CN115486834A - Wearable exhaled breath acetone detection method and device based on MXene - Google Patents
Wearable exhaled breath acetone detection method and device based on MXene Download PDFInfo
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- CN115486834A CN115486834A CN202211227767.9A CN202211227767A CN115486834A CN 115486834 A CN115486834 A CN 115486834A CN 202211227767 A CN202211227767 A CN 202211227767A CN 115486834 A CN115486834 A CN 115486834A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/08—Detecting, measuring or recording devices for evaluating the respiratory organs
- A61B5/082—Evaluation by breath analysis, e.g. determination of the chemical composition of exhaled breath
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- A—HUMAN NECESSITIES
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- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
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- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
- A61B5/6802—Sensor mounted on worn items
- A61B5/6803—Head-worn items, e.g. helmets, masks, headphones or goggles
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention discloses a wearable exhaled breath acetone detection method and device based on MXene. The device includes an exhaled breath acetone detection label. The exhaled breath acetone detection label is formed by assembling an MXene acetone sensor, a flexible detection circuit board, a polydimethylsiloxane packaging layer and a light-emitting diode circuit board and is used for detecting the concentration of acetone in exhaled breath. The invention utilizes the wireless Bluetooth between the MXene device and the mobile terminal to carry out data interaction, realizes continuous and real-time monitoring of the dynamic change of the acetone concentration of the exhaled breath, reflects the intensity of lipid metabolism activities such as diet and fat burning movement and the like, and further realizes daily metabolic health management. The method provides a wearable detection platform for exhaled breath analysis, and has the advantages of non-invasiveness, continuity, real-time performance, simplicity in operation, rapidness in detection and the like.
Description
Technical Field
The invention relates to a detection technology of exhaled breath acetone, in particular to a wearable exhaled breath acetone detection method and device based on MXene.
Background
Exhaled breath acetone is an important product of lipid metabolism and is considered to be one of the most attractive targets for lipid metabolism monitoring. Clinical evidence suggests that acetone is produced by fatty acids undergoing a series of oxidative events in liver mitochondria and is excreted primarily by exhaled breath. Therefore, the exhaled breath acetone has a clear metabolic source and pathway, and can reflect the lipid metabolism related to daily activities such as dietary habits and physical exercise. Studies have shown that the exhaled breath acetone concentration in healthy subjects ranges from hundreds of ppb (parts per billion) to 0.9ppm (parts per million), which can rise significantly to tens or hundreds of ppm after fasting, ketogenic diet, or aerobic exercise. Therefore, the detection of the exhaled breath acetone has great potential in the fields of guiding weight loss, evaluating exercise endurance, or guiding ketoacidosis treatment and the like, and is expected to be applied to clinical practice. In addition, compared with biochemical analysis for blood ketone detection, exhaled breath analysis has the outstanding advantages of simple and noninvasive sampling, and the burden on the detected object is smaller, so that the method has great prospects in the aspects of medical diagnosis and personalized health care.
At present, standard exhaled breath detection usually relies on a desktop analytical instrument, such as gas chromatography-mass spectrometry, selective ion flow tube mass spectrometry and the like, and the method is suitable for laboratory or hospital examination and is difficult to be widely applied to daily individual metabolic health monitoring. Therefore, the development of portable, wearable and miniaturized exhaled breath sensing detection schemes can serve as an important complement to clinical standard exhaled breath detection. In recent years, an emerging two-dimensional transition metal carbide and nitride nanometer material family (MXenes) receives great attention in sensor development, mainly due to a series of excellent characteristics of metal conductivity, high chemical activity surface, high signal-to-noise ratio and the like. MXenes is therefore uniquely attractive for designing high sensitivity, low detection limit room temperature gas sensors. In addition, recent studies indicate that the mask worn daily can not only provide protection for individuals, but also be combined with sensing materials to achieve wearable detection of viral and biochemical markers in exhaled breath. Therefore, aiming at detection application bottlenecks such as high humidity and multiple interferents in exhaled breath detection, sensor response drift and the like, a set of exhaled breath acetone detection MXene intelligent mask device and method integrating interferent filtering, sensor detection, response correction and wireless data transmission is developed based on an MXene nano material platform and a disposable mask, and the device and method have important significance for promoting wearable breath analysis and daily lipid metabolism management.
