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Dispersive solid-phase extraction and gas chromatography-mass spectrometry detection method of organic tin environmental hormones in marine products

A gas chromatography-mass spectrometry and disperse solid-phase technology, which is applied in the field of seafood pollution detection, can solve problems such as unsuitable for batch sample processing, complex operation of solid-phase extraction, expensive instruments, etc., and achieve satisfactory recovery and reproducibility High sensitivity, 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

For seafood with high fat and pigment content, it usually requires combined purification of gel permeation chromatography and solid phase extraction of silica gel column or Florisil column, while gel permeation chromatography equipment is expensive and requires a large amount of elution solvent , the solid-phase extraction method is complicated to operate, and requires extraction column activation, sample loading, rinsing, and elution, which takes a long time and is not suitable for batch sample processing

Method used

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  • Dispersive solid-phase extraction and gas chromatography-mass spectrometry detection method of organic tin environmental hormones in marine products
  • Dispersive solid-phase extraction and gas chromatography-mass spectrometry detection method of organic tin environmental hormones in marine products
  • Dispersive solid-phase extraction and gas chromatography-mass spectrometry detection method of organic tin environmental hormones in marine products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Detection of organotin in small yellow croaker

[0045] (1) Sample collection and sample preparation

[0046] Pack the collected small yellow croaker samples with clean aluminum foil and seal them in polyethylene bags, then transport them back to the laboratory in a portable refrigerator, remove the scales and skin, and take the muscles along the back. The samples are not larger than 0.5cm×0.5cm×0.5 cm, homogenized with a high-speed tissue grinder, dried in a freeze dryer for 12 hours after homogenization, taken out and stored at -18°C until testing.

[0047] (2) Sampling and ultrasonic extraction

[0048] Take by weighing 1.00g sample to be tested, add 5mL of the mixed solution of acetic acid and methanol 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 powe...

Embodiment 2

[0085] Detection of Organotin in Penaeus vannamei

[0086] (1) Sample collection and sample preparation

[0087] Pack the collected samples of Penaeus vannamei with clean aluminum foil and seal them in polyethylene bags, then transport them back to the laboratory in a portable refrigerator, remove the head, shell, and appendages, and take the muscle. The sample is not larger than 0.5cm× 0.5cm×0.5cm, homogenize with a high-speed tissue grinder, dry in a freeze dryer for 24 hours after homogenization, take it out and store it in a freezer at -18°C until testing;

[0088] (2) Sampling and ultrasonic extraction

[0089] Weigh 1.00g 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, ultrasonic desulfurization, high-speed centrifugation, take the supernatant, Then add 10mL of acetic acid and methanol mixed solution containing tropolone to the centri...

Embodiment 3

[0119] Organotin detection in oysters

[0120] (1) Sample collection and sample preparation

[0121] Pack the collected oyster samples with clean aluminum foil and seal them in polyethylene bags, then transport them back to the laboratory in a portable refrigerator, remove the shells, take the edible part, the sample is not larger than 0.5cm×0.5cm×0.5cm, and use Homogenize with a high-speed tissue masher, dry in a freeze dryer for 18 hours after homogenization, take it out and store it in a freezer at -18°C until testing;

[0122] (2) Sampling and ultrasonic extraction

[0123] Weigh 1.00g of the sample to be tested, add 8mL of acetic acid and methanol mixed solution containing tropolone, add 1g of copper powder to the mixed solution of acetic acid and methanol, vortex, ultrasonic desulfurization, high-speed centrifugation, take the supernatant, Then add 8 mL of acetic acid and methanol mixed solution containing tropolone to the centrifuged supernatant, vortex and ultrasonic...

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Abstract

The invention discloses a dispersive solid-phase extraction and gas chromatography-mass spectrometry detection method of organic tin environmental hormones in marine products. The organic tins in themarine products are measured by adopting ultrasonic extraction, freeze degreasing, first time dispersive solid-phase extraction purification, derivatization and back extraction, second time dispersivesolid-phase extraction purification, and gas chromatography-mass spectrometry method. The method is simple in operation, the sample pretreatment can be completed quickly, wherein twice dispersive solid-phase extraction is adopted for purification for the first time, the entire dispersive solid-phase extraction purification process plus the derivatization and back extraction only takes 20-30 min,the result is accurate, the detection limit of nine organic tins is 0.4-1.0 mu g / kg, the recovery rate is 80-117%, the relative standard deviation (n=5) is 3.8-7.5%, the sensitivity is relatively high, the recovery rate and reproducibility are satisfactory, and the dispersive solid-phase extraction and gas chromatography-mass spectrometry detection method can be used for the measurement of the content of the organic tins in the marine products.

Description

technical field [0001] The invention relates to the technical field of seafood pollution detection, in particular to a dispersive solid phase extraction gas chromatography mass spectrometry detection method for organotin environmental hormones in seafood. 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. Dissolved organotin compounds are more likely to migrate into sea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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 胡红美王姮孙秀梅张博应忠真金衍健
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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