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On-line solid phase micro-extraction method in capillary column and apparatus therefor

A technology of solid-phase microextraction column and extraction device, which is applied in the field of extraction, can solve the problems of high analysis cost of extraction stationary phase, high analysis cost, difficulty in ensuring the repeatability of analysis results, and unsatisfactory extraction and enrichment multiples, so as to achieve operability And the effect of improved stability, convenient installation and replacement, and easy operation

Active Publication Date: 2005-06-22
ANMAI TECH DALIAN INSTR
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  • Summary
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  • Description
  • Claims
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Problems solved by technology

However, the amount of adsorbed stationary phase in conventional fiber-needle solid-phase microextractors is ≤1 μL, which limits the extraction enrichment factor and cannot meet the requirements of many trace analysis; in addition, the manual offline operation mode is still used in the operation process, which is difficult to guarantee the analysis The reproducibility of the results; and the short service life of the extraction fiber in the extractor (≤30 times) also increases the analysis cost
Capillary in-column extraction technology has been paid more and more attention by analysts due to its advantages of large volume of extraction stationary phase, short extraction equilibrium time, high degree of cross-linking of extraction stationary phase, less prone to ghost peaks, and low analysis cost. Difficulties in the combined use of analytical instruments limit its popularization and citation

Method used

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  • On-line solid phase micro-extraction method in capillary column and apparatus therefor
  • On-line solid phase micro-extraction method in capillary column and apparatus therefor
  • On-line solid phase micro-extraction method in capillary column and apparatus therefor

Examples

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Embodiment 1

[0038] The parameters of the sample pretreatment device for extracting and enriching organic hydrocarbon pollutants in drinking water and surface water using the device and method of the present invention are as follows:

[0039] The capillary solid-phase microextraction column (9) is a 5M×0.53mm inner diameter×1.2μm film thickness OV-1 elastic quartz capillary column; the desorption temperature is 240°C; the transfer tube (8) uses a 1.2M×120μm inner diameter elastic quartz capillary, and The temperature of the heating tube is 220°C.

[0040] 15mL water sample with a concentration of 10μg / L nC 12 ~nC 19 , the dynamic extraction time is 2.5 minutes, analyzed by Agilent 6890-Plus gas chromatograph, the analysis spectrum obtained is as follows Figure 2A ; while the same sample (containing 10 μg / L nC 12 ~nC 19 ), and the extraction time is 35 minutes, the result is as spectrum Figure 2B . In addition, the same sample (10 μg / L nC in 15 mL of water) was tested in a short tim...

Embodiment 2

[0043] The device and method of the invention are used to extract and enrich organic pollutants such as trace polycyclic aromatic hydrocarbons in water, the sample volume is 300mL, and the concentration of organic components is 0.2-2 μg / L. The desorption temperature of the extraction column (9) is 310° C., and other conditions are the same as in Example 1. Its analytical spectrum is as image 3 .

Embodiment 3

[0045] The device and method of the invention are used to extract the residual components of organochlorine pesticides in water. The sample volume is 30mL, the concentration of pesticide residues is ~0.25μg / L, and the extraction time is 5 minutes. The desorption temperature of the extraction column (9) is 290° C., the gas chromatographic detector is an electron capture detector, and other conditions are the same as in Example 1. Its analytical spectrum is as Figure 4 .

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Abstract

This invention relates to a capillary column solid phase coated with extraction phase micro extraction method and the device used with the analysis device, which comprises the following: one capillary solid phase micro extraction column with inner wall coated with solid phase, one six-way valve, extraction column heating box and transmission tube with desorption sample, micro three-way valve, micro air-extracting pump and assistant gas. The sample enters the extraction column under the assistant gas and micro air-extracting pump. After the flow and extracting of the sample, it rotates the six-way valve and immediately starts extraction column heating box to rapidly heat the capillary solid phase micro extraction column.

Description

technical field [0001] The invention relates to a solid-phase micro-extraction technique, which is used for sample pretreatment and target component extraction and enrichment in chromatographic analysis and instrumental analysis. In particular, it relates to a solid-phase micro-extraction device in a capillary column that can be used online with an analytical instrument. [0002] The present invention also relates to an extraction method realized by using the above-mentioned device. Background technique [0003] In environmental protection, surface water, groundwater, drinking water, tea and other agricultural by-products and organic pollutants in food analysis, different forms of sample pretreatment techniques have been used, such as liquid-liquid extraction, liquid-solid extraction, gas Purge-and-trap, solid-phase extraction, solid-phase microextraction and other technologies to realize the phase transfer and selective enrichment of the target components in the sample and...

Claims

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Application Information

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IPC IPC(8): B01D11/04
Inventor 关亚风王涵文朱道乾王海龙
Owner ANMAI TECH DALIAN INSTR
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