Disclosure of Invention
The invention aims to provide a wearable exhaled breath acetone detection method and a wearable exhaled breath acetone detection device based on MXene aiming at the defects of the prior art and products, so as to realize continuous real-time wearable detection of exhaled breath acetone in daily life and reflect diet and exercise health management related to lipid metabolism.
The purpose of the invention is realized by the following technical scheme:
a wearable exhaled breath acetone detection device based on MXene, it includes: detecting the label with exhaled breath acetone; the exhaled breath acetone detection label comprises an MXene acetone sensor, a flexible detection circuit board, a polydimethylsiloxane packaging layer and an LED circuit board, wherein the MXene acetone sensor, the flexible detection circuit board, the polydimethylsiloxane packaging layer and the LED circuit board are sequentially assembled from bottom to top; the diode circuit board and the MXene acetone sensor are electrically connected with the flexible detection circuit board; the MXene acetone sensor is used for detecting the concentration of acetone in exhaled breath and converting the acetone into an electric signal, and the flexible detection circuit board is used for acquiring and processing the electric signal of the MXene acetone sensor; the MXene acetone sensor comprises a sensor substrate, a gold interdigital electrode and an MXene nano sensing layer which are sequentially assembled from bottom to top, wherein titanium dioxide nano particles and short peptide molecules are modified on the surface of the MXene nano sensing layer.
Further, the MXene nano sensing layer is obtained by mixing 2 parts by mass of ceramic phase titanium aluminum carbon powder with 2 parts by mass of lithium fluoride, dissolving the mixture in 40 parts by volume of concentrated hydrochloric acid, etching the mixture for 24 hours at 40 ℃, cleaning the precipitate by deionized water, and spraying the precipitate on the surface of the gold interdigital electrode after ultrasonic mechanical stripping assisted by a vortex generator.
Further, the titanium dioxide nanoparticles are modified by the following method: mixing the MXene nano sensing layer with 3% of hydrogen peroxide solution by mass fraction, and heating in a water bath at 80 ℃ to obtain the MXene nano sensing layer with the titanium dioxide nano particles growing on the MXene nano sensing layer in situ.
Further, the short peptide molecule is modified by the following method: mixing and dissolving the MXene nano sensing layer with titanium dioxide nano particles grown in situ according to the mass ratio of 1.
Further, an MXene-based fabric filter for filtering exhaled breath is also included; the MXene-based fabric filter is composed of a platinum nanoparticle-loaded MXene fabric and an active drying agent wrapped in the platinum nanoparticle-loaded MXene fabric, wherein the platinum nanoparticle-loaded MXene fabric is obtained by electrostatically adsorbing MXene on the surface of a cotton fabric and reducing and loading platinum nanoparticles on the surface of MXene in situ in a chloroplatinic acid solution.
Further, the platinum nanoparticle-loaded MXene fabric is prepared by the following method: the white cotton fabric which is washed by deionized water and dried is soaked in 5mg/mL MXene solution, deposition is carried out for 30 minutes, the white cotton fabric is repeatedly washed and dried and then soaked in 3.86mM chloroplatinic acid solution, reaction is carried out for 30 minutes, and the in-situ reduction of the platinum nanoparticles is realized by utilizing the chemical active surface of MXene.
Furthermore, the flexible detection circuit board consists of a detection circuit substrate, a detection circuit, a diode circuit connection pad and a sensor connection pad, wherein the detection circuit substrate consists of a polyimide film, and the detection circuit mainly comprises a miniature low-power chip and a peripheral resistor capacitor and is used for acquiring and processing an electric signal of the MXene acetone sensor; and respectively welding the LED circuit board and the MXene acetone sensor on the diode circuit connecting pad and the sensor connecting pad through low-temperature soldering tin, and realizing the electrical connection of the diode circuit board, the MXene acetone sensor and the flexible detection circuit board.
Furthermore, the detection circuit is composed of a microcontroller, a constant current source, an analog-to-digital converter, bluetooth, a low-pass network, a field effect transistor, a light emitting diode, a battery and power management circuit and a peripheral resistor capacitor.
Further, still include disposable gauze mask, fix breather valve and the breather valve shell on disposable gauze mask, the expiratory gas acetone detects the label and fixes between the breather valve and the breather valve shell of disposable gauze mask outside, and MXene based fabric filter is fixed on the breather valve of disposable gauze mask inboard for filter the expiratory gas through the breather valve.
Based on the same principle, the invention also provides a detection method of the exhaled breath acetone based on MXene, which comprises the following steps:
the device is used for acquiring the acetone concentration of the exhaled air, and the light-emitting diode is kept turned on during the acetone detection.
