A magnetically controlled dispersive solid-phase extraction method for the determination of aniline and benzidine residues in textiles

A technology for dispersing solid phase and textiles, which is applied in measurement devices, material separation, and material analysis, etc., can solve the problems of decreased extraction efficiency of aniline and benzidine, long time consumption, complicated processing steps, etc., and achieves strong selectivity, convenient operation, The effect of omitting the operation steps

Active Publication Date: 2018-01-16
宁波市纤维检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the extraction of aniline and benzidine in textiles mainly uses ether as the extractant, but ether is easy to react with oxygen in the air to form peroxide, and peroxide is easy to oxidize aniline and benzidine, thereby changing the concentration of aniline and benzidine. The nature of aniline leads to a decrease in extraction efficiency
At the same time, ether extraction has the problems of cumbersome pretreatment steps and long time consumption.

Method used

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  • A magnetically controlled dispersive solid-phase extraction method for the determination of aniline and benzidine residues in textiles
  • A magnetically controlled dispersive solid-phase extraction method for the determination of aniline and benzidine residues in textiles
  • A magnetically controlled dispersive solid-phase extraction method for the determination of aniline and benzidine residues in textiles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1.1 Take a representative sample of uniform cotton cloth, cut it into several squares of 0.5cm×0.5cm, mix well, weigh 0.50g into a 10mL polypropylene centrifuge tube, add 0.04% acetic acid / ethanol (5:1, V / V) 5 mL of the solution, ultrasonically extracted for 5 minutes, poured out the supernatant into another centrifuge tube, repeated the operation once, combined the supernatants, and adjusted the pH to 9.0 with ammonia water respectively.

[0022] 1.2 Enrichment, purification, and magnetic control separation, then accurately weigh 3.0 mg of magnetic polyamine-based submicron molecularly imprinted particles, disperse them in the supernatant, and mix them thoroughly with ultrasound for 2 minutes. Under the action of an external magnetic field, the magnetic polyamine-based Submicron molecularly imprinted particles gathered on the wall of the centrifuge tube, the solution was discarded, the magnetic polyamine-based submicron molecularly imprinted particles were rinsed with ...

Embodiment 2

[0028] 2.1 Take a representative homogeneous acrylic fabric sample, cut it into several squares of 0.5cm×0.5cm, mix well, weigh 0.50g into a 10mL polypropylene centrifuge tube, add 0.01% acetic acid / ethanol (5:1, V / V) solution 5mL, after ultrasonic extraction for 5min, pour out the supernatant into another centrifuge tube, repeat the operation once, combine the supernatant, and adjust the pH to 9.0 with ammonia water.

[0029] 2.2 Enrichment, purification and magnetic control separation, then accurately weigh 3.0 mg of magnetic polyamine-based submicron molecularly imprinted particles, disperse them in the supernatant, and mix them thoroughly by ultrasonic waves for 2 minutes. Under the action of an external magnetic field, the magnetic polyamine-based Submicron molecularly imprinted particles gathered on the wall of the centrifuge tube, the solution was discarded, the magnetic polyamine-based submicron molecularly imprinted particles were rinsed with 2 mL of water, the eluent...

Embodiment 3

[0031] 3.1 Take a representative uniform wool fabric sample, cut it into several squares of 0.5cm×0.5cm, mix well, weigh 0.50g into a 10mL polypropylene centrifuge tube, add 0.04% acetic acid / ethanol (5:1, V / V) solution 5mL, after ultrasonic extraction for 5min, pour out the supernatant into another centrifuge tube, repeat the operation once, combine the supernatant, and adjust the pH to 9.0 with ammonia water.

[0032] 3.2 Enrichment, purification and magnetic control separation, and then accurately weigh 3.0 mg of magnetic polyamine-based submicron molecularly imprinted particles, disperse them in the supernatant, and mix thoroughly by ultrasonic for 2 minutes, and make the magnetic polyamine-based The submicron molecularly imprinted particles gather on the wall of the centrifuge tube, discard the solution, rinse the magnetic polyamine-based submicron molecularly imprinted particles with 2 mL of water, discard the eluent, and finally elute with 0.5 mL of methanol, collect th...

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Abstract

The invention discloses a magnetron disperse solid extraction method for residual aniline and benzidine measured in textiles. The method is characterized by comprising the steps of: taking a uniform representative sample, cutting the sample into several small squares, mixing well, weighing 0.40-0.6g of the sample, conducting ultrasonic extraction by using 0.01-0.05 (v / v )% of acetic acid / ethanol solution in a 10mL polypropylene centrifuge tube, adding an appropriate amount of aqueous ammonia to adjust the pH value to 8.5 to 9.5, using a right amount of spherical magnetic polyamine submicron molecular imprinting particles for enrichment and purification, conducting solid-liquid separation by using magnetic separation technology, then eluting with 0.4-0.6mL of methanol and detecting by HPLC assay. The method uses acetic acid solution-alcohol mixed solution for extraction, uses spherical magnetic polyamine submicron molecular imprinting particles for enrichment purification and separation on extract, omits complex liquid-liquid separation step, and has the advantages of less matrix interference, simple operation, low price, fastness, good sensitivity and precision. The method is applicable to suitable for sample pretreatment for analysis of residual aniline and benzidine in textiles.

Description

technical field [0001] The invention relates to a magnetically controlled dispersive solid-phase extraction method for the determination of aniline and benzidine residues in textiles, and more specifically relates to the adsorption and enrichment of magnetic polyamine-based submicron molecularly imprinted particles of aniline and benzidine residues in textiles. Its magnetic control separation method. Background technique [0002] Aniline and benzidine are important intermediates for the synthesis of azo dyes, which can cause acute / chronic poisoning through inhalation, ingestion or absorption through the skin. Aniline can cause methemoglobinemia, toxic liver disease, etc., and benzidine can cause Contact dermatitis, hemorrhagic cystitis, and bladder cancer. Banned azo dyes such as residual aniline and biphenyl in textiles are ecological safety indicators stipulated in the national mandatory standard GB 18401-2010 "National Basic Safety Technical Specifications for Textile Pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 金美菊刘优娜钱微君那英
Owner 宁波市纤维检验所
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