WO2024173966A1 - Procédé de détermination de la quantité d'une substance psychoactive dans un échantillon - Google Patents

Procédé de détermination de la quantité d'une substance psychoactive dans un échantillon Download PDF

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Publication number
WO2024173966A1
WO2024173966A1 PCT/AT2024/060050 AT2024060050W WO2024173966A1 WO 2024173966 A1 WO2024173966 A1 WO 2024173966A1 AT 2024060050 W AT2024060050 W AT 2024060050W WO 2024173966 A1 WO2024173966 A1 WO 2024173966A1
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Prior art keywords
sample
spectrum
infrared
measuring head
recorded
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PCT/AT2024/060050
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German (de)
English (en)
Inventor
Robert ZIMMERLEITER
Markus Brandstetter
Ivan ALIC
Alexander Ebner
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Research Center For Non Destructive Testing Gmbh
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Publication of WO2024173966A1 publication Critical patent/WO2024173966A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55—Specular reflectivity
    • G01N2021/555—Measuring total reflection power, i.e. scattering and specular
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/4738—Diffuse reflection, e.g. also for testing fluids, fibrous materials

Definitions

  • the invention relates to a method for determining the quantity of a psychoactive substance in a sample by means of diffuse reflection spectroscopy, in which reference spectra of reference samples with a known quantity of the substance are recorded in advance and quantity classes are defined on the basis of the reference spectra, whereupon a near-infrared spectrum of the sample is recorded and assigned to a quantity class by comparison with the reference spectra.
  • Methods are known from the state of the art in which the content of phytocannabinoids in a cannabis sample is analyzed (WO2021242964A1).
  • the sample is dried to less than 10% moisture, homogenized, sieved, placed in a sample container on the measuring window of the spectroscope and rotated during the measurement to compensate for inhomogeneities in the surface texture. Since the sample is usually a plant sample that has a rough surface due to its substance, the analysis is carried out using diffuse reflection near-infrared spectroscopy and a near-infrared spectrum of the sample is recorded.
  • the sample has to be prepared in a complex manner, meaning that the analysis can only be carried out in a stationary laboratory.
  • the sample has to be physically taken, treated and manipulated before it can be subjected to analysis.
  • the invention is therefore based on the object of determining the quantity of a psychoactive substance, for example tetrahydrogen cannabinol (THC), in a sample by means of diffuse reflection spectroscopy in mobile use, in particular by law enforcement agencies, and thereby avoiding preparation of the sample.
  • a psychoactive substance for example tetrahydrogen cannabinol (THC)
  • THC tetrahydrogen cannabinol
  • the invention solves the problem by determining a characteristic spectrum and a permissible deviation from this characteristic spectrum for each quantity class from the reference spectra, after which a near-infrared spectrum of the sample delimited by a film that is at least partially semi-transparent in the near-infrared range is recorded by means of a measuring head of a near-infrared spectrometer, the measuring head and the sample being in contact with the film and facing each other with respect to it, after which the deviation of the recorded near-infrared spectrum of the sample from the characteristic spectrum of each quantity class is determined and a signal is output that is assigned to that quantity class whose characteristic spectrum differs from the recorded near-infrared spectrum of the sample by at most the permissible deviation.
  • the samples to be analyzed are usually handled and stored in small transparent plastic sample bags
  • the content or quantity of a psychoactive substance can be determined through the film of the bag and without the sample having to be taken, manipulated or prepared. If this sample preparation is omitted, the actual determination of the quantity can be carried out with mobile near-infrared spectroscopes, in particular by law enforcement officers in the field.
  • the disadvantage is that the bags usually used contain films made of materials such as polyethylene or other plastics. In the near-infrared wavelength range, these have similar absorption bands to the substances usually to be determined, for example THC.
  • the films are at least semi-transparent to near-infrared light and prevent an evaluation of the measured near-infrared spectrum with regard to the quantity of a substance in a sample without further steps.
  • the invention defines quantity classes and permissible deviations individually associated with the quantity classes in order to reduce the negative influence of the film on the determination so that meaningful statements about the quantity can still be made using the method according to the invention. For example, several reference spectra that have a psychoactive substance content of 10-15 percent by weight can define a quantity class of 10-15, several reference spectra that have a psychoactive substance content of 15-20 percent by weight can define a quantity class of 15-20, etc.
  • a characteristic spectrum is formed from the available reference spectra of such a quantity class, which can first undergo a pre-processing step such as filtering, and then a permissible deviation from this characteristic spectrum is defined.