In the detection method, the exhaled air is filtered by the fabric filter based on MXene, and is directly detected by the MXene acetone sensor through windowing of the detection circuit board and windowing of the packaging layer without other pretreatment.
The embodiment of the invention has the following beneficial effects: the invention provides a wearable exhaled breath acetone detection method and device based on MXene, which can realize continuous and real-time wearable exhaled breath analysis. The MXene acetone sensor designed based on the MXene nano material has excellent sensitivity and low detection limit, and the selectivity and the anti-interference capability of exhaled breath acetone detection are improved in a mode of combining the MXene acetone sensor with the MXene-based fabric filter. Exhaled breath acetone detection label based on flexible electronic technology constructs combines with disposable gauze mask, provides wearing formula testing platform for the exhaled breath analysis that need not the preliminary treatment. The Bluetooth in the MXene intelligent mask is used for wireless communication, so that continuous real-time display of a breathing curve on a mobile terminal and monitoring and analysis of physiological and biochemical parameters such as the concentration of acetone and the breathing frequency of exhaled breath can be further realized.
Compared with table type exhaled gas analysis instruments such as a meteorological chromatography-mass spectrum instrument, a selective ion flow tube mass spectrum instrument and the like, the MXene intelligent mask does not need manual operation, is flexible and convenient to use and is not restricted by users and scenes. Compared with the similar portable exhaled breath analysis technology, the method realizes the wearable exhaled breath acetone detection, is more convenient to use, and can realize continuous and real-time exhaled breath acetone analysis. The wearing body feeling of the MXene intelligent mask is similar to that of a common disposable mask, and the concentration change of exhaled breath acetone generated by lipid metabolism activities such as diet and exercise in daily life can be further reflected while daily health protection is realized. According to the advantages, the device and the method can be widely applied to daily metabolic health management.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic diagram of an outer side of an MXene intelligent mask package provided in an embodiment of the present invention;
fig. 2 is a schematic view of the inside of an MXene smart mask according to an embodiment of the present invention;
fig. 3 is a hierarchical structure diagram of an exhaled breath acetone detection tag according to an embodiment of the present invention;
figure 4 is an assembly drawing of an exhaled breath acetone detection tag provided by an embodiment of the present invention;
fig. 5 is a modified diagram of an MXene acetone sensor provided in an embodiment of the present invention;
fig. 6 is a diagram of an MXene-based fabric filter architecture provided by an embodiment of the present invention;
fig. 7 is a diagram of MXene-based fabric filter modification provided by an embodiment of the present invention;
FIG. 8 is a functional block diagram of a detection circuit provided in accordance with an embodiment of the present invention;
fig. 9 is an acetone detection response diagram of the acetone detection device provided by the embodiment of the present invention;
FIG. 10 is a linear fit of acetone detection by the acetone detection device provided in the embodiments of the present invention;
fig. 11 is a acetone detection repetitive response diagram of the acetone detection device provided by the embodiment of the present invention;
fig. 12 is an acetone detection stability response diagram of the acetone detection apparatus provided in the embodiment of the present invention;
FIG. 13 is a graph of humidity filtration performance of an acetone detection device provided by an embodiment of the present invention;
FIG. 14 is a graph of ethanol filtration performance of an acetone detection device provided by an embodiment of the present invention;
FIG. 15 is a graph illustrating ammonia gas filtration performance of an acetone detection apparatus according to an embodiment of the present invention;
FIG. 16 is a diagram illustrating acetone filtration performance of an acetone detection device according to an embodiment of the present invention;
FIG. 17 is a diagram illustrating acetone detection selectivity of the acetone detection device according to the embodiment of the present invention;
fig. 18 is a schematic diagram of an embodiment of an MXene smart mask according to an embodiment of the present invention;
fig. 19 is a graph showing the correlation between the detection result of acetone in exhaled breath and the detection result of blood ketones performed by the MXene smart mask of the present invention;
in the figure: the disposable mask comprises a disposable mask 1, a breather valve 2, a breather valve shell 3, an expiratory gas acetone detection label 4, an MXene-based fabric filter 5, an MXene acetone sensor 41, a flexible detection circuit board 42, a detection circuit board windowing 421, a polydimethylsiloxane packaging layer 43, a packaging layer windowing 431, an LED circuit board 44, an LED substrate 441, an LED 442, a detection circuit substrate 422, a detection circuit 423, a diode circuit connection pad 424, a sensor connection pad 425, a sensor substrate 411, a gold interdigital electrode 412, an MXene nano sensing layer 413, titanium dioxide nanoparticles 414, short peptide molecules 415, an active desiccant 51, a platinum nanoparticle loaded MXene fabric 52, an MXene intelligent mask 11, a mobile terminal 12, a real-time breathing curve display functional area 13 and a breathing result analysis functional area 14.
