Detection method for phthalate ester residue

A detection method and phthalate technology are applied in the detection field of phthalate residues, which can solve the problems of long extraction time and low extraction efficiency, and achieve the effects of less impurity interference, fast extraction speed and improved enrichment effect.

Inactive Publication Date: 2009-08-05
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Similar methods have one thing in common, that is, in the extraction process, the appropriate organic solvent is selected through the "similar compatibility principle", and the extraction of the target compound is achieved by increasing the temperature or applying a certain pressure. Although the separation speed and efficiency can be improved, However, there are still problems

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  • Detection method for phthalate ester residue
  • Detection method for phthalate ester residue
  • Detection method for phthalate ester residue

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: Detection of release amount and total content of phthalates (PAEs) in solid samples.

[0035] Accurately weigh 0.5g of the pulverized test sample, put it in a 15mL sample bottle, use water, simulated saliva, acid sweat and normal saline as the extraction bottom liquid (the amount of the bottom liquid is 10mL), add the internal standard substance (ISTD) adjacent Didecyl phthalate (DNDP) (CAS No. 84-77-5) 100 μL was sealed with a bottle stopper lined with polytetrafluoroethylene septa, then soaked for 15 min, ultrasonically assisted in an ultrasonic bath at 40°C for 45 min, and transferred Leave the water bath, cool, purify and enrich through the solid-phase extraction column filled with multi-walled carbon nanotube materials, and wash the collection bottle with 2×3mL ether at the same time, pass the cleaning solvent through the column together, let it stand for 10min, then use 10mL ether Wash three times, and concentrate the eluent by rotary evaporation at ...

Embodiment 2

[0045] Example 2: Research on detection and analysis methods of phthalates (PAEs).

[0046] 1 Materials and methods

[0047] 1.1. Instruments and reagents:

[0048] Agilent HP6890GC gas chromatograph equipped with 5972MSD (with HP-5 elastic quartz capillary column (5% phenylpolysiloxane)); Dionex.ASE200 fast solvent extractor (with 11mL extraction pool, fiber extraction sleeve); SUPELCO Visiprep TM DL 12-hole solid-phase extraction device; Branson 200ULTRASONIC Cleaner ultrasonic instrument; Büchi Rotavapor R-200 rotary evaporator; Büchi Heating Bath B-40 water bath. Empty tubes for polypropylene SPE cartridges: Varian TM Or equivalent (with polyethylene sieve plate with 20μm aperture); multi-walled carbon nanotubes (specification, purity ≥ 95%, specification 10-20nm, length 5-15μm, ash content ≤ 0.2wt%, surface area 40-300m 2 / g) is provided by Shenzhen Nami Port Co., Ltd., and the modification and activation method of multi-walled carbon nanotubes is as follows: weigh a ...

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Abstract

The invention discloses a test method for the residual phthalate ester, including the steps that after a solid sample is decomposed into blocks which are immersed in the dummy body fluid, the transferring amount of the phthalate ester in the solid sample under the condition with the dummy body fluid can be obtained through the auxiliary lixiviation by water bath ultrasound, the purification and the enrichment of solid extraction columellas filled with multi-walled carbon nano-tubes, and the measurement by a gas mass spectroscopy; and meanwhile, after the solid sample is decomposed into blocks, the total content of the phthalate ester in the solid sample can be obtained through the extraction by an accelerating solvent extraction method, the purification and the enrichment of small solid extraction columns filled with multi-walled carbon nano-tubes, and the measurement by a gas mass spectroscopy. The invention has the advantages of less dosage of organic solvent, rapid extraction speed, less impurity interference, high sample recovery ratio, and the like. In addition, prefilled small solid extraction columns are made from the multi-walled carbon nano-tubes, thereby the enrichment effect of the phthalate ester in the dummy body fluid extract of samples to be tested can be greatly improved, and a phthalate ester hazard evaluation system can be better perfected according to the difference of the total residual quantity and the dissolved quantityof phthalate ester in the solid sample.

Description

technical field [0001] The invention belongs to the technical field of product safety and detection, and in particular relates to a detection method for phthalate residues. Background technique [0002] Phthalate esters are commonly used plasticizers in the manufacture of soft polyvinyl chloride (PVC), and their potential toxicity has already attracted close attention, especially the bioaccumulation and potential carcinogenic risks of long-chain phthalate esters, as well as the biological The destructiveness of the hormone secretion function makes the evaluation of the impact of phthalates on human health through food, water, air and other exposure routes become one of the hot issues in the environment and health. [0003] International research on phthalate plasticizer residues in consumer products has been going on for some time, and the potential environmental and health risks of phthalates have prompted countries to take corresponding measures to limit their use. Europe...

Claims

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Application Information

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IPC IPC(8): G01N30/72G01N30/04
Inventor 陈军孙成柳艳朱建民陈骏峰
Owner NANJING UNIV
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