  • the level of the deviation can depend on various parameters, such as the absorption of infrared light at certain frequency bands, and can differ for each quantity class.
  • a characteristic spectrum is formed from the reference spectra that define a quantity class. In the simplest case, the characteristic spectrum can be the mean value of the reference spectra. In order to enable the most reliable determination of the quantity of a psychoactive substance despite the similar absorption bands of the foil and the sample, it is suggested that the characteristic spectra are formed from the weighted averages of the respective reference spectra.
  • a measured near-infrared spectrum of a sample is now compared with the characteristic spectra of each quantity class. If the reference spectra have undergone an optional pre-processing step described above, the measured near-infrared spectrum also undergoes the same pre-processing step for comparison. Naturally, a measured near-infrared spectrum will not completely match a characteristic spectrum of a quantity class, which is why a permissible deviation is determined for each characteristic spectrum.
  • This permissible deviation is not predetermined, but can be different for each characteristic spectrum and enables compensation for external sources of interference such as the similar absorption band of the foil, since, for example, for quantity classes in which the signal component of the measured near-infrared spectrum originating from the psychoactive substance strongly overlaps with the signal component of an interference source such as the foil, a higher permissible deviation can be defined than for quantity classes in which no high overlap is to be expected.
  • the respective characteristic spectrum can be stored as a regression vector and the reference spectra as reference vectors for each quantity class and the scalar products of the regression vector can be formed with the reference vectors, whereby the permissible deviation from the reference spectra from which the regression vector is formed is determined from the value range of these scalar products.
  • Both the reference spectra and the measured near-infrared spectra can be preprocessed with a Savitzky-Golay filter.
  • a partial least squares algorithm can be used, for example.
  • the measured near-infrared spectrum can also be stored as a measurement vector and multiplied by each regression vector. This multiplication results in a number of scalar products corresponding to the number of quantity classes.
  • To assign a measured near-infrared spectrum to a quantity class it is then checked which of these scalar products differs from one of the scalar products defined for a quantity class by at most the permitted deviation.
  • the measured near-infrared spectrum is then assigned to the quantity class corresponding to this scalar product and the signal of the corresponding quantity class is output so that the person taking the measurement can see which quantity class the measured near-infrared spectrum has been assigned to.
  • the reference spectra of the reference samples can also be recorded using near-infrared spectroscopy.
  • the quantity of the psychoactive substance in a reference sample can be determined using gas chromatography or high-performance liquid chromatography.
  • the assignment of a measured near-infrared spectrum to a specific quantity class means that the measured near-infrared spectrum differs from the characteristic spectrum of this quantity class by at most the permissible deviation
  • two quantity classes can be provided, of which one quantity class is defined by reference spectra of reference samples with a quantity above a threshold value and the other quantity class is defined by reference spectra of reference samples with a quantity below a threshold value.
  • one quantity class is defined by reference spectra of reference samples with a quantity above a threshold value
  • the other quantity class is defined by reference spectra of reference samples with a quantity below a threshold value.
  • the Threshold value of the legally permitted quantity of a psychoactive substance in a sample with a red light being emitted as a signal if this threshold is exceeded and a green light being emitted if the threshold is not reached.
  • another signal such as a flashing red light, can be emitted if the measured near-infrared spectrum of the sample could not be assigned to a quantity class.
  • the permissible deviations can be determined more precisely if at least one reference spectrum is recorded using diffuse reflection spectroscopy, whereby the measuring head and the reference sample are in contact with a film that is at least partially semi-transparent in the near-infrared range and are opposite one another in relation to this in order to record the near-infrared spectrum of the reference sample.
  • diffuse reflection spectroscopy whereby the measuring head and the reference sample are in contact with a film that is at least partially semi-transparent in the near-infrared range and are opposite one another in relation to this in order to record the near-infrared spectrum of the reference sample.
  • the influences of the films on the measurement can be recorded and taken into account. These influences subsequently affect the characteristic spectrum of the corresponding quantity class and the permissible deviations can be better determined, for example, by comparing the reference spectra of the same sample once with and once without a film.
  • reference spectra are recorded from the same reference sample, which is at least partially delimited by semi-transparent films of different materials, and are used to determine the characteristic spectrum as well as the permissible deviation for the corresponding quality class, so that the measured near-infrared spectrum of a sample can be reliably assigned largely independently of the film used.
  • the reference samples can be used for this purpose be limited by small transparent sample bags in which the substances are usually handled and stored.
  • the near-infrared light detected by the measuring head may not come entirely from the sample, as the detector also records background noise and light reflected from other objects, for example.
