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Method for the detection of chlorophenols in textiles by hollow fiber liquid phase microextraction

A detection method and fiber liquid technology are applied in the field of analytical chemistry to achieve the effects of high extraction efficiency, increased solubility and improved extraction efficiency

Inactive Publication Date: 2017-09-22
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] At present, there is no relevant standard method and literature for the simultaneous determination of 10 chlorophenol compounds in textiles by high performance liquid chromatography

Method used

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  • Method for the detection of chlorophenols in textiles by hollow fiber liquid phase microextraction
  • Method for the detection of chlorophenols in textiles by hollow fiber liquid phase microextraction
  • Method for the detection of chlorophenols in textiles by hollow fiber liquid phase microextraction

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Experimental program
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Effect test

Embodiment 1

[0061] A method for detecting chlorophenols in hollow fiber liquid-phase microextraction textiles, specifically comprising the following steps:

[0062] (1) Preparation before the experiment:

[0063] 1) Sodium hydroxide solution (0.1 mol / L): Weigh 0.4 g of sodium hydroxide and dissolve it in water and dilute to 100 mL, shake well and set aside.

[0064] 2) Hydrochloric acid solution (3 mol / L): Pipette 25 mL of hydrochloric acid, dilute to 100 mL with water, shake well and set aside.

[0065] 3) Methanol water solution: Methanol and water are mixed at a volume ratio of 1:1, and the pH of the solution is adjusted to 1 with the above-mentioned hydrochloric acid solution.

[0066] 4) Magnetic stirrer: with micro-rotor.

[0067] 5) Polypropylene hollow fiber tube: 600 μm in diameter, 200 μm in wall thickness, and 0.2 μm in pore size. The polypropylene hollow fiber tube was cut into small pieces with a length of about 4.5 cm (volume about 10 μL), ultrasonically cleaned in aceton...

Embodiment 2

[0078] According to the method of embodiment 1, carry out following experiment:

[0079] Such as figure 1 As shown, the ratio of the concentration of the analyte in the receiving phase after extraction to the concentration of the analyte in the sample before extraction is the enrichment factor, according to the enrichment factor EF = C1 / C2 (where C1 is the concentration of the analyte in the extractant, C2 is the initial concentration of the sample solution), and the 1µg / mL chlorinated phenol standard solution was analyzed and determined, and the enrichment factors of 2,3,6-TrCP, 2,3,4,5-TeCP, and PCP were respectively 95 .

[0080] Such as figure 2 As shown, in order to verify the extraction and enrichment effect of this method on 10 kinds of chlorophenols and whether the properties of analytes changed before and after extraction, the direct injection chromatograms of 10 kinds of chlorophenol standard solutions were compared with those after enrichment by liquid phase micr...

Embodiment 3

[0082] According to the method of embodiment 1, carry out following experiment:

[0083] Purification effect test, such as image 3 As shown, because the hollow fiber membrane has a microporous structure, some macromolecular compounds and suspended particles can be filtered out by the hollow fiber membrane during extraction and enrichment, so it is more suitable for sample pretreatment of complex matrices. In this method, the sample solution enriched and extracted by the fiber tube is compared with the sample solution not enriched by the fiber tube. The results show that the purification effect of this method is obvious, and it has outstanding sample purification function. It can be used for direct analysis of complex matrix samples.

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Abstract

The invention belongs to the field of analytical chemistry, and relates to a detection method of chlorinated phenols in a textile through hollow fiber liquid-phase microextraction. The detection method comprises the steps of extracting a sample by using acetone, after concentrating an extracting solution to nearly dry, dissolving by using normal hexane to obtain a solvent, then taking a porous hollow fiber tube as a carrier of microextraction solvent, and transferring all extracted solvent into a high performance liquid chromatograph for subsequent assay determination. The detection method provided by the invention has the advantages that a hollow fiber tube liquid-phase microextraction method is adopted, namely, the hollow fiber tube is taken as the carrier of the microextraction solvent, the extraction, gathering, separation and purification are integrated into a whole, the extraction efficiency is high, the organic solvent consumption is less, the extraction is fast and sensitive, and the like; according to experiment results, the recovery rate and precision of the method both satisfy the demands, and the method can be used for the detection of chlorinated phenol mildew preventives in the textile, and has wide application prospect.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a method for detecting chlorinated phenols in textiles by liquid-phase microextraction of hollow fibers, in particular to a hollow fiber-liquid-liquid two-phase microextraction method for enriching and extracting chlorinated phenols in textiles Purification detection method. Background technique [0002] Chlorine-containing phenolic compounds have a wide range of uses in the textile industry. They are commonly used in textiles, leather, weaving pastes and printing pastes as an anti-mold preservative, which is convenient for the storage of semi-finished textile products (such as gray cloth) and finished products. In the production process (the main sizing process), a small amount of preservatives are generally added, which are commonly used in the storage and transportation of cotton fibers and wool, and are also raw materials for rubber anti-aging agents, mineral dressing agents...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08G01N2030/027
Inventor 高永刚牛增元张艳艳叶曦雯高山王铭苏杰孙立曲京武
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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