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Method for dispersive solid phase extraction gas chromatography-mass spectrometry detection of organotin environmental hormones in marine sediments

A technology of gas chromatography mass spectrometry and marine sediments, which is applied in the field of dispersed solid phase extraction gas chromatography mass spectrometry detection of organotin environmental hormones in marine sediments, achieving the effects of simple operation, high sensitivity and accurate results

Inactive Publication Date: 2019-07-19
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the current domestic and foreign literature, there is no literature report on the application of dispersive solid-phase extraction to the analysis and purification of organotin in marine sediment samples.

Method used

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  • Method for dispersive solid phase extraction gas chromatography-mass spectrometry detection of organotin environmental hormones in marine sediments
  • Method for dispersive solid phase extraction gas chromatography-mass spectrometry detection of organotin environmental hormones in marine sediments
  • Method for dispersive solid phase extraction gas chromatography-mass spectrometry detection of organotin environmental hormones in marine sediments

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Detection of Organotin in Sediment Samples Collected from Zhoushan Antarctic Sea Area

[0043] (1) Sample collection and sample preparation

[0044] The sediment samples collected in the Zhoushan Antarctic sea area were packed with clean aluminum foil and sealed in polyethylene bags, and then transported back to the laboratory in a portable refrigerator, and then dried in a freeze dryer for 12 hours, taken out and dried for 80 hours. Mesh stainless steel sieve, placed in -18 ℃ frozen storage, to be tested.

[0045] (2) Sampling and ultrasonic extraction

[0046] Take by weighing 2.00g of the sample to be tested, add 5mL of acetic acid and methanol mixed solution containing tropolone, in the mixed solution of acetic acid and methanol, the mass concentration of tropolone is 0.03%, and the volume ratio of acetic acid and methanol is 1:9, ultrasonic extraction after vortexing to obtain extract, vortex time 1min, ultrasonic power 200W, ultrasonic temperature 40°C, ultrason...

Embodiment 2

[0079] Organotin Detection in Sediment Samples Collected from Hangzhou Bay

[0080] (1) Sample collection and sample preparation

[0081] The sediment samples collected in Hangzhou Bay were packaged with clean aluminum foil and sealed in polyethylene bags, then transported back to the laboratory in a portable refrigerator, and then dried in a freeze dryer for 24 hours, and then taken out through a 100-mesh stainless steel sieve , stored at -18°C until testing.

[0082] (2) Sampling and ultrasonic extraction

[0083]Weigh 2.00g of the sample to be tested, add 10mL of acetic acid and methanol mixed solution containing tropolone, add 3g of copper powder to the mixed solution of acetic acid and methanol, vortex for 3min, ultrasonic desulfurization, high-speed centrifugation, take the supernatant , then add 10 mL of acetic acid and methanol mixed solution containing tropolone to the centrifuged supernatant, vortex and ultrasonically extract to obtain the extract; in the mixed sol...

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Abstract

The invention discloses a method for dispersive solid phase extraction gas chromatography-mass spectrometry detection of organotin environmental hormones in marine sediments. The method determines organotin in marine sediments by adopting ultrasonic extraction, first dispersion solid phase extraction purification, derivatization and back extraction, second dispersion solid phase extraction and purification, and gas chromatography-mass spectrometry, which is easy to operate and can quickly complete sample pretreatment, wherein two times of dispersion solid phase extraction are firstly used forpurification, the entire dispersion solid phase extraction and purification plus derivatization and back extraction processes only takes 20-30min, the results are accurate, the detection limits of thenine organotins are 0.2-0.5[mu]g / kg, the recovery is 82-117%, and the relative standard deviation (n=5) is 3.8-8.2%, which has high sensitivity and satisfactory recovery and reproducibility and can be used to determine the content of organotin in marine sediments.

Description

technical field [0001] The invention relates to the technical field of detection of marine sediment pollution, in particular to a method for detecting organic tin environmental hormones in marine sediment by dispersive solid phase extraction gas chromatography mass spectrometry. Background technique [0002] As an important class of environmental hormones, organotin is widely distributed in various media such as the atmosphere, water, soil, sediment, and organisms. It has androgenic effects, interferes with the endocrine system, and causes abnormal reproduction, development, and behavior. Used as PVC stabilizer, hull antifouling material, wood preservative, insecticide, fungicide, among which tributyltin, triphenyltin and their degradation products have been listed as "priority pollutant blacklist" by many countries in the world . Although organotin pollution has attracted global attention, it can persist due to its long half-life. Marine sediments are important carriers, ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/12G01N30/72G01N30/04G01N30/86
CPCG01N30/02G01N30/06G01N30/14G01N30/12G01N30/72G01N30/04G01N30/8634G01N2030/062G01N2030/067G01N2030/146G01N2030/126G01N2030/047
Inventor 胡红美郭远明张博金衍健孙秀梅应忠真
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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