  • the measuring head In order to inform the user without complicated calibration and display methods whether the signal quality of a recorded near-infrared spectrum of a sample is high enough for a meaningful determination of the quantity of a psychoactive substance, it is therefore proposed to use the measuring head to create a specular reflection spectrum and then to use this and the recorded near-infrared spectrum of the sample to determine the signal portion of diffusely reflected light in the recording, with a warning signal being issued if this signal portion falls below a diffusivity limit value.
  • the sample reflects the near-infrared light diffusely, while other interfering objects in the beam path reflect it regularly, i.e. with specular reflection. If a specular reflection spectrum, i.e. the spectrum of a sample that has the
  • the specular reflection spectrum can preferably be designed in such a way that it reflects the measurement conditions in actual use.
  • a special sample is made from a known, highly specularly reflecting material, such as gold, for a specular reflection spectrum. In this way, the maximum proportion of specularly reflected light to be expected in the expected area of use can be estimated and, accordingly, the minimum signal proportion of diffusely reflected near-infrared light required for a meaningful quantity determination can be determined.
  • the film be part of a sealable bag in which the sample is stored. Since samples are usually stored and handled in sealable bags, the quantity of the psychoactive substance in the sample can be determined without removing it from the bag. This makes manipulating the sample before measurement very difficult, since no direct physical external contact with the sample is possible.
  • the invention also relates to a device for carrying out the method with a computing unit and a near-infrared spectrometer having a measuring head, wherein a storage unit is provided for the quantity classes, the characteristic spectra and the permissible deviations from these, a sample support is arranged opposite the measuring head and the measuring head and the sample support can be displaced relative to one another between a measuring position and an insertion position.
  • the measuring head can record the near-infrared spectrum of the sample, store it in the storage unit if necessary, and the computing unit can process this taking into account the reference spectra stored in the storage unit and their associated data, such as characteristic spectra, permissible deviations and quantity classes.
  • the sample support and the ability to move it between the measuring and insertion positions enable the relative position of the sample to be reproducibly established, so that the measurement of the near-infrared spectra of the samples can be compared to one another and to the reference spectra.
  • the measuring head is pressed against the film and thus against the sample in the measuring position, so that contact between the measuring head, film and sample can be easily established and any layer of air between the measuring head and film and/or sample and film is pushed aside.
  • the contact pressure to reach the measuring position is preferably set, for example via a spring, as this can further increase the reproducibility of the results.
  • the inclination of the measuring head or the angle of incidence for the near-infrared light can be set for the device.
  • the measurement results can also be optimized for different geometries of the device or for different specifications of the measuring head and the near-infrared spectrometer.
  • the shift between the insertion and the measuring position can be carried out in a particularly user-friendly way for mobile applications by providing two arms connected to a handle, with one arm supporting the measuring head and the other arm surrounds the sample support.
  • This allows the device to be easily carried by the person measuring with one hand, while the sample is positioned between the arms with the other hand.
  • the arms enable simple and reproducible contact between the measuring head and the film or between the sample and the film and allow easy application of contact pressure.
  • at least one arm can be moved about a joint so that the contact pressure can be applied more easily due to the leverage effect.
  • the device can be operated one-handed via the handle after the sample has been positioned between the arms.
  • a signal generator such as one or more LEDs, can be attached to the handle in order to output the signal assigned to the respective quantity class.
  • the sample support forms a second measuring head.
  • two near-infrared spectra of the same sample can be recorded at two spatially separate locations during one measurement run. If the measuring heads are opposite each other with respect to the sample, this also enables easy determination at two different locations without having to take the size of the sample into account.
  • the measurement results of the two measuring heads can then be compared, averaged or otherwise processed.
  • two near-infrared spectrometers can be used, each with a measuring head.
  • the quality of the determination depends, particularly in particularly compact versions of the device, on whether the sample can be correctly placed in the measuring position.
  • a color sensor directed towards the recording area for the sample be provided to verify the measuring position. The idea behind this is that the color in the recording area can be determined more easily and therefore more quickly than the near-infrared spectrum of any sample that may be present therein.
  • the color sensor can also be used to carry out a white reference before the near-infrared spectrum is measured.
  • An RGB sensor for example, can be used as a color sensor.
  • the relevant signal component for determining the quantity is the near-infrared light diffusely reflected from the sample.
  • the measuring head also detects specularly reflected light from other objects, whereby the signal component of diffusely reflected light cannot be read directly from the spectrum.