Detailed Description
The embodiments, features and aspects of the present disclosure will be described in detail below with reference to the accompanying drawings, but the present disclosure is not limited thereto. Any embodiment extended based on the embodiment of the present invention belongs to the protection scope of the present invention for all other embodiments obtained by those skilled in the art without any creative work. In the drawings, like reference numbers can indicate identical or functionally similar elements. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
Furthermore, while the present disclosure has been described in terms of several specific details for purposes of illustration, it will be apparent to those of ordinary skill in the art that the present disclosure may be practiced without some of these specific details, and that some methods and instrumentalities, well known to those skilled in the art, and the use of components and parts may not be described in detail in order to avoid obscuring the subject matter of the present disclosure.
The embodiment of the invention provides a wearable exhaled breath acetone detection device based on MXene, which mainly comprises: an exhaled breath acetone detection tag 4, the exhaled breath acetone detection tag 4 being for detecting the acetone concentration in exhaled breath.
Fig. 3 shows a hierarchical structure diagram of the exhaled breath acetone detection label 4. The exhaled breath acetone detection label 4 is formed by assembling a light-emitting diode circuit board 44, a polydimethylsiloxane packaging layer 43, a flexible detection circuit board 42 and an MXene acetone sensor 41 from top to bottom. The polydimethylsiloxane packaging layer 43 is used for top layer packaging of the flexible detection circuit board 42 through a solution thermosetting method, windowing processing is carried out on the polydimethylsiloxane packaging layer 43 and the flexible detection circuit board 42 through laser cutting, and the sizes of the packaging layer windowing 431 and the detection circuit board windowing 421 are consistent with those of the MXene acetone sensor 41. This design facilitates direct contact of the MXene acetone sensor 41 located on the bottom of the exhaled breath acetone detection tag 4 with exhaled breath to enable exhaled breath acetone detection. The polydimethylsiloxane encapsulation layer 43 serves to protect the flexible detection circuit board 42 and also serves as a spacer to fix the working distance between the led circuit board 44 and the MXene acetone sensor 41. By adjusting the thickness of the polydimethylsiloxane encapsulation layer 43, different illumination working distances can be controlled. The illumination working distance is related to the sensor received power density, which is 1.5mm in this embodiment.
Fig. 4 shows an assembly diagram of the exhaled breath acetone detection label 4. The flexible inspection circuit board 42 is composed of an inspection circuit substrate 422, an inspection circuit 423, a diode circuit connection pad 424, and a sensor connection pad 425. The led 442 is fixed on the led substrate 441, further assembled on the pdms encapsulation layer 43, aligned with the MXene acetone sensor 41 through the encapsulation layer opening window 431 and the inspection board opening window 421 to fix the light irradiation working distance, and soldered to the diode circuit connection pad 424 through the low temperature solder, and electrically connected to the flexible inspection board 42. The MXene acetone sensor 41 comprises a sensor substrate 411 and gold interdigital electrodes 412, and is welded with sensor connection pads 425 through low-temperature soldering, so as to realize electrical connection with the exhaled breath acetone detection label 4.
