Light flash thermal desorption-pulse sample injection method for on-site rapid and high-sensitivity detection of drugs

A sensitive detection and thermal desorption technology, applied in the field of ion analysis and detection instruments, can solve the problems of low sensitivity, aggravated peak broadening, complex composition, etc., and achieve the effects of improving detection sensitivity, increasing saturated vapor pressure, and high purging efficiency

Active Publication Date: 2020-05-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Today, the composition of emerging psychotropic drugs and plant samples is very complex. There are more than 170 types of emerging psychotropic drugs that have been controlled in my country. However, it is difficult to volatilize and easy to use traditional continuous purging, metal contact heating thermal analysis. When volatile drugs are mixed with samples, the detection sensitivity of the instrument is low
The main reasons are: 1) some detection instruments with low sampling duty ratio, such as mass spectrometers using DAPI discontinuous sampling, some samples will be taken out of the ionization region by the continuous purging gas and will not be detected in time in the future; 2) it is difficult to Due to the low saturated vapor pressure of volatile drugs, when the heating rate is not fast enough or the temperature is not high enough, the gasification efficiency is low, and the detection sensitivity is even worse; 3) During the sample transmission process, the loss of gaseous drug samples
[0004] In the current design of ion detection instruments such as mass spectrometry or mobility spectrometry, in order to avoid residual contamination of thermal analysis samples, the thermal analysis area and the ionization area are not together, so the sample needs to be transported from the thermal analysis area to the ionization chamber, and the continuous There is a certain diffusion and delay effect when purging passes through the channel with a large diameter, resulting in the decrease of the detection signal and the residue of the sample, which aggravates the broadening of the peak

Method used

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  • Light flash thermal desorption-pulse sample injection method for on-site rapid and high-sensitivity detection of drugs
  • Light flash thermal desorption-pulse sample injection method for on-site rapid and high-sensitivity detection of drugs
  • Light flash thermal desorption-pulse sample injection method for on-site rapid and high-sensitivity detection of drugs

Examples

Experimental program
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Effect test

Embodiment 1

[0055] The above method is applied, 0.1 μg / mL methamphetamine methanol standard solution is sucked with a 1 μL sampling needle and dropped on the tetrafluoro sample cloth, while ensuring that the flash focus of the halogen lamp falls on the sample. After the solvent volatilizes, four The absolute amount of the sample on the fluorocloth was 0.1 ng. The boiling point of methamphetamine is around 200°C. image 3 For 0.1ng methamphetamine halogen light flash thermal analysis pulse injection mass spectrogram, 91 is the fragment ion of methamphetamine [M-C 3 h 9 N] + 150 is the molecular ion plus proton peak of methamphetamine, and 117 is the plus proton peak of acetone dimer.

Embodiment 2

[0057] The above method is applied, and the boiling point of fentanyl is about 500°C, which is a drug that is relatively difficult to volatilize. The 0.1 μg / mL fentanyl methanol standard solution was sucked up with a 1 μL syringe and dropped on the tetrafluorocloth, while ensuring that the flash focus of the halogen lamp fell on the sample. After the solvent volatilized, the concentration of the sample on the tetrafluorocloth The absolute amount is 0.1ng. Figure 4 Mass Spectrum of 0.1ng Fentanyl Halogen Light Flash Desorption Pulse Injection. 337 is the molecular ion plus proton peak of fentanyl, and 117 is the proton plus peak of acetone dimer.

Embodiment 3

[0059] Applying the above method, Figure 5 It is a suspected opium sample detected by halogen lamp flash heat analysis-pulse valve injection, and the sample is provided by the Mukang Border Inspection Station in Mangshi, Yunnan Province. After drying the paste solid, grind it into powder, then use 10mL methanol to ultrasonically dissolve the solution obtained after extraction, then use a 1μL injection needle to absorb the solution and drop it on the black PTFE sample cloth, insert light flash thermal analysis pulse sample injection device. Six components including narcotine, morphine, papaverine, codeine, heroin and thebaine were successfully detected at the same time. Figure 5 The identification of the main mass spectrum peaks in the solid, so it can be confirmed that the solid is opium.

[0060] Table 1 Figure 5 Identification of major mass spectral peaks in

[0061]

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Abstract

The invention discloses a method for realizing on-site rapid high-sensitivity detection of drugs by combining pulse purging and halogen lamp flash thermal desorption. Devices in the method mainly comprise a photo-thermal halogen lamp, a high-temperature-resistant quartz optical lens, a high-voltage pulse valve, a heatable thermal desorption micro-area and the like. The main principle of the methodis that the halogen lamp is used for rapidly heating the heatable thermal desorption micro-area to heat the drugs, and the drugs can be heated to 250 DEG C or above at a focus within 2 seconds, so that the saturated vapor pressure of the drugs is greatly improved, and meanwhile, the diffusion of the samples in space is effectively reduced by virtue of the constructed narrow thermal desorption micro-area; and the instantaneous high-speed purging of a pulse valve is combined to more effectively transmit the sample steam from the heatable thermal desorption micro-area to the ionization area, sothat the utilization rate of the samples is improved. The flash thermal desorption temperature rise speed of the halogen lamp is high, sample residues are small, and compared with a traditional constant-temperature metal contact type heating mode, the method is reduced in power consumption greatly; and the combination of the two fully meets the requirements of on-site portable analytical instruments.

Description

technical field [0001] The invention relates to a mass spectrometry plasma analysis and detection instrument, in particular to an on-site detection instrument for drugs. In essence, the flash heat of halogen light is used to solve the problems of insufficient temperature and too slow heating rate during thermal desorption sample injection, thereby greatly increasing the saturated vapor pressure of drugs, and at the same time, the narrow micro-thermal desorption area constructed effectively reduces the space of the sample. Diffusion; combined with the instantaneous high-speed purge of the pulse valve, the sample vapor is more effectively transported from the heatable thermal desorption micro-zone to the ionization zone, thereby improving the sample utilization rate. Using the light flash thermal analysis-pulse sampling device, the signal intensity of drugs is increased by more than an order of magnitude compared with the traditional continuous purging and accumulation intensity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01J49/04H01J49/00G01N27/64
CPCG01N27/64H01J49/0031H01J49/0459H01J49/049
Inventor 李海洋侯可勇王伟民王爽
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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