversed-phase chromatographic column was used, with C18 bonded silica gel as the packing material and a particle size of 5 μm. The sample solution entered the reversed-phase chromatographic column under the action of the mobile phase delivery system 301 (powered by a high-pressure pump). Due to the hydrophobic surface of the C18 bonded silica gel, the interaction force between water-soluble vitamin molecules and the stationary phase is weak, while the mobile phase (usually a mixture of water and organic solvents) has a strong dissolving and carrying capacity for water-soluble vitamin molecules. The different interactions between different water-soluble vitamin molecules and the stationary and mobile phases in the chromatographic column lead to different retention times, thus achieving separation. The separated water-soluble vitamin molecules sequentially enter the detector, which detects each molecule based on its characteristic absorption properties and transmits the signal to the data processing system for analysis, obtaining the content information of each water-soluble vitamin component.

[0052] For the detection of fat-soluble vitamins, normal-phase or specialized functional columns are used. Normal-phase columns are packed with silica gel with a particle size of 3-10 μm. In normal-phase chromatography, the silica gel stationary phase has a polar surface, resulting in strong interactions between fat-soluble vitamin molecules and the stationary phase (such as van der Waals forces and dipole-dipole interactions). The mobile phase (usually a nonpolar or weakly polar solvent) has a relatively weak ability to dissolve and carry fat-soluble vitamin molecules. Different fat-soluble vitamin molecules interact with the stationary phase at different strengths, resulting in different retention times in the column, thus achieving separation. Specialized functional columns are designed specifically for the properties of fat-soluble vitamins, providing more targeted separation capabilities. The separated fat-soluble vitamin molecules are then detected by a detector, and the data processing system analyzes and processes the signals to obtain the content information of each component of the fat-soluble vitamin.

[0053] like Figure 1 As shown, the pressure range of the pump is 0-40 MPa. In a high-performance liquid chromatography (HPLC) detection system, it provides the power for the delivery of the mobile phase. Through high pressure, the mobile phase passes through the chromatographic column at a stable flow rate and pressure. Samples with different components enter the column under the carrying force of the mobile phase. Due to the different interactions between each component and the stationary phase of the column, separation is achieved within the column. The high-pressure pump ensures a stable and continuous delivery of the mobile phase, providing excellent conditions for chromatographic separation and ensuring the accuracy and repeatability of the detection results.

[0054] The detection wavelength adjustment device 302 employs grating beam splitting technology. The composite light emitted from the light source illuminates the grating, which then splits the light according to its wavelength, separating different wavelengths. By rotating the grating or changing its relative position to the detector, a specific wavelength of light can be selected to enter the detector. When detecting multiple vitamins, different vitamin components have specific absorption peaks at different wavelengths. By adjusting the detection wavelength, the detector can detect at the absorption peak wavelength of the corresponding vitamin, thereby accurately measuring the content of each vitamin component in the sample.

[0055] The automated sampler 303 employs a robotic arm-type injection structure. The robotic arm has multiple degrees of freedom, enabling precise movement to the sample location. During injection, the robotic arm accurately grasps the sample container and moves it to the injection port of the high-performance liquid chromatography (HPLC) detection unit, injecting the sample into the mobile phase. This injection method offers a high degree of automation, reducing errors caused by manual operation and improving the accuracy and efficiency of injection.

[0056] like Figure 1As shown, the data processing system is built upon hardware circuits and embedded chips. The hardware circuits are responsible for acquiring signals from detection equipment such as high-performance liquid chromatography (HPLC), atomic absorption spectrometry (AAS), and infrared spectroscopy (IR), and performing preprocessing such as amplification and filtering. The embedded chip has powerful computing and storage capabilities, enabling further analysis and processing of the preprocessed signals, such as data fitting, peak area calculation, and component content calculation. Simultaneously, the embedded chip can control the entire operation of the quality control equipment, achieving automated control and intelligent management.

[0057] like Figure 1 As shown, the liquid guide tube 101 is made of medical-grade silicone, and its inner wall is treated with an anti-adsorption coating. Medical-grade silicone has good biocompatibility and chemical stability, and will not contaminate various vitamin injection samples. The anti-adsorption coating on the inner wall prevents components in the sample from adsorbing onto the inner wall of the liquid guide tube 101, ensuring that the collected sample composition is consistent with the actual sample and improving the accuracy of sample collection.

