Detection method for trace amount of organic tin in marine products

Abstract

The invention belongs to the technical field of marine product detection, and particularly relates to a method for determining the trace amount of organic tin in marine products. The method comprises the steps that a to-be-determined sample is ground into powder after being preprocessed, the powder is soaked, extracted, frozen, purified, derived, processed through a cleanert florisil column and concentrated to obtain a to-be-determined sample solution; series of different-concentration organic tin mixed standard solutions are added in equivalent blank matrixes same as a sample matrix, soaked for a certain time and then processed through the mode same as the sample; a gas chromatography-tandem mass spectrum detection system is adopted to determine the standard mixed solutions, and a working curve is drawn; the to-be-determined sample solution is determined, the peak area ratio is obtained from a chromatogram chart of the to-be-determined sample solution, regression is performed on the working curve to obtain regression values, and then the concentration of all target objects in the to-be-determined sample can be calculated. The detection method can determine the concentration of butyltin and triphyltin simultaneously, is sensitive, accurate, rapid, simple and convenient and can be applied to detection of the organic tin in the marine products.

Description

technical field

[0001] The invention belongs to the technical field of seafood detection, and in particular relates to a method for determining trace organotin in seafood. Background technique

[0002] Organotin pollution in the marine environment has attracted widespread attention at home and abroad, and has become a research hotspot in the current environmental field. Organotin compounds are typical endocrine disruptors and persistent toxic substances with androgenic effects. They were first synthesized by Lowig in 1852. In the 1940s, the synthesis and application of various organotin compounds developed rapidly. Adding tributyltin and triphenyltin to the antifouling paint of ships and offshore structures to kill fungi, algae and molluscs attached to ships is an important application of organotin, and it is also an important application of organotin in the marine environment. main source. In my country, about 3,000 tons of antifouling coatings such as tributyltin enter t...

Examples

Embodiment 1

[0038] The present invention is used to analyze the organic tin in oysters sold in Shanghai.

[0039] (1) Sample treatment: shell the oysters, take the edible parts, wash them with ultrapure water, filter them, dry them in a freeze dryer for 48 hours, pulverize them with a ball mill, and pass them through a 0.45mm sieve to obtain freeze-dried oyster powder.

[0040] (2) Weigh 0.5g oyster powder, add 10mL extractant (methanol: acetic acid = 9:1, containing 0.03wt% tropolone), mix well, ultrasonicate for 30min, and let stand for 30min. Take 5 mL of the supernatant, freeze in -85°C refrigerator for 2 h, and centrifuge at 5000 r / min for 5 min. Transfer all the supernatant, add 100mg N-propylethylenediamine, shake for 10min (150r / min), centrifuge for 5min (5000r / min). Transfer the supernatant to a test tube, add 40mL acetic acid / sodium acetate buffer solution (c=1mol / L, pH=4.5), 2g sodium chloride, 5mL n-hexane, 100μL tripropyltin internal standard stock solution (c =1mg cation / L...

Embodiment 2

[0056] The detection method of the present invention is used to analyze the organotin in the biological organotin standard reference material (ERM-CE477).

[0057] Weigh 0.5g organotin standard reference substance (ERM-CE477) for processing. Carry out with reference to step (2) in Example 1.

[0058] Standard mixed solution: Accurately weigh 7 parts of blank mussel powder equal to the standard reference substance, add 0, 10, 20, 40, 100, 200, 400 μL organic tin mixed standard solution (monobutyltin, dibutyltin, tributyltin , diphenyltin, triphenyltin standard mixture, 5mg cation / L), add methanol to make up to 2.0mL, after immersion for 24 hours, take the same method as the sample to extract, purify, derivatize, florisil The soil column was adjusted to 0.5mL.

[0059] The gas chromatography-tandem mass spectrometry detection system was used to measure the standard mixture, and the peak area ratio (the ratio of the peak area of ​​the target substance to the peak area of ​​the ...

technical field

[0001] The invention belongs to the technical field of seafood detection, and in particular relates to a method for determining trace organotin in seafood. Background technique

[0002] Organotin pollution in the marine environment has attracted widespread attention at home and abroad, and has become a research hotspot in the current environmental field. Organotin compounds are typical endocrine disruptors and persistent toxic substances with androgenic effects. They were first synthesized by Lowig in 1852. In the 1940s, the synthesis and application of various organotin compounds developed rapidly. Adding tributyltin and triphenyltin to the antifouling paint of ships and offshore structures to kill fungi, algae and molluscs attached to ships is an important application of organotin, and it is also an important application of organotin in the marine environment. main source. In my country, about 3,000 tons of antifouling coatings such as tributyltin enter t...

Examples

Embodiment 1

[0038] The present invention is used to analyze the organic tin in oysters sold in Shanghai.

[0039] (1) Sample treatment: shell the oysters, take the edible parts, wash them with ultrapure water, filter them, dry them in a freeze dryer for 48 hours, pulverize them with a ball mill, and pass them through a 0.45mm sieve to obtain freeze-dried oyster powder.

[0040] (2) Weigh 0.5g oyster powder, add 10mL extractant (methanol: acetic acid = 9:1, containing 0.03wt% tropolone), mix well, ultrasonicate for 30min, and let stand for 30min. Take 5 mL of the supernatant, freeze in -85°C refrigerator for 2 h, and centrifuge at 5000 r / min for 5 min. Transfer all the supernatant, add 100mg N-propylethylenediamine, shake for 10min (150r / min), centrifuge for 5min (5000r / min). Transfer the supernatant to a test tube, add 40mL acetic acid / sodium acetate buffer solution (c=1mol / L, pH=4.5), 2g sodium chloride, 5mL n-hexane, 100μL tripropyltin internal standard stock solution (c =1mg cation / L...

Embodiment 2

[0056] The detection method of the present invention is used to analyze the organotin in the biological organotin standard reference material (ERM-CE477).

[0057] Weigh 0.5g organotin standard reference substance (ERM-CE477) for processing. Carry out with reference to step (2) in Example 1.

[0058] Standard mixed solution: Accurately weigh 7 parts of blank mussel powder equal to the standard reference substance, add 0, 10, 20, 40, 100, 200, 400 μL organic tin mixed standard solution (monobutyltin, dibutyltin, tributyltin , diphenyltin, triphenyltin standard mixture, 5mg cation / L), add methanol to make up to 2.0mL, after immersion for 24 hours, take the same method as the sample to extract, purify, derivatize, florisil The soil column was adjusted to 0.5mL.

[0059] The gas chromatography-tandem mass spectrometry detection system was used to measure the standard mixture, and the peak area ratio (the ratio of the peak area of ​​the target substance to the peak area of ​​the ...

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