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A gas chromatography-mass spectrometry detection method for octylphenol and nonylphenol in aquatic products

A mass spectrometry detection and gas chromatography technology is applied in the field of aquatic product quality and safety detection, which can solve the problems of interfering with the measurement results of the instrument, no alkylphenol detection, complex matrix, etc., and achieves the effects of good extraction effect, simple operation and low consumption cost.

Inactive Publication Date: 2014-10-22
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex matrix of aquatic product samples, if the impurities are not removed well during the sample pretreatment process, it may directly interfere with the measurement results of the instrument, or even damage the instrument.
At present, there is no domestic method for the detection of alkylphenols in aquatic products

Method used

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  • A gas chromatography-mass spectrometry detection method for octylphenol and nonylphenol in aquatic products
  • A gas chromatography-mass spectrometry detection method for octylphenol and nonylphenol in aquatic products
  • A gas chromatography-mass spectrometry detection method for octylphenol and nonylphenol in aquatic products

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Gas chromatography-mass spectrometry detection of octylphenol and nonylphenol in grass carp in embodiment 1

[0017] (1) Ultrasonic solvent extraction: Accurately weigh 1.0 g of grass carp samples mixed with a high-speed tissue grinder, add them to a stoppered test tube, and accurately add 10 mL of chromatographically pure acetone; shake for 1 min after stoppering; Perform 40KHz ultrasonic extraction for 10 minutes; then centrifuge the extracted sample for 5 minutes at a speed of 5000 rpm; after centrifugation, use a straw to collect the upper layer extract in a rotary evaporator;

[0018] (2) Enrichment and purification of solid phase extraction: Fill the upper end of the Florisil solid phase extraction column (1 g / 6 mL) with 1 g of anhydrous sodium sulfate for dehydration, first rinse and activate the solid phase extraction column with 5 mL of acetone, and then inject the extract into In the solid-phase extraction column, the liquid flowed out naturally, and the efflu...

Embodiment 2

[0025] Example 2 Gas Chromatography-Mass Spectrometry Detection of Octylphenol and Nonylphenol in Grass Carp

[0026] (1) Solvent ultrasonic extraction: Accurately weigh 3.0 g of grass carp samples mixed with a high-speed tissue grinder, add them into a stoppered test tube, and accurately add 10 mL of chromatographically pure acetone; shake for 1 min after stoppering; Perform 40KHz ultrasonic extraction for 10 minutes; then centrifuge the extracted sample for 5 minutes at a speed of 5000 rpm; after centrifugation, use a straw to collect the upper layer extract in a rotary evaporator;

[0027](2) Enrichment and purification of solid-phase extraction: Florisil solid-phase extraction column, model 1 g / 6 mL, filled with 1.5 g of anhydrous sodium sulfate for dehydration at the top, first rinse and activate the solid-phase extraction column with 5 mL of acetone, and then extract Inject into the solid-phase extraction column, the liquid flows out naturally, discard the effluent; then...

Embodiment 3

[0034] Example 3 Gas Chromatography-Mass Spectrometry Detection of Octylphenol and Nonylphenol in Grass Carp

[0035] (1) Ultrasonic solvent extraction: Accurately weigh 5.0 g of grass carp samples mixed with a high-speed tissue grinder, add them to a stoppered test tube, and accurately add 10 mL of chromatographically pure acetone; shake for 1 min after stoppering; Perform 40KHz ultrasonic extraction for 10 minutes; then centrifuge the extracted sample for 5 minutes at a speed of 5000 rpm; after centrifugation, use a straw to collect the upper layer extract in a rotary evaporator;

[0036] ⑵Enrichment and purification of solid-phase extraction: Fill the upper end of the Florisil solid-phase extraction column with 2g of anhydrous sodium sulfate for dehydration, first rinse and activate the solid-phase extraction column with 5 mL of acetone, and then inject the extract into 1 g / 6 mL of solid-phase extraction In the column, the liquid flows out naturally, discard the effluent; t...

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Abstract

The invention relates to a gas chromatography-tandem mass spectrometric detection technology for octyl phenol and nonyl phenol in aquatic products and belongs to the technical field of the detection for the quality safety of the aquatic products. The gas chromatography-tandem mass spectrometric detection technology comprises the following steps of: taking acetone as an extracting agent for ultrasonically extracting the octyl phenol and the nonyl phenol in the aquatic products; removing interferent from the extractive through solid-phase extraction; drying an eluant by blowing nitrogen and then using the acetone and the derivatization reagent N,O-bi(trimethyl silicon alkyl) fluoroacetamide (BSTFA) / trimethylchlorosilane (TMCS) at a volume ratio of 99:1 for deriving; carrying out selected ion scanning detection by utilizing gas chromatography; and fixing the quantity according to an external standard method. The gas chromatography-tandem mass spectrometric detection technology has the advantages of convenience for operation, excellent reproducibility, accuracy in nature determination, higher recovery rate and capability of rapidly analyzing the octyl phenol and the nonyl phenol in the aquatic products.

Description

technical field [0001] The invention relates to a gas chromatography-mass spectrometry detection technology for octylphenol and nonylphenol in aquatic products, belonging to the technical field of aquatic product quality and safety detection. Background technique [0002] Alkylphenols are a class of endocrine-disrupting, lipophilic organic compounds that are widely used worldwide in detergents, insecticides, plastic additives, textile auxiliaries, and paper and oilfield chemicals. About 500,000 tons of alkylphenol ethoxylates are produced in the world every year, of which nonylphenol ethoxylates (NPnEO) account for 80% of the total production, and the rest are basically octylphenol ethoxylates (OPnEO). In the environment, alkylphenols mainly originate from the degradation of nonionic surfactants, alkylphenol ethoxylates. In the natural environment and sewage treatment process, alkylphenol polyoxyethylene ether is converted into octylphenol and nonylphenol, and enters water...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 孙秀梅郭远明胡红美钟志金衍健丁跃平陈朋何依娜
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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