Extraction head detachable type solid phase micro extraction probe and preparation method thereof

An extraction head and detachable technology, applied in the field of analytical chemistry, can solve the problems of high cost, easy breakage, high analysis cost, and achieve the effects of strong operability and reliability, high sensitivity and reproducibility, and simple preparation process.

Active Publication Date: 2010-12-15
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The commercialized SPME probe is about 700-800 yuan a piece, which can be used about 100 times, and the analysis cost is relatively high. It can only be used once when analyzing biological samples, which is expensive; and its extraction head is mainly made of quartz fiber, which is easy to use. break off
The main reason for the high price of commercialized SPME probes is that the extraction head cannot be replaced, and the entire probe needs to be scrapped after the extraction capacity drops, resulting in serious waste and economic pressure on scientific researchers.

Method used

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  • Extraction head detachable type solid phase micro extraction probe and preparation method thereof
  • Extraction head detachable type solid phase micro extraction probe and preparation method thereof
  • Extraction head detachable type solid phase micro extraction probe and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of the extraction head detachable solid-phase microextraction probe:

[0037] Cut a 1cm polydimethylsiloxane (PDMS) tube (inner diameter 0.2mm,) for use; cut about 2.5cm of steel wire with a diameter of 0.1mm, immerse it in acetone for ultrasonic cleaning, take it out and dry it for use; coat one end of the steel wire with Cover with a very thin layer of high-temperature epoxy resin glue, insert the PDMS tube into the steel wire and stick it firmly to make the extraction head. Coat high-temperature epoxy resin, quickly pull it out from the perforated rubber septum, and then cover the steel wire with a very thin layer of glue, and then quickly put it on the PDMS tube; use small pliers to flatten the inner tube of the SPME probe Form a depression, the degree of flattening the tweezers makes the gap span inside the depression = the diameter of the steel wire × 0.9, so that the steel wire can pass through the flattened place of the tweezers and be stuck, and it ...

Embodiment 2

[0044] Preparation of the detachable solid-phase microextraction probe The preparation is as in Example 1.

[0045] Accurately prepare 20mL of BTEX aqueous solution with a concentration of 1mg / L, use commercial 30μm PDMS fiber and the detachable solid-phase microextraction probe, and conduct headspace extraction for 20min under magnetic stirring at a speed of 1500r / min. After taking it out, insert Thermal analysis was carried out in the GC inlet for 1 min, and the MS spectrum was obtained (as shown in Figure *). Comparing the peak areas of the two compounds, it is known that the detachable SPME probe has a better extraction effect than the commercial 30 μm PDMS fiber. The chromatographic conditions are the same as in Example 1. The results are shown in Table 2 and image 3 shown.

[0046] Table 2 Data table of BTEX peak area extracted by self-made needle and commercial needle

[0047]

[0048]

[0049] The results showed that repeating the above experiments with a cu...

Embodiment 3

[0051] Preparation of detachable solid-phase microextraction probe with extraction head: cut a 1cm polydimethylsiloxane (PDMS) tube (inner diameter 0.2mm) for use; cut about 2.0cm of metal wire with a diameter of 0.1mm, dip it into Ultrasonic cleaning in acetone, take it out and dry it for later use; coat one end of the wire with a very thin layer of high-temperature epoxy resin glue, put the PDMS tube into the wire and stick it to make the extraction head, the specific method is: put the metal The wire is inserted into the rubber septum that has been inserted into the hole with a micro-syringe in advance, and high-temperature epoxy resin is coated on the metal wire, and it is quickly pulled out from the rubber septum with holes to cover the wire with a very thin layer of glue. Then quickly put on the PDMS tube; slightly bend the free metal wire of the self-made extraction head with tweezers to form two bends, and the distance from the outermost part of the bent part to the lon...

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Abstract

The invention belongs to the field of analytical chemistry and relates to an extraction head detachable type solid phase micro extraction probe and a preparation method thereof. The preparation method comprises the following steps of: shearing a polydimethyl siloxane tube and a metal wire; coating a layer of high-temperature epoxy resin glue on the metal wire and sleeving the polydimethyl siloxane tube on the metal wire for fixedly bonding to obtain a self-made extraction head, wherein a sleeve is arranged at one end of the self-made extraction head, and a free metal wire is arranged at the other end of the self-made extraction head; then properly extruding at the position of an inner tube of a solid phase micro extraction probe suit, which is away from the tail end by 0.2-0.5cm so as to generate a dent, or bending the free metal wire part of the self-made extraction head by more than one bent; and inserting the metal wire into the inner tube. The probe is simple and convenient in theuse and preparation processes; the probe can be continuously used by extracting the extraction head and inserting a new self-made extraction head after being used; and the repeated selective examination times can reach 80-120 times. The cost of each probe is one thousand of that of the traditional commercial probe and has strong operability and reliability.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a solid phase microextraction probe and a preparation method thereof. Background technique [0002] Solid phase microextraction (SPME) is a new sample processing technology, which integrates sampling, extraction, concentration, and sample introduction. It has the advantages of simplicity, convenience, time saving and labor-saving, and does not use solvents. One of the 100 technological innovations with potential. This technology has been widely used in the fields of environment, food, medicine, clinical analysis and so on. [0003] The commercialized SPME probe is about 700-800 yuan a piece, which can be used about 100 times, and the analysis cost is relatively high. It can only be used once when analyzing biological samples, which is expensive; and its extraction head is mainly made of quartz fiber, which is easy to use. break off. The main reason for the high price of commer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/285B01J20/30B01D15/08
Inventor 欧阳钢锋何淑明朱芳吴佩燕栾天罡
Owner SUN YAT SEN UNIV
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