Medical oxygen multi-component detection gas chromatography system and method based on planar microcolumn

The medical oxygen multi-component detection gas chromatography system based on planar microcolumns achieves simultaneous separation and detection of oxygen and trace impurities, solving the problems of inaccurate detection results and bulky equipment in existing technologies, meeting pharmacopoeia requirements, and supporting portable detection.

CN120927883APending Publication Date: 2025-11-11BEIHANG UNIV
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Patent Information

Application Number
CN202511256710.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-04
Publication Date
2025-11-11

AI Technical Summary

Technical Problem

Current technology cannot simultaneously determine multiple components of medical oxygen, especially trace impurities, in a single analysis, and the test results are easily affected by human factors, making it difficult to meet pharmacopoeia requirements.

Method used

The medical oxygen multi-component detection gas chromatography system based on planar microcolumns integrates chromatographic separation, detection, and control and data processing modules. It achieves simultaneous separation and detection of impurities such as oxygen, CO, and CO2 through three independent chromatographic lines, and uses a micro detector and planar microcolumn to support battery power and vehicle deployment.

Benefits of technology

It enables rapid and accurate detection of all components of medical oxygen, meets pharmacopoeia sensitivity requirements, and reduces the bulkiness of equipment and dependence on laboratories.

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Abstract

The invention discloses a medical oxygen multi-component detection gas chromatography system and method based on a planar microcolumn, and relates to the technical field of oxygen multi-component detection, the medical oxygen multi-component detection gas chromatography system comprises a chromatographic separation module, a detection module, a control and data processing module and a verification and calibration module; the chromatographic separation module comprises a plurality of independent chromatographic lines and is used for separating multiple groups of components of medical oxygen to obtain multiple groups of separated gases; the detection module comprises a thermal conductivity detector, a thermochemical detector and a signal processor, and is used for detecting the plurality of groups of separation, processing a detection signal and outputting a digital signal; and the control and data processing module is used for calculating the gas concentration according to the digital signal and issuing a control instruction to the chromatographic separation module. Through the synergistic effect of the three independent chromatographic lines, synchronous separation and detection of oxygen purity and impurities such as CO and CO2 are completed, and the requirement of pharmacopeia for rapid screening of medical oxygen is met.
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Description

Technical Field

[0001] This invention relates to the field of oxygen multi-component detection technology, and more specifically to a medical oxygen multi-component detection gas chromatography system and method based on planar microcolumns. Background Technology

[0002] Medical oxygen is a crucial resource for respiratory oxygen supply, making its quality control paramount. Traditional gas detection methods (such as paramagnetic analyzers, infrared analyzers, and chemical absorption methods) require multiple independent devices to detect oxygen and different impurities (such as CO and CO2) separately. This approach cannot simultaneously determine multiple components in a single analysis and cannot identify undeclared impurities (such as methane and nitrogen), posing potential safety risks. Furthermore, chemical absorption methods and qualitative reactions are highly dependent on operator experience and reagent quality, making the accuracy of results susceptible to human error. Additionally, the quantitation limits for low-concentration impurities (such as CO < 0.0005%) often fail to meet pharmacopoeia requirements. Therefore, developing a portable integrated system that enables simultaneous determination of all components (including trace impurities) of medical oxygen in a single injection while meeting pharmacopoeia sensitivity requirements is a pressing issue for those skilled in the art. Summary of the Invention

[0003] In view of this, the present invention provides a gas chromatography system and method for multi-component detection of medical oxygen based on planar microcolumns, which overcomes the above-mentioned defects.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] A medical oxygen multi-component detection gas chromatography system based on planar microcolumns, integrated in a shockproof box, includes: a chromatographic separation module, a detection module, a control and data processing module, and a verification and calibration module;

[0006] The chromatographic separation module includes multiple independent chromatographic lines for separating multiple components of medical oxygen to obtain multiple sets of separated gases;

[0007] The detection module includes a thermal conductivity detector, a thermochemical detector, and a signal processor, used to detect multiple sets of separations and process the detection signals to output digital signals;

[0008] The control and data processing module is used to calculate the gas concentration based on the digital signal and issue control commands to the chromatographic separation module.