  • the measuring head is designed so that the proportion of diffusely reflected light in the recorded near-infrared spectrum is at least 20%, preferably at least 50%.
  • the near-infrared spectra of two calibration samples are determined using a given measuring arrangement. One of the two calibration samples is designed such that it predominantly reflects diffusely. A white reference sample can be used for this, for example.
  • the second calibration sample is designed such that it predominantly reflects specularly.
  • a gold mirror can be used for this, for example.
  • the signal of the predominantly specularly reflecting sample can be subtracted from the signal of the predominantly diffusely reflecting sample and the relative proportion of the diffusely reflected signal can be determined.
  • the proportion of the measured diffusely reflected light depends on the near-infrared spectrometer used, in particular on the relative arrangement of the light sources and the sensor to each other.
  • the proportion of diffusely reflected infrared light is preferably high in relation to the specularly reflected infrared light, since the diffusely reflected infrared light contains information about the sample and the specularly reflected light comes from other interfering objects in the beam path.
  • Fig. 1 shows the schematic sequence of a method according to the invention
  • Fig. 2 shows the absorption spectra of a sample, a sample delimited by a film that is at least partially semi-transparent in the near infrared range and the film alone,
  • Fig. 3 is a partially broken away schematic perspective view of an apparatus for carrying out the method according to the invention
  • Fig. 4 is a view corresponding to Fig. 3 of a device for carrying out the method according to the invention in a slightly opened position and
  • Fig. 5 is a section along the line V - V of Fig. 4 with the sample inserted in the measuring position on a larger scale.
  • reference spectra of reference samples are recorded. These reference samples contain a known quantity of the substance to be determined, whereby the quantity of the substance to be determined can be determined from the respective spectra.
  • the reference spectra can also be recorded using diffuse reflection spectroscopy and/or other analysis methods, such as high performance liquid chromatography. Due to the determinability of the quantity from the respective reference spectra, quantity classes can therefore be defined in a further step 2. These quantity classes can be defined, for example, via the reference spectra of samples in a certain quantity range, such as "15-20 percent by weight" or "more than 10 percent by volume".
  • the reference spectra are then subjected to one or more optional preprocessing steps, such as passing through one or more filters, and a characteristic spectrum is determined from the reference spectra of a quantity class in step 3. This can be done, for example, by calculating the mean value of the reference spectra of the quantity class. The permissible deviation from this characteristic spectrum is also determined in this step. This deviation can be determined taking into account the individual reference spectra and external circumstances and can be different for each quantity class.
  • the sample P to be determined is delimited by a film that is at least partially semi-transparent in the near infrared range, since commercially available plastic bags in which the substances are usually traded and stored are made of such films.
  • the method according to the invention solves the problem that the absorption bands of many substances to be determined overlap with the absorption bands of a film that is at least partially semi-transparent in the near infrared range and thus a direct determination of the quantity is not possible.
  • the measures according to the invention can reduce the influence of these interference factors to the extent that a meaningful determination is possible again.
  • This circumstance can be further promoted by not defining too many quantity classes, but by setting a threshold value that only delimits two quantity classes from each other. This threshold value can be, for example, the legally prescribed maximum permitted value of the substance.
  • the two quantity classes are then defined using the reference spectra of the reference samples with a quantity above or below this threshold. Since fewer quantity classes have to be checked and the permissible deviation can be kept larger, the measurement can be simplified and accelerated.
  • Another way to carry out the determination reliably despite the disturbing influences of the film is to record at least one reference spectrum in the same way as the near-infrared spectrum of the sample P to be determined.
  • the measuring head and the reference sample are in contact with a film that is at least partially semi-transparent in the near-infrared range and are opposite each other with respect to this.
  • the same reference sample can be recorded with and without a film and used to define a quantity class.
  • a near-infrared spectrum of a sample P is measured, the quantity of which is unknown and the sample P is delimited by a film that is at least partially semi-transparent in the near-infrared range.
  • a film can be, for example, a polyethylene film from which the bags in which the samples are usually traded and stored are at least partially made. If the reference spectra were subjected to an optional pre-processing step, it is recommended that this pre-processing step is also applied to the measured near-infrared spectrum.
  • step 5 the deviation of the measured near-infrared spectrum of the sample P from the characteristic spectrum of each quantity class is determined and then it is determined whether a characteristic spectrum exists from which the measured near-infrared spectrum deviates by at most the permissible deviation of this spectrum. If such a characteristic spectrum is found, the measured near-infrared spectrum is assigned to the quantity class of this characteristic spectrum in step 6. If no such characteristic spectrum is found, the measured Near-infrared spectrum is not assigned to a quantity class and this is output in an optional step 7. Conversely, if a characteristic spectrum is found, a signal is output in step 8 which is specific to the quantity class to which the measured near-infrared spectrum was assigned.
