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Top cavity syringe needle tip deriving method for sample and its uses

A technology for derivatization and derivatization of reagents, applied in the field of analytical chemistry, can solve the problems of easy pollution, high cost, time-consuming, etc., and achieve the effect of reducing dosage, low cost, and improving sensitivity

Inactive Publication Date: 2012-12-05
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to propose a method and its application based on needle tip derivatization in the headspace of a sample in view of the problems existing in the above-mentioned prior art. It is time-consuming, laborious, and requires a large amount of organic solvents for conventional derivatization methods. Insufficiency of high and easy to cause pollution and the shortcomings of the derivatization method combined with solid-phase microextraction, liquid phase microextraction technology and derivatization technology are integrated, and the extraction and separation, purification, concentration and derivatization of analytes are completed in one step. A sample pretreatment method that combines low volatility solvents with volatile derivatization reagents to improve method operability

Method used

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  • Top cavity syringe needle tip deriving method for sample and its uses
  • Top cavity syringe needle tip deriving method for sample and its uses
  • Top cavity syringe needle tip deriving method for sample and its uses

Examples

Experimental program
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Effect test

Embodiment 1

[0018] GC-MS analysis of volatile acids in tobacco: according to the properties of volatile acids, select a suitable derivatization reagent A (N, O-bis(trimethylsilyl) trifluoroacetamide or N, O-bis(trimethylsilyl) trifluoroacetamide A mixture of fluoroacetamide, n-decane, and n-dodecane), and draw 2 μL of derivatization reagent A with a microsyringe. After heating the sealed headspace vial with a certain amount of sample (0.1g tobacco powder) at 80°C for a period of time, insert the needle of the microinjector into the headspace of the sample through the sealing cap of the sample vial; depress the microinjector carefully The plunger of the derivatization reagent is suspended on the needle tip of the microinjector, and the derivatization time is 1 min; subsequently, the liquid droplet is sucked back, and the gas chromatographic analysis is performed directly. Using retention time and selected ions for qualitative analysis, the analysis results are shown in Table 1:

[0019] T...

Embodiment 2

[0022] Mass spectrometry analysis of aldehydes and ketones in smoke: According to the properties of aldehydes and ketones, select a suitable derivatization reagent B (aniline or phenylhydrazine or nitrophenylhydrazine), and draw 3 μL of derivatization reagent B with a micro syringe. Use a headspace vial to collect a certain amount of smoke (the amount of smoke from a cigarette), seal it and immediately insert the needle of the microinjector into the headspace of the sample through the sealing cap of the sample vial; carefully depress the plunger of the microinjector so that The derivatization reagent was suspended on the needle tip of the micro-syringe, and the derivatization time was 2 min; then, suck back the liquid drop, and then suck in a certain amount of acetonitrile (to dilute the sample), and repeatedly pull the plunger of the syringe to make the mixture even, and then directly carry out electro Spray mass spectrometry (positive ion mode) analysis. Adopt molecular weig...

Embodiment 3

[0026] Selective analysis of aldehyde compounds in smoke: According to the properties of aldehyde compounds, select a suitable derivatization reagent C (diphenylamine), and draw 2 μL of derivatization reagent C with a micro-syringe. Use a headspace vial to collect a certain amount of smoke (the amount of smoke from a cigarette), seal it and immediately insert the needle of the microinjector into the headspace of the sample through the sealing cap of the sample vial; carefully depress the plunger of the microinjector so that The derivatization reagent was suspended on the needle tip of the microsyringe, and the derivatization time was 1.5 min; subsequently, the liquid droplet was sucked back, and the droplet was added to the MALDI target of matrix-assisted laser desorption ionization (MALDI) Fourier transform mass spectrometry, and the liquid Mass spectrometry (positive ion mode) analysis was performed directly after the drops dried. Adopt precise molecular weight calculation, ...

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Abstract

The present invention provides a derivatization method and the application thereof of a sample based on the needlepoint in a top empty bottle, and includes the following procedures: 1, using a minim injector to suck the derivatization reagent and insert the needlepoint into the empty top of a top empty battle in which the sample is preset. 2, making the derivatization reagent form a liquid drop hanging on the needlepoint of the injector and exposes in the empty top of the sample. 3, after a period of derivatization, sucking back the derivatization reagent, and the derivatization process is finished. 4, taking the injector out conducts analysis by instruments directly according to requirements. The derivatization method can be applied in top air of the tobacco sample, or acid ingredient in cigarette smoke and the derivatization of aldehyde ketone ingredient. The present invention has the advantages of simple operation, high efficient derivatization, and lower cost; a trace of derivatization reagent can meet the derivatization purpose of the analysis requirements without memory effect and discrimination effect of the analyzed object. Simultaneously, the present invention combines the liquid phase extraction technology and the derivatization means, improves the sensitivity by the enrichment function of the liquid phase extraction, reduces the dosage of the extraction solvent, and shortens the preparation time.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a sample pretreatment method before analysis. Specifically, it is a method based on needle tip derivatization in the headspace of a sample and its application. The method can realize the extraction and concentration of analytes , Derivatization proceeds simultaneously. Background technique [0002] Some chemical components (more polar amines, organic acids, aldehydes and ketones, etc.) have unique advantages in the analysis of chromatographic mass spectrometry. However, direct chromatographic analysis of such components usually cannot obtain better analysis results . To improve the chromatographic behavior of such substances by gas chromatography, it is often necessary to derivatize them. Usually, the sample preparation process is cumbersome, and the more mature method is: firstly, solvent extraction, followed by repeated solvent extraction processes, and finally derivatizatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N1/28
Inventor 谢剑平孙世豪宗永立谢复炜
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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