[0009] Optionally, the chromatographic separation module employs three independent chromatographic lines, each integrating a micro-dose generator, a temperature control unit, and a carrier gas channel. The configuration of each chromatographic line is as follows:

[0010] First chromatographic line: Compressed air is used as the carrier gas, and the micro-packed column is filled with Carboxen 1000 molecular sieves;

[0011] Second chromatographic line: Helium is used as the carrier gas, and a micro-packed column is filled with PorapakN adsorbent;

[0012] The third chromatographic line: using helium as the carrier gas, a micro-packed column filled with NaX molecular sieve.

[0013] Optionally, the step of the detection module generating the digital signal is as follows:

[0014] The detected signal is differentially amplified, filtered, power frequency suppressed, and gain processed to generate the digital signal.

[0015] Optionally, the control and data processing module employs an embedded controller to perform temperature PID control, carrier gas flow rate closed-loop regulation, data processing, and instruction generation.

[0016] Optionally, the shockproof box also includes a built-in miniature carrier gas cylinder and a lithium battery power supply module.

[0017] A gas chromatography method for multi-component detection of medical oxygen based on planar microcolumns, comprising the following steps:

[0018] Multiple independent chromatographic lines are used to separate the multiple components of medical oxygen to obtain multiple sets of separated gases;

[0019] The separation of multiple groups is grouped for detection, and the detection signals are processed and output as digital signals;

[0020] The gas concentration is calculated based on the digital signal, and control commands are issued to the chromatographic separation module.

[0021] Optionally, the method for acquiring the digital signal is as follows: the detected signal is sequentially subjected to differential amplification, filtering, power frequency suppression, and gain processing.

[0022] Optionally, the formula for calculating gas concentration is:

[0023]

[0024] In the formula, S i S0 and S0 represent the peak areas of the sample and standard, respectively; X0 represents the concentration of the standard gas.

[0025] As can be seen from the above technical solution, compared with the prior art, the present invention discloses a gas chromatography system and method for multi-component detection of medical oxygen based on planar microcolumns. Through the synergistic effect of three independent chromatographic lines, the simultaneous separation and detection of oxygen purity and impurities such as CO and CO2 can be achieved, meeting the pharmacopoeia's requirements for rapid screening of medical oxygen. At the same time, the use of a micro detector and a planar microchromatographic column supports battery power and vehicle-mounted deployment, reducing the bulkiness and reliance on laboratories of traditional equipment. Attached Figure Description

[0026] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0027] Figure 1 This is a schematic diagram of the system structure provided by the present invention;

[0028] Figure 2 (a) A comparison diagram of the separation of oxygen, carbon monoxide, and methane; (b) A comparison diagram of the separation of oxygen and carbon dioxide; (c) A comparison diagram of the separation of oxygen and nitrogen. Detailed Implementation

[0029] 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.

[0030] This invention discloses a medical oxygen multi-component detection gas chromatography system based on planar microcolumns, integrated within a shockproof enclosure, such as... Figure 1 As shown, it includes: a chromatographic separation module, a detection module, a control and data processing module, and a verification and calibration module;

[0031] The chromatographic separation module includes multiple independent chromatographic lines for separating multiple components of medical oxygen to obtain multiple sets of separated gases;

[0032] The detection module includes a thermal conductivity detector, a thermochemical detector, and a signal processor, which are used to detect multiple sets of separations and process the detection signals to output digital signals.

[0033] The control and data processing module is used to calculate the gas concentration based on the digital signal and issue control commands to the chromatographic separation module.