[0058] The electromagnetic metering valve 102 has a flow control accuracy of ±1μL and a response time of ≤50ms. During sample collection, the electromagnetic metering valve 102 can precisely control the amount of sample collected. By adjusting the valve opening, the sample flow rate passing through per unit time is accurately controlled to the set value, ensuring that the sample volume error for each collection is within ±1μL. The fast response time allows for timely adjustment of the flow rate based on the control signal, ensuring the stability and accuracy of sample collection.

[0059] The test tube transfer assembly 2 employs a six-axis robotic arm and a vision positioning system, achieving a positioning accuracy of ≤0.05mm and a gripping force adjustable from 10 to 500g. The six-axis robotic arm has six degrees of freedom, enabling flexible movement and rotation in three-dimensional space to achieve complex trajectories. The vision positioning system acquires the test tube's position information via a camera, processes and analyzes the image to determine the test tube's precise location, and feeds this information back to the six-axis robotic arm. Based on the feedback from the vision positioning system, the six-axis robotic arm precisely moves to the test tube's position and uses an appropriate gripping force (adjustable within the 10-500g range) to grasp the test tube and move it to the designated location, completing the test tube transfer operation.

[0060] like Figure 1As shown, the hollow cathode lamp 4 employs a pulsed power supply mode. Compared to traditional DC power supply, pulsed power supply can provide a large current pulse in a short time, rapidly ionizing the gas inside the lamp and generating high-intensity characteristic spectral lines. During each pulse interval, the gas inside the lamp has a recovery time, reducing electrode sputtering and thermal effects, thereby extending the lamp's lifespan and improving the stability and intensity of the spectral lines. The lamp current is adjustable from 1 to 10 mA. By adjusting the current, the degree of ionization of the gas inside the lamp can be controlled, thus adjusting the intensity of the characteristic spectral lines to meet the needs of different detection sensitivities and sample concentrations. Stability ≤5% ensures minimal fluctuations in the intensity of the characteristic spectral lines output by the hollow cathode lamp 4 during detection, providing a stable light source for atomic absorption spectrometry and improving the accuracy of the detection results. When the characteristic spectral lines emitted by the hollow cathode lamp 4 pass through the sample vapor, the ground-state atoms of the analyte in the sample absorb spectral lines of specific wavelengths. By measuring the change in spectral line intensity before and after absorption, the content of the analyte in the sample can be calculated according to the Lambert-Beer law.

[0061] like Figure 1 As shown, the Michelson interferometer 5 mainly consists of a beam splitter, a fixed mirror, and a moving mirror. Infrared light emitted from the light source is split into two beams by the beam splitter. One beam is directed to the fixed mirror and returns to the beam splitter after reflection; the other beam is directed to the moving mirror, which moves at a certain speed and also returns to the beam splitter after reflection. The two returning beams re-merge at the beam splitter. Due to the movement of the moving mirror, the optical path difference between the two beams changes continuously, resulting in interference. The interference light signal contains information about the sample's absorption of infrared light. By detecting the change of the interference light signal over time and performing mathematical processing such as Fourier transform, the infrared spectrum of the sample can be obtained. Mercury cadmium telluride (MCT) is a semiconductor material sensitive to infrared light. When infrared light shines on the MCT detector, electron-hole pairs are generated, forming a photocurrent. Lowering the detector's temperature using a cooling device reduces thermal noise and improves the signal-to-noise ratio and sensitivity. The detector converts the received infrared light signal into an electrical signal, which is then transmitted to the subsequent data processing system for analysis. The system requires at least 32 scans. Multiple scans allow for repeated measurements of the same sample, and averaging the results effectively reduces random errors and improves the accuracy and repeatability of the detection results. A resolution of ≤4 cm⁻¹ is crucial. Higher resolution distinguishes more finely the infrared spectral peaks, enabling more accurate identification of characteristic absorption peaks of different functional groups and chemical bonds in the sample, thus facilitating more precise analysis of the sample's composition and structure. A signal-to-noise ratio (SNR) of ≥5000:1 is also essential. A higher SNR means the signal strength is significantly greater than the noise level, allowing for clearer detection of the sample's absorption of infrared light, thus improving detection sensitivity and reliability.