  • Fig. 2 clearly shows how the absorption spectrum of the sample 10 bordered by the film results from the superposition of the absorption spectra of the film 11 and the sample, and how strongly the absorption spectrum of the film 11 influences the resulting absorption spectrum 10.
  • Figs. 3, 4 and 5 show a device for carrying out the method according to the invention.
  • This comprises a measuring head 14 of a near infrared spectrometer and a handle 15 in which the near infrared spectrometer, a storage unit and a computing unit are arranged.
  • the quantity classes, the characteristic spectra and the permissible deviations from these are stored in the storage unit.
  • the device also comprises a sample support 16.
  • the measuring head 14 and sample support 16 can be moved relative to one another between a measuring position and an insertion position.
  • the sample P to be determined is placed in the insertion position on the sample support, as can be seen in Fig. 5.
  • the sample P is bordered by a film which is at least partially semi-transparent in the near infrared range, which in the embodiment shown forms a bag B in which on which the sample P is stored.
  • the measuring head 14 and the sample P are opposite one another with respect to this film, whereby both the measuring head 14 and the sample P are pressed against the film of the bag B.
  • the near infrared spectrum of a sample P can now be recorded according to the invention and the deviation of the recorded near infrared spectrum of the sample P from the characteristic spectrum of each quantity class can be determined.
  • the signal to be output in the method according to the invention is transmitted via a light source
  • the embodiment shown has two arms 19, 20 connected to the handle 15, which preferably apply an adjustable preload to the sample P in the measuring position.
  • One arm 19 encompasses the measuring head 14 and the other arm 20 the sample support 16.
  • both arms 19, 20 are brought closer together in the measuring position.
  • the sample support 16 can form a second measuring head 21, whereby measurement data from two different points on the sample P are obtained during one measuring process.
  • Fig. 4 shows the insertion position in which the two arms 19, 20 are spaced apart from each other so that a sample B can be placed on the sample support 16.
  • a color sensor (not shown) directed towards the receiving space 22 for the sample P can be present.

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Abstract

L'invention concerne un procédé de détermination de la quantité d'une substance psychoactive dans un échantillon (P) au moyen d'une spectroscopie de réflectance diffuse, dans lequel des spectres de référence d'échantillons de référence ayant une quantité connue de la substance sont d'abord capturés (1), et des catégories de quantité sont définies (2) sur la base des spectres de référence, après quoi un spectre proche infrarouge de l'échantillon (P) est capturé et est attribué (6) à une catégorie de quantité sur la base d'une comparaison avec les spectres de référence. L'objectif de l'invention est de concevoir le type de procédé susmentionné de telle sorte que la quantité d'une substance psychoactive telle que le tétrahydrocannabinol (THC) dans un échantillon peut être déterminée au moyen d'une spectroscopie de réflectance diffuse lors d'une utilisation mobile, en particulier par des autorités exécutives, sans qu'il soit nécessaire de prétraiter l'échantillon. À cet effet, un spectre caractéristique et un écart admissible par rapport à ce spectre caractéristique sont déterminés (3) pour chaque catégorie de quantité à partir des spectres de référence, après quoi un spectre proche infrarouge de l'échantillon (P), qui est délimité par un film, dont au moins des parties sont semi-transparentes dans la plage proche infrarouge, est acquis (4) au moyen d'une tête de mesure (14) d'un spectromètre proche infrarouge, la tête de mesure (14) et l'échantillon (P) étant en contact avec le film et étant situés à l'opposé du film, après quoi l'écart du spectre proche infrarouge capturé de l'échantillon (P) à partir du spectre caractéristique de chaque catégorie de quantité est déterminé (5), et un signal est délivré qui est attribué à la catégorie de quantité dont le spectre caractéristique diffère (8) du spectre proche infrarouge capturé de l'échantillon (P) d'une amplitude qui ne dépasse pas l'écart autorisé.
PCT/AT2024/060050 2023-02-20 2024-02-15 Procédé de détermination de la quantité d'une substance psychoactive dans un échantillon WO2024173966A1 (fr)

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ATA50110/2023A AT526965A1 (de) 2023-02-20 2023-02-20 Verfahren zum Bestimmen der Quantität einer psychoaktiven Substanz in einer Probe
ATA50110/2023 2023-02-20

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