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ESI-MS (electrospray Ionization mass spectrometry) for rapidly detecting organic tin ions in aqueous solution through complexation and enrichment

A technology of organotin and aqueous solution, which is applied in the preparation of test samples, measuring devices, and material analysis by electromagnetic means.

Inactive Publication Date: 2015-04-29
ELECTROMECHANICAL PRODS DETECTING TECH CENT OF SHANGHAI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The entire analysis and detection process does not exceed 5 minutes

Method used

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  • ESI-MS (electrospray Ionization mass spectrometry) for rapidly detecting organic tin ions in aqueous solution through complexation and enrichment
  • ESI-MS (electrospray Ionization mass spectrometry) for rapidly detecting organic tin ions in aqueous solution through complexation and enrichment
  • ESI-MS (electrospray Ionization mass spectrometry) for rapidly detecting organic tin ions in aqueous solution through complexation and enrichment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: the complexation of diethyldithioformic acid ion and organotin ion

[0038] Use diethyldithioformate ion (DDTC) as a kind of organotin ion complexing agent in the present embodiment, with tributyltin ion ((C 4 h 9 ) 3 sn + ) as an example. The conditions in this example are all optimized results.

[0039] Complexation of diethyldithioformate ions and organotin ions: first, a mixture containing 0.5 mg / L tributyltin ions ((C 4 h 9 ) 3 sn + ) after adjusting the pH value of the water sample to 4.0 (this experiment can be carried out under the condition of pH3-7), take out a 5.0mL volume of water sample and add it to a centrifuge tube, add 500μL of 20g / L DDTC aqueous solution to this water sample, and then At the same time, a mixed solution of 50 μL tetrachlorethylene and 500 μL acetone (as a dispersant) was quickly added to the water sample using a disposable syringe, and immediately sonicated until a uniform microemulsion was formed (sonication time ...

Embodiment 2

[0043] Embodiment 2: the establishment of standard curve

[0044] With tributyltin ion ((C 4 h 9 ) 3 sn + ) as an example.

[0045] (1) Add 5 mL of water samples with a pH value of 4.0 into six 25 mL glass centrifuge tubes, in which tributyltin ions ((C 4 h 9 ) 3 sn + ) concentrations are 0, 0.2, 0.5, 1.0, 1.5, 2.0mg / L;

[0046] (2) operate according to the step of embodiment 1, prepare tributyltin ion ((C 4 h 9 ) 3 sn + ) perchlorethylene standard solution of DDTC complex;

[0047] (3) The standard sample prepared above was directly analyzed by electrospray tandem mass spectrometer in MRM mode (multiple ion reaction mode), and the precursor ion was m / z728.3 ([(C 4 h 9 ) 3 Sn) 2 +DDTC] + ), the product ions are m / z382.0 ([(C 4 h 9 ) 2 Sn+DDTC] + ) and m / z177.0 ([Sn+But] + ), see Table 1 and Figure 16 shown. The present invention can also adopt the SCAN mode, and the scanning ion is m / z728.3 ([(C 4 h 9 ) 3 Sn) 2 +DDTC] + , see Table 1 and Figure ...

Embodiment 3

[0052] Embodiment 3: the mensuration of soluble organotin ion in toy sample

[0053] Reference standard: EN71-3:2013

[0054]This embodiment shows the situation when the sample to be tested is a toy, and all accessible parts on the toy sample are tested.

[0055] 1. Sample preparation

[0056] For toys such as textile fabrics, plastic or rubber, use scissors or pliers to cut the material into small pieces of 5mm×5mm as the samples to be tested.

[0057] For toys with paint, ink or similar coatings, use a clean razor blade to scrape off the part as the sample to be tested.

[0058] For toys that are liquid paint or ink, take a part of the paint and apply it on a clean glass plate, let it dry naturally at room temperature, and then scrape it off as the sample to be tested. If the sample to be tested cannot be dried at room temperature, it should be dried in an oven according to the temperature used, and scraped off to obtain the sample to be tested.

[0059] All powdery samp...

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Abstract

The invention discloses ESI-MS (electrospray Ionization mass spectrometry) for rapidly detecting organic tin ions in an aqueous solution through complexation and enrichment, and provides a rapid ESI tandem mass spectrometer analysis method for detecting the organic tin ions in the aqueous solution through organic complexation and dispersive liquid-liquid micro-extraction enrichment simultaneously. According to the method, Na-DDTC (diethyldithiocarbamate) is taken as a complexing agent, and under the condition that pH is 3-7, DDTC ions in the complexing agent is subjected to complexation with various types of organic tin ions in the aqueous solution to form various corresponding different types of organic tin metal complex compounds; the dispersive liquid-liquid micro-extraction technology is adopted for extraction, hundredfold extraction and enrichment is performed simultaneously on the organic tin complex compounds in the solution, finally, an ESI tandem mass spectrometer is adopted directly for qualitative and quantitative analysis of the organic tin complex compounds in the solution, and corresponding qualitative and quantitative information of the organic tin ions is obtained. The ESI-MS has the advantages of high enrichment factor of the organic tin ions in the aqueous solution, complete enrichment, simplicity, convenience and rapidness in operation, qualitative and quantitative analysis of the organic tin ions and the like.

Description

technical field [0001] The invention relates to the field of detection and analysis of organotin ions in aqueous solution, and proposes an electrospray mass spectrometry method for rapid detection of organotin ions in aqueous solution by simultaneously utilizing organic complexation and dispersion liquid-liquid microextraction for enrichment. Background technique [0002] Organotins are of the general formula R n wxya (4-n) A general term for a class of substances, where n=1 to 4, R is an alkyl or aromatic group, and X is an inorganic or organic acid group, halogen, etc. The toxicity of organotin is mainly determined by its chemical structure, where R 3 SnX is the most toxic, R 2 wxya 2 and RSnX 3 relatively less toxic. Organotins are fat-soluble, easy to enter organisms, have reproductive toxicity to animals, and have poisonous effects on the human nervous system, skin, liver and endocrine system. In the past 20 years, the problem of organotin pollution has attracted...

Claims

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Application Information

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IPC IPC(8): G01N27/64G01N1/40
Inventor 于文佳卫碧文郑翊林莉高欢
Owner ELECTROMECHANICAL PRODS DETECTING TECH CENT OF SHANGHAI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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