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A solid phase microextraction device

An extraction device and extraction head technology, which is applied in the field of analysis and detection, can solve the problems of easy breakage, high price, poor effect of enriching oil characteristic impurities, etc., and achieve the effect of not easy breakage, low cost and favorable adhesion

Active Publication Date: 2016-07-06
INSTITUTE OF ANALYSIS GUANGDONG ACADEMY OF SCIENCES (CHINA NATIONAL ANALYTICAL CENTER GUANGZHOU)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, at present, the enrichment matrix of the micro-extraction head of solid phase microextraction (SPME) is glass fiber, which is easy to break and is very expensive, and the enrichment matrix of glass fiber is not effective in enriching the characteristic impurities of oil.

Method used

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  • A solid phase microextraction device
  • A solid phase microextraction device
  • A solid phase microextraction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Enrichment and determination of a suspected waste oil sample

[0027] 1. Instruments and samples

[0028] 1.1. Agilent6890GC / 5973iMS gas chromatography-mass spectrometry.

[0029] 1.2, the solid-phase microextraction apparatus of the present embodiment, its preparation method is as follows:

[0030] Such as figure 1 As shown, the solid-phase microextraction device of the present embodiment comprises the sleeve in the glass syringe 3 and the syringe, and the sleeve of the present embodiment is a stainless steel column tube 2 (its diameter is 1.10mm, and the length is 92.62mm). The front end of the glass syringe 3 has a stainless steel needle tube 5 (diameter is 0.60mm, length is 4.314cm), the stainless steel needle tube 5 communicates with the stainless steel column tube 2, and the joint is sealed with a rubber septum 4, and an extraction head is fixed in the sleeve. The front end of the extraction head has an enrichment matrix 6, and the enrichment matrix ...

Embodiment 2

[0047] This embodiment is basically the same as Embodiment 1, except that the solid-phase microextraction device has the following differences: the stainless steel needle 1 has a diameter of 0.2 cm and a length of 15 cm. It is etched by chemical etching method. The electrochemical etching step is as follows: a stainless steel needle with a diameter of 0.3 cm is ultrasonicated in a dichloromethane / acetone mixture with a volume ratio of 1:1 for 10 minutes, then ultrasonicated in water for 10 minutes, and taken out at room temperature. The solvent was evaporated to dryness. Then electrochemically etch the 0.5cm of the front end of the stainless steel needle. The electrochemical etching conditions are as follows: place the segment to be electrochemically etched in a 1.8mol / L hydrochloric acid solution for 0.8min at a current intensity of 40mA, and take out the water for 2min. , repeated 8 times to obtain the enriched matrix.

[0048] Using the enrichment matrix to absorb and anal...

Embodiment 3

[0050] The present embodiment is basically the same as Embodiment 1, except that the solid-phase microextraction device has the following differences: its diameter is 0.5 cm, and its length is 30 cm. The enrichment matrix is ​​made by electrochemically etching the front end 2 cm of the stainless steel needle 1. It is formed by etching, and the electrochemical etching steps are as follows: a stainless steel needle with a diameter of 0.5 cm is ultrasonicated for 10 minutes in a dichloromethane / acetone mixture with a volume ratio of 1:1, and then ultrasonicated for 10 minutes in water, and the solvent is evaporated at room temperature. . Then the 2.5cm of the front end of the stainless steel needle is subjected to electrochemical etching. The electrochemical etching conditions are as follows: place the segment to be electrochemically etched in 2.2mol / L hydrochloric acid solution for 1.2min at a current intensity of 20mA, and then take out the water and ultrasonicate for 5min. , r...

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Abstract

The invention discloses a solid phase micro-extraction apparatus. The apparatus comprises a syringe and a sleeve in the syringe, the front end of the syringe has a needle tube, an extraction head is fixed in the sleeve, the front end of the extraction head is provided with an enrichment matrix, the enrichment matrix is coated with an adsorption material, and the enrichment matrix is prepared through the following steps: etching a stainless steel needle with the diameter of 0.3-0.5mm in 1.8-2.2mol / L of a hydrochloric acid solution under 20-40mA through an electrochemical etching process for 0.8-1.2min, taking out the stainless steel needle, and cleaning. The solid phase micro-extraction apparatus has the advantages of difficult breaking, durability, low cost, enrichment of a tiny amount of characteristic impurity components in oil, improvement of the enrichment time, and detection sensitivity improvement.

Description

Technical field: [0001] The invention belongs to the field of analysis and detection, and in particular relates to a solid-phase microextraction device. Background technique: [0002] The detection of waste oil is currently a major technical problem. There is no standard detection method at home and abroad, and it is impossible to accurately identify waste oil. Therefore, it is difficult for relevant government departments to effectively crack down on the illegal behavior of using waste oil as cooking oil. There is an urgent need to study and establish a detection method for waste oil. [0003] The main components of gutter oil are the same as normal edible oil, all of which are fatty acid glycerides. The difference between the two lies in trace impurities. Waste kitchen oil will introduce impurities due to its contact with food and seasonings during the cooking process, and waste oil will also bring impurities into contact with packaging materials during recycling and proc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/10G01N1/40
Inventor 吴惠勤黄晓兰李晴陈江韩
Owner INSTITUTE OF ANALYSIS GUANGDONG ACADEMY OF SCIENCES (CHINA NATIONAL ANALYTICAL CENTER GUANGZHOU)