[0034] In one embodiment, the chromatographic separation module employs three independent chromatographic lines, each integrating a micro-dose dispenser, a temperature control unit, and a carrier gas channel. The configuration of each chromatographic line is as follows:

[0035] First chromatographic line: Compressed air is used as the carrier gas, and the micro-packed column is filled with Carboxen 1000 molecular sieves;

[0036] Second chromatographic line: Helium is used as the carrier gas, and a micro-packed column is filled with PorapakN adsorbent;

[0037] The third chromatographic line: using helium as the carrier gas, a micro-packed column filled with NaX molecular sieve.

[0038] Furthermore, the chromatographic separation module consists of three independent chromatographic lines, responsible for separating O2, N2, CO, CO2, and CH4. Each line consists of a planar microchromatographic column, a microdosage unit, a temperature control module, and a carrier gas channel. The chromatographic column configurations are as follows: The first chromatographic line uses a 2-meter long, 1-m inner diameter micro-packed column filled with Carboxen 1000 molecular sieve (60 / 80 mesh) and compressed air as carrier gas (flow rate 10±2 mL / min) for CO and CH4 separation, operating at 70-80℃; the second chromatographic line uses a 2-meter long, 1-m inner diameter micro-packed column filled with PorapakN adsorbent (80 / 100 mesh) and helium as carrier gas (Grade A, flow rate 10±2 mL / min) for CO2 separation, operating at 70℃; the third chromatographic line uses a 2-meter long, 1-m inner diameter micro-packed column filled with NaX molecular sieve (80 / 100 mesh) and helium as carrier gas (Grade A, flow rate 10±2 mL / min) for O2 and N2 separation, operating at 40-60℃. The separation results are as follows. Figure 2 As shown.

[0039] In one embodiment, the step of the detection module generating a digital signal is as follows:

[0040] The detection signal is differentially amplified, filtered, power frequency suppressed, and gain processed to generate a digital signal.

[0041] Furthermore, the detection module consists of a thermal conductivity detector (TCD), a thermochemical detector (DTC), and a signal processor. The thermal conductivity detector (TCD) is used to detect O2, N2, and CO2, with a sensitivity of 0.0001% and a baseline noise ≤0.06mV. The thermochemical detector (DTC) is used for the detection of trace CO and CH4, with detection limits of 0.0001% and 0.0005%, respectively. The detector output from the signal processor is differentially amplified (AD620 operational amplifier), RC filtered (5kHz bandwidth), subjected to a double-T notch filter (50Hz power frequency suppression), and then amplified twice (3x gain) to finally output a digital signal.

[0042] In one embodiment, the control and data processing module employs an embedded controller to perform temperature PID control, carrier gas flow rate closed-loop regulation, data processing, and instruction generation.

[0043] Furthermore, the control and data processing module employs an embedded controller based on an ARM Cortex-M7 processor to achieve temperature PID control (accuracy ±0.5℃), carrier gas flow rate closed-loop regulation (error ≤2%), and data acquisition. Peak area normalization is used for data analysis; the calculation formula is as follows:

[0044]

[0045] In the formula, X0 is the standard gas concentration, and S i S0 and S0 represent the peak areas of the sample and standard, respectively.

[0046] In one embodiment, a verification and calibration module is also included, which has automatic calibration and verification parameter functions, four built-in standard gases (concentration coverage 0.00025%-0.7%), and supports one-click three-point automatic calibration (linear correlation coefficient R). 2 ≥0.999), and can verify whether the specificity (resolution ≥1.5), precision (RSD: O2<0.01%, N2<2%, CO<4%), limit of detection (DL) and limit of quantitation (QL) meet the pharmacopoeia requirements.

[0047] In one embodiment, the shockproof box also contains a miniature carrier gas cylinder and a lithium battery power supply module.

[0048] Furthermore, the portable design adopts a miniaturized structure, with all components integrated into a shockproof box (size ≤40×30×20cm), and includes a built-in 0.7-1L miniature carrier gas bottle (helium / compressed air) and a lithium battery power supply module (battery life ≥8 hours); a single analysis requires only 250μL of sample, and the carrier gas consumption is ≤20mL / min, supporting rapid on-site detection.

