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Cigarette smoke chromatographic data retention time drifting MWFFT (Moving Windows Fast Fourier Transform) calibration method

A technology of cigarette smoke and time drift, which can be used in measurement devices, instruments, scientific instruments, etc., and can solve problems such as no public reports.

Inactive Publication Date: 2013-09-11
YUNNAN RES INST OF TOBACCO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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  • Cigarette smoke chromatographic data retention time drifting MWFFT (Moving Windows Fast Fourier Transform) calibration method
  • Cigarette smoke chromatographic data retention time drifting MWFFT (Moving Windows Fast Fourier Transform) calibration method
  • Cigarette smoke chromatographic data retention time drifting MWFFT (Moving Windows Fast Fourier Transform) calibration method

Examples

Experimental program
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Embodiment 1

[0034] Each cigarette is filled with cut tobacco of 0.7±0.015g (84mm pipe) by the pipe filling machine, and the smoking machine smokes 20 cigarettes at the same time; the finished cigarettes are put into the smoking machine in groups for smoking, and the Cambridge filter is φ92mm. In the extraction bottle containing the Cambridge filter, add 60ml of the extract, which is a mixed solution of dichloromethane:ethanol=3:2, and extract by ultrasonic for 10min. Then use 20ml of dichloromethane solution to sonicate twice, and combine them in a separatory funnel. Wash twice with 20ml and 10ml of dichloromethane, respectively, and combine. Add 1ml 3% H2SO4 dropwise to adjust the pH to 5-6. Rinse the Cambridge filter extraction bottle with 20ml of distilled water and pour it into a separatory funnel. Fully shake the separatory funnel and let it stand for 5-10 minutes. After the two layers of liquid are completely separated, release the lower layer of liquid from the piston to the rece...

Embodiment 2

[0036] The gas chromatography conditions are as follows: the chromatographic column is DB-35MS (30m×0.25mm, 0.25 μm); the temperature of the injection port is 250°C; the carrier gas is high-purity helium, the flow rate is 1.5ml / min; the split ratio is 30:1 ;Temperature program: initial temperature 50°C, maintain 5min, increase to 280°C at a rate of 5°C / min, maintain 29min, total 80min; mass spectrometry parameters: interface temperature 250°C; ion source temperature 220°C; ionization mode EI+ ; The electron energy is 70eV; the scanning range is 40-400amu. Because the chemical components of the flue gas mainly include heterocyclic hydrocarbons, phenols, aldehydes, ketones, and organic acids, most of which are weak polar substances, so the weak polarity column DB-35MS is selected. The mass spectrum scan range is 40-500. Put the cigarette smoke extract obtained in Example 1 into the sampling device of GC / oa-TOF-MS, inject the same cigarette smoke sample 8 times, obtain the chrom...

Embodiment 3

[0038] Cross-correlation: two chromatographic signals r and s of cigarette smoke extract, there is a lag of 20 points between them, use cross-correlation to find how many points to move the signal s, and the similarity between it and the reference signal r to reach maximum. The s signal is shifted point by point along the x-axis, and then its correlation coefficient with the signal r is calculated. From figure 1 It can be seen that the cross-correlation reaches its maximum value when the signal s and the reference signal r achieve the best match. This is because all peaks in the signal will contribute most to the correlation coefficient when they are aligned with peaks in the reference signal.

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Abstract

The invention relates to a cigarette smoke chromatographic data retention time drifting MWFFT (Moving Windows Fast Fourier Transform) calibration method and belongs to the technical field of tobacco chemical industry and application. A cigarette smoke extractive is a full extractive; the full extractive is subjected to HRMS (High Resolution Mass Spectrometer) analysis; a tobacco product is a cigarette, a cigar, a pipe cut tobacco or a module tobacco leaf which is perfumed or not perfumed. The MWFFT calibration method disclosed by the invention comprises the steps of cross correlation, rapid fourier cross correlation, a moving window strategy, evaluation of calibration mass, and further optimization of an MWFFT speed. Instruments and equipment used by the invention are all purchased from a market. The cigarette smoke chromatographic data retention time drifting MWFFT calibration method disclosed by the invention has the beneficial effects that MWFFT adopts the moving window strategy to replace a subsection strategy, and the defects of leading in flaws by a subsection strategy method and deleting a chromatographic peak point are overcome. A novel application field for a tobacco chemical metrology analyzing technology and an application aspect is explored, and novel method and concept are provided for chemical researches of a cigarette mass spectrum.

Description

Technical field: [0001] The invention relates to a MWFFT calibration method for retention time drift of cigarette smoke chromatographic data, which belongs to the technical field of tobacco chemical industry and application. Background technique: [0002] Chromatography is an instrument commonly used in analytical laboratories to analyze complex systems. A chromatogram consists of peaks associated with components in a mixture. Ideally, the same substance in different samples should have the same retention time in the chromatogram. However, due to instrument drift, uneven mixing of the mobile phase, decomposition of the stationary phase, changes in the chromatographic column during use, and reactions between analytes in the experiment, there will be retention time drift between the chromatographic peaks of the same compound in different samples. Based on the basic chemometric algorithm, when the entire chromatogram is used for similarity calculation, pattern recognition or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86
Inventor 李忠黄静蒋次清魏杰郭生云张虹娟冯文
Owner YUNNAN RES INST OF TOBACCO SCI
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