[0062] The PLC (Programmable Logic Controller) possesses powerful logic control capabilities, enabling real-time acquisition of status information from field equipment, such as sensor signals and equipment operating status. It then controls the equipment according to preset programs, including starting, stopping, and adjusting parameters. The industrial computer 601 boasts robust data processing and storage capabilities, allowing for further analysis and processing of the data acquired by the PLC. This enables the generation of various reports and charts, facilitating comprehensive monitoring and management of the quality control process. Furthermore, the industrial computer 601 provides a human-machine interface for convenient system operation and configuration. The status indicator 602 uses tri-color LEDs; different colors represent different equipment states, such as green for normal operation, yellow for warning, and red for fault. Operators can quickly understand the equipment's operating status by observing the status indicator 602. The alarm device 603 supports simultaneous sound and light signals. When equipment malfunctions or detection results exceed preset ranges, the alarm device 603 simultaneously emits sound and light signals to alert operators for timely intervention. With a response time of ≤2 seconds, it can quickly respond to abnormal situations and minimize losses.

[0063] The Industrial Ethernet protocol is based on Ethernet technology and optimized and improved for the characteristics of industrial environments, featuring high reliability, real-time performance, and anti-interference capabilities. It adopts standard Ethernet physical layer and data link layer protocols, while adding features suitable for industrial control, such as real-time communication and device redundancy, to the upper-layer protocols. Through network communication units, the online monitoring system can transmit and communicate with field devices and host computers. With a transmission rate ≥100Mbps, it can quickly and accurately transmit large amounts of monitoring data, meeting the needs of real-time monitoring. Remote control is supported, allowing operators to operate and configure the online monitoring system remotely via host computers or mobile terminals, such as adjusting monitoring parameters, viewing monitoring data, and controlling equipment operation, improving the convenience and flexibility of management.

[0064] like Figure 2 As shown, a quality control method for injectable multivitamins includes the following steps:

[0065] Sample collection and pretreatment steps

[0066] Sample Collection: After the sample collection mechanism is activated, the liquid delivery tube 101, acting as a liquid transfer channel, utilizes its suitable inner diameter and material properties (such as medical-grade silicone material with an anti-adsorption coating on the inner wall to prevent sample component adsorption) to introduce the multivitamin injection solution from the storage container into the sample tube. The electromagnetic metering valve 102 precisely controls the valve opening and, based on the set volume parameters, accurately controls the volume of the collected injection solution, ensuring that the sample volume collected each time is accurate and consistent.

[0067] Sample transfer: The test tube transfer assembly 2 utilizes the multiple degrees of freedom of the six-axis robotic arm, combined with a vision positioning system (positioning accuracy ≤0.05mm), to accurately identify the position of the sample tube, fix the sample tube with an appropriate gripping force (adjustable range 10-500g), and then move it to the sample pretreatment mechanism to achieve precise sample transfer.

[0068] Sample stirring: In the sample pretreatment mechanism, the stirring component 201 thoroughly stirs the injection solution by rotation or vibration, so that the components in the injection solution are evenly distributed, avoiding the impact of component precipitation or aggregation on the accuracy of subsequent test results.

[0069] Sample dilution: The high-precision volumetric metering device of the automatic dilution component 202 determines the accurate volume of the required diluent, and the flow control valve precisely controls the flow rate of the diluent, adding the diluent to the injection solution according to the set ratio so that the sample reaches the concentration range suitable for detection.

[0070] High Performance Liquid Chromatography Detection Procedure

[0071] Column selection: Choose a suitable chromatographic column based on the differences in the chemical properties of the vitamins to be detected. Water-soluble vitamins have different polarities. In reversed-phase chromatographic columns, the stationary phase is nonpolar and the mobile phase is polar. Water-soluble vitamins are separated in the column based on the different partition coefficients between the stationary and mobile phases according to their polarity. Fat-soluble vitamins are separated in normal-phase chromatographic columns (polar stationary phase, nonpolar mobile phase) or special functional columns based on the differences in their interaction with the stationary phase.

