On-line solid phase extraction gas chromatography-mass spectrometry detection method for organotin in marine sediment

A technology of gas chromatography mass spectrometry and marine sediments, which is applied in the field of on-line solid phase extraction gas chromatography mass spectrometry detection of organotin in marine sediments, can solve the problems of large amount of eluent, etc., and achieve simple operation, high sensitivity, and amazing Satisfactory recovery and reproducibility results

Inactive Publication Date: 2019-11-05
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] The present invention aims to solve the technical problems of the detection method of organotin environmental hormones in marine sediments that usually requires additional stripping, time-consuming, and large amount of eluent, and provides an operation Simple, rapid sample pretreatment, high sensitivity and satisfactory recovery and reproducibility of online solid-phase extraction gas chromatography-mass spectrometry detection method for organotin in marine sediments

Method used

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  • On-line solid phase extraction gas chromatography-mass spectrometry detection method for organotin in marine sediment
  • On-line solid phase extraction gas chromatography-mass spectrometry detection method for organotin in marine sediment
  • On-line solid phase extraction gas chromatography-mass spectrometry detection method for organotin in marine sediment

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Embodiment 1

[0041] Detection of Organotin in Sediment Samples Collected from Zhoushan Antarctic Sea Area

[0042] (1) sample preparation

[0043] The sediment samples collected from the Zhoushan Antarctic sea area were placed in a freeze dryer for freeze-drying for 12 hours, after being ground, passed through an 80-mesh stainless steel sieve, and frozen at -18°C to obtain the samples to be tested.

[0044] (2) Microwave-assisted extraction

[0045] Weigh 2.00g of the sample to be tested, put it in a microwave digestion tank, add 10mL of a mixed solution of acetic acid and methanol (1:1, V / V), and perform microwave extraction to obtain an extract. The microwave extraction power is 200W, and the temperature is 100°C , extraction time 5min.

[0046] (3) Add water to volume

[0047] After distilled water was added to the extract to dilute, the pH was adjusted to 5 with sodium hydroxide solution, and the volume was adjusted to 25 mL to obtain the dilute extract.

[0048] (4) On-line solid ...

Embodiment 2

[0076] Organotin Detection in Sediment Samples Collected from Hangzhou Bay

[0077] (1) sample preparation

[0078] The sediment samples collected in Hangzhou Bay were freeze-dried in a freeze dryer for 242 hours, ground and passed through a 100-mesh stainless steel sieve, and frozen at -18°C to obtain the samples to be tested.

[0079] (2) Microwave-assisted extraction

[0080] Weigh 2.00g of the sample to be tested, add 15mL of acetic acid and methanol (1:1, V / V) mixed solution, then add 3g of copper powder, vortex at 2000r / m for 2min for desulfurization, and centrifuge at 6000r / m for 3-5min , take the centrifugal supernatant, put the centrifugal supernatant in a microwave digestion tank, and extract it through microwave extraction. The microwave extraction power is 100W, the temperature is 120°C, and the extraction time is 5min. The copper powder is treated with dilute hydrochloric acid before use to remove Its surface is oxidized, then rinsed with distilled water to remo...

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Abstract

The invention discloses an on-line solid phase extraction gas chromatography-mass spectrometry detection method for organotin in marine sediment. The method comprises the following steps of (1) samplepreparation; (2) microwave-assisted extraction; (3) water addition for making up to a volume; (4) online solid phase extraction purification-derivatization; (5) concentration and making up to a volume; (6) gas chromatography-mass spectrometry detection; (7) standard curve drawing; (8) sample determination. The method has the advantages that the operation is simple, the sample pretreatment can bequickly completed, a C70 column is adopted for the first time to achieve online enrichment, purification and derivatization, it only takes 12-15 minutes in the whole online solid phase extraction purification-derivatization process, the C70 column can be used multiple times, the service cycle is 6 months, the result is accurate, the detection limit of nine kinds of organotin is 0.2-0.5 microgram / kg, the recovery rate is 78-119%, the relative standard deviation (n=5) is 3.4-9.6%, and the method has high sensitivity, a satisfactory recovery rate and great reproducibility.

Description

technical field [0001] The invention relates to the technical field of marine sediment pollution detection, in particular to an online solid phase extraction gas chromatography mass spectrometry detection method for organic tin in marine sediments. 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, destinations and accumulation a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/54G01N30/88
CPCG01N30/02G01N30/06G01N30/72G01N30/54G01N30/88G01N2030/025G01N2030/062G01N2030/884
Inventor 胡红美孙秀梅张博金衍健应忠真
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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