As shown in fig. 5, the MXene acetone sensor 41 is modified with an MXene nano sensing layer 413, a titanium dioxide nano particle 414 and a short peptide molecule 415 on a gold interdigital electrode 412, the short peptide molecule 415 can improve the detection performance, and the short peptide molecule of the present invention can use, for example, phenylalanine-serine-lysine, methionine-cysteine-histidine, tryptophan-alanine-leucine, and the like, but is not limited thereto. The MXene nano sensing layer 413 is prepared by etching ceramic phase titanium-aluminum-carbon with hydrochloric acid/lithium fluoride solution. Specifically, 2 parts by mass of lithium fluoride was dissolved in 40 parts by volume of concentrated hydrochloric acid (mass fraction: 36% to 38%), and stirred at room temperature for 30 minutes to prepare an etching solution. Then 2 parts by mass of ceramic phase titanium aluminum carbon powder was slowly added to the solution, and the reaction was stirred at 40 ℃ for 24 hours. After the reaction was completed, the mixed solution was centrifuged at 3500 rpm, the supernatant was removed and washed with deionized water, mechanically oscillated by a vortex generator, centrifuged again at 3500 rpm, and the supernatant was removed again. The above procedure was repeated until the black precipitate swelled and clearly layered. The black precipitate was collected and dispersed with deionized water and the MXene multilayer film was further peeled off using an ultrasonic method to obtain the MXene nano sensing layer 413. And (3) preparing the MXene nano sensing layer 413 into a proper concentration, mixing the MXene nano sensing layer 413 with 3% of hydrogen peroxide in a mass fraction according to different volume ratios, and heating in a water bath at 80 ℃ for 5 minutes to prepare the MXene nano sensing layer 413 loaded with the titanium dioxide nano particles 414 with different concentrations. The above materials were mixed and dissolved with a short peptide molecule 415 (phenylalanine-serine-lysine) at a mass ratio of 1. Centrifuging the obtained solution at 8000 rpm, washing the sediment with deionized water, dispersing the sediment into proper concentration again to obtain an MXene nano sensing layer co-modified by titanium dioxide nano particles and short peptides, spraying the MXene nano sensing layer on the sensor substrate 411 and the gold interdigital electrode 412 which are cleaned by plasma by using a spray gun, and drying to finally obtain the MXene acetone sensor 41.
The detection system function of the device is shown in fig. 8. The detection circuit 423 is mainly composed of a microcontroller, a constant current source, a low-pass network, an analog-to-digital converter, a Bluetooth, a field effect transistor, a battery, a power management circuit and a peripheral resistor capacitor. The microcontroller realizes the functions of signal modulation, data processing and the like, and particularly provides a reference voltage Vref for the constant current source, acquires a sampling signal of the analog-digital converter through buses such as I2C and the like, performs data transmission with Bluetooth, controls the on-off of the field effect transistor and the like. The constant current source outputs constant test current Imeasure according to the reference voltage Vref, voltage signals are generated after the constant current passes through the MXene acetone sensor 41, power frequency noise interference is removed through low-pass network filtering, and finally the constant current is converted by the analog-to-digital converter to generate sampling signals. The microprocessor generates a control signal to adjust the on-off of the field effect transistor, so as to realize the on-off of the light emitting diode 442 and control the light irradiation time of the MXene acetone sensor 41. The Bluetooth carries out signal transmission with the mobile terminal through wireless communication, and data processing and display are carried out on the mobile terminal. The system is powered by the battery and the power management module to provide a supply voltage Vcc to drive the detection circuit 423. In order to realize a compact and miniaturized circuit design, the detection circuit 423 may employ a micro low power consumption chip, including but not limited to an MSP430FR2632 microprocessor chip, an AD8605 operational amplifier chip, an ADs1115 analog-to-digital conversion chip, and the like.
The device can monitor the exhaled breath acetone with the concentration of 0.5-50ppm in real time and calibrate the exhaled breath acetone before use. In the calibration experiment, standard acetone gas (100 ppm) and standard air are mixed to prepare the acetone gas with different concentrations, and the standard acetone gas is prepared by completely volatilizing anhydrous acetone in the standard air.
Because the MXene acetone sensor 41 has an irreversible acetone adsorption phenomenon, in order to realize acetone sensing detection with good repeatability and quantitative analysis, the MXene acetone sensor 41 is subjected to light irradiation by introducing the light-emitting diode 442. Since the photoelectric response hetero-interface composed of the titanium dioxide nanoparticles 414 and the MXene nano-sensing layer 413 in the MXene acetone sensor 41 can generate photogenerated carriers under the condition of light irradiation, the acetone desorption condition is improved, and therefore the LED 442 is kept turned on during the acetone detection period, and the response of the MXene acetone sensor 41 is corrected.
As shown in fig. 9, the MXene acetone sensor 41 produced a positive normalized resistance response when acetone gas was passed, indicating that the sensor resistance increased with acetone gas passage. The acetone response returned to baseline values when the air was re-aerated, indicating that the acetone response was completely reversible under light irradiation conditions and the response values increased sequentially with increasing acetone concentration. In addition, fig. 9 shows that the MXene acetone sensor 41 has a faster acetone response and recovery speed, which is beneficial to further shortening the exhaled breath analysis time. Three independent replicates of the same batch of MXene acetone sensors 41 were run and the results plotted as scatter plots and fitted using piecewise linear fit. As shown in FIG. 10, the acetone response exhibited linear correlations over the concentration ranges of 0.5-2ppm and 2-50ppm, respectively, with the coefficient of linear correlation R in the range of 0.5-2ppm 2 0.98, sensitivity 0.672%/ppm; linear correlation coefficient R in the range of 2-50ppm 2 It was 0.97, and the sensitivity was 0.145%/ppm. The results of the independent repeat tests were of better consistency, represented by the smaller error bars in fig. 10.