[0072] Mobile phase delivery: The high-pressure pump (pressure range 0-40MPa) of the mobile phase delivery system 301 provides power to the mobile phase, enabling it to pass through the chromatographic column at a stable flow rate and pressure. After the mobile phase carries the sample into the chromatographic column, different components of the sample continuously undergo partitioning and adsorption-desorption processes between the stationary and mobile phases. Due to the different interactions between each component and the stationary phase, separation is achieved in the chromatographic column.

[0073] Detection wavelength adjustment: The detection wavelength adjustment device 302 employs grating spectral dispersion technology. The composite light emitted by the light source illuminates the grating, which disperses the light according to its wavelength. By rotating the grating or changing its relative position with the detector, light of a specific wavelength is selected to enter the detector. Different vitamin components have specific absorption peaks at different wavelengths. Adjusting the detection wavelength to a suitable range allows the detector to detect at the absorption peak wavelength of the corresponding vitamin, accurately measuring the content of each vitamin component in the sample.

[0074] Sample injection and detection: The automated sampler 303 (robotic arm injection structure) utilizes the precise movement of the robotic arm to accurately inject the pretreated sample into the column inlet. After separation in the column, the sample sequentially enters the detector, which converts the optical signal into an electrical signal. The data processing system (built on hardware circuitry and embedded chips) amplifies, filters, fits, and analyzes the detection signal to obtain relevant data such as the retention time and peak area of ​​vitamin components, thereby determining the content of each vitamin in the sample.

[0075] Atomic absorption spectrometry detection steps

[0076] Characteristic spectral line emission: After starting the atomic absorption spectrometry detection mechanism, the hollow cathode lamp 4 adopts a pulse power supply mode (lamp current adjustable from 1 to 10 mA, stability ≤5%). Under the action of the pulse current, the gas inside the lamp is rapidly ionized, generating high-intensity characteristic spectral lines. Pulse power supply can reduce electrode sputtering and thermal effects, extend the lamp's service life, and ensure the stability and intensity of the spectral lines.

[0077] Atomic vapor absorption: The pretreated sample is introduced into the atomic absorption spectroscopy detection region, and the elements in the sample are atomized to form atomic vapor through heating or other methods. The ground-state atoms in the atomic vapor absorb the characteristic spectral lines emitted by the hollow cathode lamp 4, and the degree of absorption is related to the atomic concentration of that element in the sample.

[0078] Signal detection and analysis: The detector detects the intensity of the spectral lines after absorption. The data processing system processes and analyzes the detection data according to the Lambert-Beer law. By comparing the changes in spectral line intensity before and after absorption, the content information of relevant elements in the sample is calculated.

[0079] Infrared spectroscopy detection steps

[0080] Interference Modulation: After starting the infrared spectroscopy detection mechanism, the pretreated sample is placed in the detection area. The beam splitter of the Michelson interferometer 5 splits the infrared light emitted by the sample into two beams. One beam is directed towards the fixed mirror and returns to the beam splitter after reflection; the other beam is directed towards the moving mirror. The movement of the moving mirror causes an optical path difference between the two beams, resulting in interference. The interference light signal contains information about the sample's absorption of infrared light.

[0081] Signal reception: A mercury cadmium telluride cooled detector (≥32 scans, resolution ≤4cm⁻¹, signal-to-noise ratio ≥5000:1) receives the interferometric infrared light signal. The cooling device lowers the detector temperature, reduces thermal noise, improves the detector's signal-to-noise ratio and sensitivity, and converts the infrared light signal into an electrical signal.

[0082] Data Processing and Analysis: The data processing system performs mathematical processing, such as Fourier transform, on the signals received by the detector, converting the interference signals into infrared spectra. By analyzing information such as the position and intensity of absorption peaks in the infrared spectra, the types and structures of functional groups in the sample can be determined.

[0083] Quality control process management and online monitoring steps

[0084] Status Display and Alarm: After the quality control process management system is running, the equipment operating status is displayed in real time via status indicator lights 602 (three-color LEDs). Different colors represent different statuses (e.g., green indicates normal operation, yellow indicates warning, and red indicates fault). When an abnormal situation occurs in the equipment, the alarm device 603 (supports simultaneous sound and light, with a response time of ≤2s) emits sound and light signals to remind operators to handle the situation promptly.

