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Microcolumn enrichment sample introduction method

A sampling and enrichment technology, applied in the direction of sampling, instruments, analysis materials, etc., to achieve high enrichment multiples, avoid measurement errors, and save the effect of concentration steps

Active Publication Date: 2017-07-18
WUHAN SEPENRICH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The difference is that liquid phase microextraction (mLLE) uses a very small amount of organic solvent (hundreds of microliters) to extract hundreds of milliliters of samples once, and the operation steps are not much different from traditional LLE.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In this example, polycyclic aromatic hydrocarbon sample fluorene was used as the analysis target to investigate the enrichment effect of the method

[0041] (1) Preparation of Microextraction Column Syringes

[0042] 1. Pretreatment of capillary

[0043] (1) Wash the quartz capillary (320 μm, I.D.) with 1mol / L NaOH solution at a flow rate of 0.1mL / min for 2 hours, fill the column with NaOH solution, seal both ends with silicone rubber, and place it in a gas chromatography column oven at 50°C for reaction 2h;

[0044] (2) Rinse with ultrapure water until neutral at a flow rate of 0.2mL / min; then rinse with 1mol / L HCl at a flow rate of 0.1mL / min for 1 hour, then wash with ultrapure water until neutral;

[0045] (3) Then dry at 160° C. with nitrogen for 10 h.

[0046] 2. Preparation of Octyl Microextraction Columns

[0047] Add 140 μL of tetraethoxysilane (TEOS) and n-octyltriethoxysilane (C8-TEOS) to a mixed solution of 300 μL of methanol, 20 μL of water and 20 μL of ...

Embodiment 2

[0060] In this example, 7 kinds of organochlorine pesticides are used as the application results of the investigation method for the analysis target

[0061] (1), preparation of microextraction column injection needle: same as embodiment 1;

[0062] (2), sample analysis

[0063] 1. Sample: Use 7 kinds of organochlorine pesticides (α-HCH, β-HCH, γ-HCH, δ-HCH, P, P-DDE, P, P-DDD and O, P-DDT) to make the concentration 100ng / L mixed aqueous solution was used as a sample solution; the above-mentioned 7 kinds of organochlorine pesticides were used to prepare a dichloromethane solution with a concentration of 100 μg / L, which was used as a control group.

[0064] 2. Sample pretreatment and sample injection: same as implementation case 1

[0065] 3. Analysis method

[0066] Analytical instrument: gas chromatograph with mass spectrometry detector (GC-MS).

[0067] Main chromatographic conditions: Injection port temperature 250°C, injection in splitless mode for 2 minutes. Temperat...

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Abstract

The invention belongs to the field of sample pretreatment, and concretely discloses a microcolumn enrichment sample introduction method, which comprises the steps of adopting a microextraction column with an extraction function as a sample introduction needle, enabling a sample to flow through the sample introduction needle, and during the period, extracting an analyte into an extracting medium in the sample introduction needle; then filling the sample introduction needle with an organic solvent, keeping for a certain time, and enabling the extracted analyte to dissolve in the organic solvent in the microextraction column so as to form a sample introductions solution; finally, sealing one end of the sample introduction needle, directly inserting the other end of the sample introduction needle into a gas chromatography sample introduction port, enabling the sample introduction solution to expand by heat so as to automatically release from the sample introduction needle to the sample introduction port, and finishing the sample introduction operation. The microcolumn enrichment sample introduction method provided by the invention integrates separation, enrichment and sample introduction into a whole, the dosage of the sample and the organic solution is less, and the enrichment efficiency is high; the necessary nitrogen blowing concentration operation in a solid-phase extraction method is omitted, so that the work efficiency of sample pretreatment can be greatly improved.

Description

technical field [0001] The invention belongs to the field of sample pretreatment, and in particular relates to a microcolumn enrichment sample injection method. Background technique [0002] The main purpose of sample pretreatment is to convert the target substance in the sample into a measurable form through the process of extraction, purification and concentration, and to remove the interfering substances in the sample matrix. Traditional sample pretreatment methods include Soxhlet extraction, liquid-liquid extraction (LLE), etc. However, these methods have disadvantages such as long processing time, cumbersome operation, and large consumption of organic solvents to varying degrees. In order to solve these problems, a series of new sample pretreatment methods appeared later, such as ultrasonic-assisted extraction (USAE), microwave-assisted extraction (MWAE), pressurized solvent extraction (PLE) and supercritical fluid extraction (SCFE), etc. Effectively improve the extrac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/16G01N30/06G01N30/08
CPCG01N30/06G01N30/08G01N30/16G01N2030/062G01N2030/085G01N2030/009G01N30/18B01J20/28042B01J2220/64G01N1/2214G01N1/405G01N2001/2217
Inventor 邢钧叶晓雨黄文瑜
Owner WUHAN SEPENRICH TECH CO LTD
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