This example tests the repeatability and long-term stability of the detection of the MXene acetone sensor 41. As shown in fig. 11-12, the MXene acetone sensor 41 showed good reversibility in the 5ppm acetone response-recovery for consecutive cycles with the response amplitude remaining well consistent. The stability test for 15 continuous days shows that the MXene acetone sensor 41 has better long-term stability and can be applied to long-term exhaled breath acetone detection under smaller response attenuation.
As a preferred embodiment, the invention provides an MXene-based fabric filter 5 capable of suppressing respiratory disturbance, which is a preferred embodiment, in response to the typical disturbance such as humidity, exhaled ethanol, ammonia, etc. existing in exhaled breath, the MXene-based fabric filter 5 is composed of MXene fabric 52 loaded with platinum nanoparticles and an active desiccant 51, as shown in fig. 6. The active desiccant 51 may be in the form of granules harmless to the human body, including but not limited to activated alumina, allochroic silica gel, etc. The platinum nanoparticle-loaded MXene fabric 52 was prepared by a two-step solution process, as shown in fig. 7. The white cotton fabric, washed with deionized water and dried, was first soaked in 5mg/mL MXene solution and deposited for 30 minutes. The MXene and rich oxygen-containing functional groups on the surface of the cotton fabric form a hydrogen bond network, so that stable electrostatic adsorption of the MXene on the cotton fabric is realized. The unadsorbed MXene was washed with deionized water and dried. The above procedure was repeated until a black MXene fabric was obtained. And soaking the MXene fabric in a chloroplatinic acid solution of 3.86nM for reaction for 30 minutes, and realizing in-situ reduction of the platinum nanoparticles by using the chemical active surface of MXene to prepare the MXene fabric 52 loaded with the platinum nanoparticles. Filling an active desiccant 51 between the platinum nanoparticle-loaded MXene fabrics 52, and packaging and bonding the platinum nanoparticle-loaded MXene fabrics 52 by using polydimethylsiloxane glue with good air permeability to obtain the MXene-based fabric filter 5.
The invention calibrates the interference filtering performance. As shown in fig. 13-16, simulated exhaled breath (5% carbon dioxide, 79% nitrogen, 16% oxygen) was mixed with 10ppm ammonia, ethanol, acetone, and 90% relative humidity, respectively, to give an unfiltered standard gas. The unfiltered interferent response was tested using the MXene acetone sensor 41 with calibration of humidity using a commercial hygrometer and ammonia, ethanol, acetone concentrations using a gas chromatograph, respectively. Meanwhile, the simulated exhaled breath containing the interferents passes through an MXene-based fabric filter 5, the response of the filtered simulated exhaled breath is tested by an MXene acetone sensor 41, the tail gas is collected by an air bag, a commercial hygrometer is performed again to calibrate the humidity, and a gas chromatograph is performed to calibrate the ammonia, ethanol and acetone concentrations. Fig. 13-16 show that the MXene based fabric filter 5 has good filtration effect on ammonia, ethanol, humidity, and a certain filtration effect on acetone, but the MXene acetone sensor 41 still maintains a high acetone response. Thus, the MXene-based fabric filter 5 is able to improve the selectivity of exhaled breath acetone detection.
Further, the device of the invention can realize selective detection of exhaled breath acetone in the presence of interferents. As shown in fig. 17, the experiment configured 90% rh humidity simulated exhaled breath mixed with 10ppm of acetone, ammonia, ethanol, hexane, and isoprene, respectively, showed that the device of the present invention produced the highest response to acetone, had significant suppression of both polar and non-polar exhaled breath interferents, and was able to meet the acetone detection requirements in the exhaled breath complex environment from the selectivity perspective.