[0085] Data Reception and Analysis: The data processing unit of the online quality monitoring system receives real-time detection data from high-performance liquid chromatography (HPLC), atomic absorption spectrometry (AAS), and infrared spectroscopy (IR) testing institutions. The data processing unit performs comprehensive analysis and processing on the received data, such as determining whether each detection data point is within the normal range and whether there is a correlation between different test results.

[0086] Data transmission and remote control: The system transmits test results to a remote control terminal via a network communication unit (using industrial Ethernet protocol, transmission rate ≥100Mbps), while also supporting remote control of equipment operation and parameter adjustment. Operators can operate and configure the testing equipment remotely from a distance, improving management efficiency.

[0087] Result Determination and Recording Steps

[0088] Result Determination: Based on the preset quality standards, the various data obtained from the testing steps (such as vitamin content data detected by high-performance liquid chromatography, elemental content data detected by atomic absorption spectrometry, and functional group information detected by infrared spectroscopy) are analyzed and determined. By comparing with the allowable ranges in the quality standards, it is determined whether the quality of the injectable multivitamins is up to standard.

[0089] Data recording: All data (including raw data and processed data), judgment results, and other information from the testing process are recorded in detail to facilitate subsequent quality traceability and data analysis.

[0090] The above are merely specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions, or modifications made based on the present invention to solve essentially the same technical problems and achieve essentially the same technical effects are all covered within the protection scope of the present invention.

Claims

1. A quality control device for injectable multivitamins, characterized in that, include: The sample collection mechanism includes a liquid guide tube (101) for guiding the finished multivitamin injection solution, the liquid guide tube (101) being provided with an electromagnetic metering valve (102), and a test tube transfer assembly (2) for fixing and moving the sample tube. The sample pretreatment mechanism includes a stirring assembly (201) and an automatic dilution assembly (202), wherein the automatic dilution assembly (202) is equipped with a high-precision volume metering device and a flow control valve; A high-performance liquid chromatography (HPLC) detection system includes multiple chromatographic columns, a mobile phase delivery system (301), a detection wavelength adjustment device (302), an automated sampler (303), and a data processing system, wherein the mobile phase delivery system (301) includes a high-pressure pump; Atomic absorption spectrometry detection apparatus, including hollow cathode lamp (4); The infrared spectroscopy detection mechanism includes an interferometer (5) and a detector; The quality control process management system is built on a programmable logic controller and an industrial computer (601), and is equipped with status indicator lights (602) and alarm devices (603). The online quality monitoring system includes a data processing unit, which is signal-connected to the high-performance liquid chromatography detection mechanism, the atomic absorption spectrometry detection mechanism, and the infrared spectroscopy detection mechanism. The data processing unit is also signal-connected to a network communication unit.

2. The quality control device for injectable multivitamins according to claim 1, characterized in that, The stirring assembly (201) uses a magnetic stir bar made of Teflon material in conjunction with an external magnetic drive device; the flow control valve is an electromagnetic proportional valve; the external magnetic drive device of the stirring assembly (201) uses a brushless motor; and the flow control valve of the automatic dilution assembly (202) is a piezoelectric driven electromagnetic proportional valve.

3. The quality control device for injectable multivitamins according to claim 2, characterized in that, The brushless motor speed is adjustable from 0 to 2000 rpm, and the radius of the stir bar rotation trajectory is adjustable from 5 to 30 mm. A reversed-phase chromatography column is used for the detection of water-soluble vitamins, with C18 bonded silica gel as the packing material and a particle size of 5 μm. A normal-phase chromatography column or a special-function chromatography column is used for the detection of fat-soluble vitamins, with silica gel as the packing material and a particle size of 3 to 10 μm.

4. The quality control device for injectable multivitamins according to claim 1, characterized in that, The high-pressure pump has a pressure range of 0-40MPa; the detection wavelength adjustment device (302) adopts grating spectral technology; the automated sampler (303) adopts a robotic arm sample introduction structure; and the data processing system is built based on hardware circuits and embedded chips.

5. The quality control device for injectable multivitamins according to claim 1, characterized in that, The sample collection mechanism's liquid guide tube (101) is made of medical-grade silicone material, and its inner wall is treated with an anti-adsorption coating; the electromagnetic metering valve (102) has a flow control accuracy of ±0.1μL and a response time of ≤50ms; the test tube transfer assembly (2) uses a six-axis robotic arm and a vision positioning system.