[0049] This embodiment also discloses a gas chromatography method for the multi-component detection of medical oxygen based on planar microcolumns, the specific steps of which are as follows:

[0050] Multiple independent chromatographic lines are used to separate the multiple components of medical oxygen to obtain multiple sets of separated gases;

[0051] Multiple groups of separations are grouped for detection, and the detection signals are processed and output as digital signals;

[0052] The gas concentration is calculated based on the digital signal, and control commands are sent to the chromatographic separation module.

[0053] In one embodiment, the method for acquiring the digital signal is as follows: the detection signal is sequentially subjected to differential amplification, filtering, power frequency suppression, and gain processing.

[0054] In one embodiment, the gas concentration calculation formula is as follows:

[0055]

[0056] In the formula, S i S0 and S0 represent the peak areas of the sample and standard, respectively; X0 represents the concentration of the standard gas.

[0057] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on its differences from other embodiments. Similar or identical parts between embodiments can be referred to interchangeably. For the apparatus disclosed in the embodiments, since they correspond to the methods disclosed in the embodiments, the description is relatively simple; relevant parts can be referred to the method section.

[0058] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A medical oxygen multi-component detection gas chromatography system based on planar microcolumns, integrated within a shockproof enclosure, characterized in that, include: The system includes a chromatographic separation module, a detection module, a control and data processing module, and a validation and calibration module. The chromatographic separation module includes multiple independent chromatographic lines for separating multiple components of medical oxygen to obtain multiple sets of separated gases; The detection module includes a thermal conductivity detector, a thermochemical detector, and a signal processor, used to detect multiple sets of separations and process the detection signals to output digital signals; The control and data processing module is used to calculate the gas concentration based on the digital signal and issue control commands to the chromatographic separation module.

2. The medical oxygen multi-component detection gas chromatography system based on planar microcolumns according to claim 1, characterized in that, The chromatographic separation module employs three independent chromatographic lines, each integrating a micro-dose generator, a temperature control unit, and a carrier gas channel. The configuration of each chromatographic line is as follows: First chromatographic line: Compressed air is used as the carrier gas, and the micro-packed column is filled with Carboxen 1000 molecular sieves; Second chromatographic line: Helium is used as the carrier gas, and a micro-packed column is filled with PorapakN adsorbent; The third chromatographic line: using helium as the carrier gas, a micro-packed column filled with NaX molecular sieve.

3. The medical oxygen multi-component detection gas chromatography system based on planar microcolumns according to claim 1, characterized in that, The steps by which the detection module generates the digital signal are as follows: The detected signal is differentially amplified, filtered, power frequency suppressed, and gain processed to generate the digital signal.

4. The medical oxygen multi-component detection gas chromatography system based on planar microcolumns according to claim 1, characterized in that, The control and data processing module uses an embedded controller to perform temperature PID control, carrier gas flow rate closed-loop regulation, data processing, and command generation.

5. The medical oxygen multi-component detection gas chromatography system based on planar microcolumns according to claim 1, characterized in that, The shockproof box also contains a miniature carrier gas cylinder and a lithium battery power supply module.

6. A gas chromatographic method for multi-component detection of medical oxygen based on planar microcolumns, characterized in that, The specific steps are as follows: Multiple independent chromatographic lines are used to separate the multiple components of medical oxygen to obtain multiple sets of separated gases; The separation of multiple groups is grouped for detection, and the detection signals are processed and output as digital signals; The gas concentration is calculated based on the digital signal, and control commands are issued to the chromatographic separation module.

7. The gas chromatography method for multi-component detection of medical oxygen based on planar microcolumns according to claim 6, characterized in that, The method for acquiring digital signals is as follows: the detected signal is sequentially subjected to differential amplification, filtering, power frequency suppression, and gain processing.

8. The gas chromatography method for multi-component detection of medical oxygen based on planar microcolumns according to claim 6, characterized in that, The formula for calculating gas concentration is: In the formula, S i S0 and S0 represent the peak areas of the sample and standard, respectively; X0 represents the concentration of the standard gas.