In order to realize stable detection, as a preferred embodiment, the device further comprises a disposable mask 1, a breather valve 2 and a breather valve housing 3, forming an MXene intelligent mask 11, wherein the exhaled breath acetone detection label 4 is fixed between the breather valve 2 and the breather valve housing 3 outside the disposable mask 1, and is used for detecting the acetone concentration in exhaled breath. An MXene based fabric filter 5 is fixed on the exhalation valve 2 inside the disposable mask 1 for filtering the exhaled breath passing through the exhalation valve 2, as shown in fig. 1-2.
Fig. 18 is a schematic diagram of an embodiment of an MXene smart mask 11 according to an embodiment of the present invention. The MXene-based fabric filter 5 is assembled on the inner surface of the disposable mask 1 close to the breather valve 2, the exhaled breath acetone detection tag 4 is assembled between the breather valve 2 and the breather valve shell 3 on the outer side of the disposable mask 1, and data communication and subsequent data display processing between the MXene intelligent mask 11 and the mobile terminal 12 are achieved through Bluetooth wireless transmission. The exhaled breath is filtered through the MXene based fabric filter 5, directly detected by the MXene acetone sensor 41 through the detection circuit board fenestration 421 and the encapsulation layer fenestration 431 without further pre-treatment. The mobile terminal 12 draws a continuous real-time respiration curve according to the received data, and displays the exhaled breath rhythm and the exhaled breath acetone concentration change caused by the respiration activity in the real-time respiration curve display functional region 13, and displays the calculated exhaled breath acetone concentration and the breath rate per minute in the respiration result analysis functional region 14.
Further, in this embodiment, 5 volunteers were recruited to perform in vivo breath test verification on the MXene smart mask 11 of the present invention, and blood ketone concentration changes of 5 volunteers were detected as a standard reference for the concentration change of the exhaled breath acetone. The blood ketone test is a clinical common ketone body test method and is also a common reference value for detecting the exhaled breath acetone. In the experimental process, the volunteers wear the MXene intelligent mask 11 for detecting the exhaled breath acetone according to the guidance of the experimenters to carry out exhaled breath acetone test within 5 minutes, and simultaneously collect the fingertip blood and carry out blood ketone level detection. Before blood sampling, an alcohol cotton sheet is used for disinfecting fingertips, a blood sampling pen and a disposable minimally invasive blood sampling needle are used during blood sampling, and standard biochemical test paper is used for detecting the blood ketone level as a reference. One test for exhaled breath acetone and one test for blood ketone level were taken as one standard test. Two volunteers participated in diet tests, and took balanced diet, ketogenic diet, and high-carbohydrate diet respectively in three days, the first day was tested in standard once every five and half night, the second day was tested in standard once every 3 hours from eight and half morning to eight and half night, the third day was tested in standard once every 3 hours from eight and half morning to five and half night, and each person totaled 11 standard tests. Three other volunteers participated in the exercise test, performing two and a half hour cycling exercises on the working day for a total of one hour of exercise, controlling the exercise load of the subject in the experiment, and monitoring the cardiac output as the exercise intensity reference, and then the volunteers needed to rest for a total of two hours in a resting state, and the experiment lasted for a total of three hours. During the test, standard tests were performed at 0, 30, 90, 120, 180 minutes, for a total of 5 standard tests per person.
As shown in fig. 19, the MXene smart mask 11 provided by the embodiment of the present invention is used for exhaled breath acetone detection, and the correlation between the obtained result and the blood ketone level of the volunteers is analyzed. The pearson correlation coefficient of the exhaled breath acetone and the blood ketone obtained by the linear regression was 0.911, which proves that the intelligent mask 11 for MXene can be used for reliable exhaled breath acetone detection.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention, and those skilled in the art will appreciate that various modifications and variations can be made in the present invention. Any modification, equivalent replacement, improvement and the like made without the creative efforts shall be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a wearable exhaled breath acetone detection device based on MXene which characterized in that, it includes: an exhaled breath acetone detection label (4); the exhaled breath acetone detection label (4) comprises an MXene acetone sensor (41), a flexible detection circuit board (42), a polydimethylsiloxane packaging layer (43) for packaging the flexible detection circuit board (42) and a light-emitting diode circuit board (44) which are sequentially assembled from bottom to top, wherein the light-emitting diode circuit board (44) comprises a light-emitting diode substrate (441) and a light-emitting diode (442) fixed on the light-emitting diode substrate (441), and windows are arranged on the flexible detection circuit board (42) and the polydimethylsiloxane packaging layer (43) so that the light-emitting diode (442) is opposite to the MXene acetone sensor (41); the diode circuit board (44) and the MXene acetone sensor (41) are electrically connected with the flexible detection circuit board (42); the MXene acetone sensor (41) is used for detecting the concentration of acetone in the exhaled breath and converting the acetone into an electric signal, and the flexible detection circuit board (42) is used for acquiring and processing the electric signal of the MXene acetone sensor (41); the MXene acetone sensor (41) comprises a sensor substrate (411), a gold interdigital electrode (412) and an MXene nano sensing layer (413) which are sequentially assembled from bottom to top, wherein titanium dioxide nanoparticles (414) and short peptide molecules (415) are modified on the surface of the MXene nano sensing layer (413).
