Solid-phase microextraction head as well as preparation method and application thereof

A solid-phase microextraction head and solution technology, applied in the detection field, can solve problems such as complicated operation, sample interference, unsuitable elution, etc., and achieve the effects of saving costs, saving costs, and improving processing efficiency

Active Publication Date: 2021-11-02
潍坊海关综合技术服务中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, for the above methods, the liquid-liquid extraction has a wide range of extracts, and there are many co-produced substances, which may cause interference to extremely complex samples; moreover, liquid-liquid extraction relies on manual work and cannot be automated
In addition, if the solid-phase extraction method of "GB / T20752-2006 Determination of Nitrofuran Metabolite Residues in Pork, Beef, Chicken, Pork Liver and Aquatic Products" is used for pretreatment by liquid chromatography-tandem mass spectrometry, it will also There are the following disadvantages: ①The column needs to be pre-washed with methanol and water → the extract solution is passed through the column → the impurities are washed with water → eluted, and the operation is complicated; ②The cost of the solid-phase extraction column is relatively high; ③It can be used by automatic solid-phase extraction However, the price of fully automatic solid-phase extraction instrument is high, and it is difficult to equip it in general laboratories; ④ There are problems such as easy clogging and unsuitable elution for viscous and colloidal complex samples

Method used

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  • Solid-phase microextraction head as well as preparation method and application thereof
  • Solid-phase microextraction head as well as preparation method and application thereof
  • Solid-phase microextraction head as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1 Method for preparing a tooth sign solid phase microexture head

[0052] 1. The 7 g of the polyacrylonitrile PAN powder is dissolved in 100 ml of dimethylformamide (DMF), and the mixture is constantly stirred at room temperature to ensure uniform dissolution.

[0053] 2, OASIS HLB particles (30 μm) are formed using a ball mill at 240 rpm for 2 hours.

[0054] 3, 1 g of HLB was mixed with 10 ml PAN solution to obtain the final PAN-HLB slurry. It was then mixed with 1800 rpm under the oscillator to be mixed 12 hours to provide a mixture of pellets sufficiently uniform.

[0055] 4, use the toothpick to pick up the PAN-HLB slurry, with a length of about 1 cm, so that it is evenly applied to the toothpick, and then take it once after drying.

[0056] 5. Even the toothpick in the solvent solution at a rate of 1500 rpm (methanol, isopropyl alcohol and acetonitrile (MeOH / IPA / ACN, 50: 25: 25) for a total of 15 minutes to remove the residue.

[0057] 6. Pretreatment of t...

Embodiment 2

[0058] Example 2 Study on Adsorption Effect of Toothpog Follow Microenection

[0059] 1. Derived to a certain concentration of nitrofuran metabolite standards, specifically:

[0060] A 4 nitrofuran metabolite of 200 μl of concentration of 0.1 μg / ml was taken, and 17 ml of 0.125 mol / L hydrochloric acid solution and 1.0 ml of 2-nitrobenate were added, and the constant temperature oscillator was derived at a constant temperature oscillator of 37 ° C. The 1 ml of the potassium hydrogen phosphate solution was adjusted between pH 7.2 to 7.4 with a 1 mol / L sodium hydroxide solution and a water solution of 0.1 mol / L of hydrochloric acid.

[0061] 2, the average derived standard is divided into two copies, one with ethyl acetate reaction, nitrogen blowing, reacting, and calculates the quality of derivatives 0 The other part was extracted with a prepreg for 3 minutes with a prepared toothg, and after removing the extract, the remaining liquid was reversed with ethyl acetate, and the...

Embodiment 3

[0063] Example 3 Repeated Utilization of Toothpog Follow Microenest

[0064] 1. Treatment of the toothpog solid phase microextment of the residual sample is obtained 3 times in ethyl acetate, the nitrogen blowing, and retracted, and the desorption and residual case of the teeth signs and the microextament should be studied.

[0065] The results showed that the toothpog solid phase of the present invention was taken out, and the desorption rate was 99% at once, and the analysis rate was 100%, and the analysis was eluted by ethyl acetate, and the target can be adsorbed. All of the things were desirable, and there was no residue.

[0066] 2, the above-described treatment of the toothpick solid phase microexture is again performed, and the recovery rate is calculated.

[0067] In order to assess the repeatable use of the teeth signs, it is carried out by analyzing pork with 40 μl of NFS standard (concentration of 0.1 μg / mL), and the adsorption experiment of 5 cycles was carried out....

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Abstract

The invention provides a solid-phase microextraction head as well as a preparation method and application thereof, and belongs to the technical field of detection. The invention provides a novel solid-phase microextraction concept, and a toothpick solid-phase microextraction head is developed on the basis of the concept and is used for improving and optimizing a pretreatment technology in the process of detecting the residual quantity of nitrofuran metabolites in animal-derived food. The microextraction head has the characteristics of no solvent, high extraction speed, good reproducibility, low sample consumption, simplicity and convenience in operation, capability of performing field analysis and the like. The solid-phase microextraction head provided by the invention has efficient adsorption and desorption capabilities on nitrofuran metabolites and excellent impurity removal capability, the quantitation limit of the nitrofuran metabolites can be effectively improved, and the effect is obviously superior to that of a detection result of the national standard.

Description

Technical field [0001] The invention belongs to the field of detection, and more particularly to a solid phase microendure and its preparation method and application thereof. Background technique [0002] At present, the detection standards of nitrofuran drug metabolites have mainly "GB / T21311-2007 animal-derived foods] High-performance liquid chromatography - tandem mass spectrometry," GB / T20752 -2006 Pork, beef, chicken, pig liver and aquatic product measuring liquid chromatography-series mass spectrometry, the method in the above standard is high performance liquid chromatography - tandem mass spectrometry (HPLC -MS / MS), its common extraction purification method is liquid extraction and solid phase extraction. [0003] However, for the above method, the liquid extraction extract has a wide range of substances, and there is more substance, which may cause interference to extremely complex samples; and liquid extraction is dependent to manually completion, and automation c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/062G01N2030/067
Inventor 宫小明
Owner 潍坊海关综合技术服务中心
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