6. The quality control device for injectable multivitamins according to claim 1, characterized in that, The hollow cathode lamp (4) is powered by a pulse; the infrared spectroscopy detection mechanism uses a Michelson interferometer (5) and a mercury cadmium telluride cooled detector.

7. The quality control device for injectable multivitamins according to claim 1, characterized in that, The quality control process management system adopts a PLC and industrial computer (601) architecture, and the status indicator (602) is a tri-color LED.

8. A quality control method for injectable multivitamins, utilizing the quality control equipment for injectable multivitamins as described in any one of claims 1-7, characterized in that, Includes the following steps: Sample collection and pretreatment steps: Start the sample collection mechanism and introduce the multivitamin injection solution into the sample tube through the liquid guide tube (101). Use the electromagnetic metering valve (102) to precisely control the volume of the collected injection solution. Use the test tube transfer assembly (2) to fix and move the sample tube and transfer the sample tube containing the injection solution to the sample pretreatment mechanism. In the sample pretreatment mechanism, start the stirring assembly (201) to fully stir the injection solution. Start the automatic dilution unit (202), use a high-precision volume metering device to determine the volume of the diluent, and use a flow control valve to precisely control the flow rate of the diluent to add the diluent to the injection solution for dilution. High-performance liquid chromatography (HPLC) detection steps: Select a suitable chromatographic column according to the type of vitamin to be detected. For water-soluble vitamins, a reversed-phase chromatographic column is used, and for fat-soluble vitamins, a normal-phase chromatographic column or a special-function chromatographic column is used. Start the mobile phase delivery system (301) and use a high-pressure pump to deliver the mobile phase to the chromatographic column. Adjust the detection wavelength to a suitable range using the detection wavelength adjustment device (302). Inject the pretreated sample into the chromatographic column using an automated sampler (303). After the sample is separated in the chromatographic column, it enters the detector. The data processing system processes and analyzes the detection signal to obtain relevant data on vitamin components. Atomic absorption spectroscopy detection steps: Start the atomic absorption spectroscopy detection mechanism, and the hollow cathode lamp (4) emits characteristic spectral lines; The pretreated sample is introduced into the atomic absorption spectroscopy detection region, where atomic vapor in the sample absorbs the characteristic spectral lines. The detector detects the intensity of the absorbed spectral lines, and the data processing system processes and analyzes the detection data to obtain the content information of relevant elements in the sample. Infrared spectroscopy detection steps: Start the infrared spectroscopy detection mechanism; place the pretreated sample in the detection area, and the interferometer (5) modulates the infrared light emitted by the sample; The detector receives the interferometric infrared light signal; the data processing system processes the signal received by the detector to obtain the infrared spectrum of the sample and analyze information such as functional groups in the sample. Quality control process management and online monitoring steps: The quality control process management system operates, and the equipment operating status is displayed in real time through the status indicator (602). When an abnormal situation occurs, the alarm device (603) will sound an alarm. The data processing unit of the online quality monitoring system receives the detection data from the high performance liquid chromatography detection mechanism, the atomic absorption spectrometry detection mechanism, and the infrared spectroscopy detection mechanism in real time. The data processing unit performs comprehensive analysis and processing on the received data, and transmits the detection results to the remote control terminal through the network communication unit. At the same time, it supports remote control of equipment operation and parameter adjustment. Results Judgment and Recording Steps: Based on the preset quality standards, analyze and judge the various data obtained from the testing steps to determine whether the quality of the injectable multivitamins is up to standard; record all data and judgment results of the testing process in detail.

9. The quality control method for injectable multivitamins according to claim 8, characterized in that, In the sample collection and pretreatment steps, the sample collection mechanism includes a liquid guide tube (101), a sample tube, an electromagnetic metering valve (102), and a test tube transfer assembly (2). The sample pretreatment mechanism includes a stirring assembly (201), an automatic dilution assembly (202), a high-precision volumetric metering device, and a flow control valve.

10. The quality control method for injectable multivitamins according to claim 8, characterized in that, In the high performance liquid chromatography detection step, the mobile phase delivery system (301) includes a high pressure pump; in the quality control process management and online monitoring step, the online quality monitoring system includes a data processing unit and a network communication unit.

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