2. The device according to claim 1, wherein the MXene nano sensing layer (413) is prepared by mixing 2 parts by mass of ceramic phase titanium aluminum carbon powder, 2 parts by mass of lithium fluoride and 40 parts by volume of concentrated hydrochloric acid, etching at 40 ℃ for 24 hours, cleaning precipitate by deionized water, and spraying the mixture on the surface of the gold interdigital electrode (412) after ultrasonic mechanical stripping assisted by a vortex generator.
3. The device according to claim 1, characterized in that the titanium dioxide nanoparticles (414) are modified by: mixing the MXene nano sensing layer (413) with 3% of hydrogen peroxide solution by mass fraction, and heating in a water bath at 80 ℃ to obtain the nano sensing material, wherein the titanium dioxide nano particles (414) grow on the MXene nano sensing layer (413) in situ.
4. The device of claim 1, wherein the short peptide molecule (415) is modified by: mixing and dissolving the MXene nano sensing layer (413) of the in-situ grown titanium dioxide nanoparticles (414) according to the mass ratio of 1.
5. The device according to claim 1, further comprising an MXene-based fabric filter (5) for filtering exhaled breath; the MXene-based fabric filter (5) is composed of a platinum nanoparticle-loaded MXene fabric (52) and an active drying agent (51) wrapped in the platinum nanoparticle-loaded MXene fabric (52), wherein the platinum nanoparticle-loaded MXene fabric (52) is obtained by performing electrostatic adsorption on MXene on the surface of cotton fabric and performing in-situ reduction on the loaded platinum nanoparticles on the MXene surface in a chloroplatinic acid solution.
6. The device according to claim 5, characterized in that the platinum nanoparticle loaded MXene fabric (52) is prepared in particular by: the white cotton fabric which is washed by deionized water and dried is soaked in 5mg/mL MXene solution, deposition is carried out for 30 minutes, the white cotton fabric is repeatedly washed and dried and then soaked in 3.86mM chloroplatinic acid solution, reaction is carried out for 30 minutes, and the in-situ reduction of the platinum nanoparticles is realized by utilizing the chemical active surface of MXene.
7. The device according to claim 1, wherein the flexible detection circuit board (42) is composed of a detection circuit substrate (422), a detection circuit (423), a diode circuit connection pad (424) and a sensor connection pad (425), the detection circuit substrate (422) is composed of a polyimide film, the detection circuit (423) mainly comprises a miniature low-power chip and a peripheral resistor-capacitor, and is used for acquiring and processing the electric signal of the MXene acetone sensor (41); and respectively welding the light-emitting diode circuit board (44) and the MXene acetone sensor (41) on the diode circuit connecting pad (424) and the sensor connecting pad (425) through low-temperature soldering tin, so that the electrical connection between the diode circuit board (44), the MXene acetone sensor (41) and the flexible detection circuit board (42) is realized.
8. The device according to claim 7, characterized in that the detection circuit (423) is composed of a microcontroller, a constant current source, an analog-to-digital converter, bluetooth, a low-pass network, a field effect transistor, a light emitting diode, a battery and power management circuit, and a peripheral resistor-capacitor.
9. The device according to any one of claims 1 to 8, further comprising a disposable mask (1), a breather valve (2) and a breather valve housing (3) fixed on the disposable mask (1), wherein the exhaled breath acetone detection label (4) is fixed between the breather valve (2) and the breather valve housing (3) on the outside of the disposable mask (1), and an MXene-based fabric filter (5) is fixed on the breather valve (2) on the inside of the disposable mask (1) for filtering the exhaled breath passing through the breather valve (2).
10. A detection method of exhaled breath acetone based on MXene is characterized by comprising the following steps:
use of the device of any of claims 1-9 to obtain the acetone concentration of exhaled breath, keeping the light emitting diode (442) on during the acetone detection.
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