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Matrix dispersion purification tube for phthalate ester detection

A phthalate and purification tube technology, applied in the field of pretreatment purification tubes, can solve the problems of high cost, expensive instruments and high operating costs, and achieve the effect of accurate instruments

Inactive Publication Date: 2013-03-27
SHANGHAI ANPEL SCI INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In 2008, my country released GB / T 21911-2008-Methods for the determination of phthalates in food, especially for the detection of phthalates in oily substances. The pretreatment method uses GPC to remove oils interference, but GPC instruments are expensive, the general price of imported ones is more than one million, and domestic ones generally cost more than 700,000, and the operating cost is high, requiring a large amount of reagents, because the purification by GPC generally needs to be concentrated 50 times, so The requirements for the selection of reagents are also very high. Generally, imported pesticide-grade reagents are required, which are expensive. A GPC instrument can only process one sample at a time, and it takes more than 30 minutes to process a sample at the fastest.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: For a matrix containing a lot of water, the implementation steps: 2mL solution sample, add 1G pesticide residue sodium chloride, add 4mL 10% tert-butyl methyl ether acetonitrile solution, shake well, centrifuge at 4000r / min for 5min, add the supernatant In the purification tube, after fully shaking, centrifuge at 4000r / min for 5min, and take the supernatant for analysis (1PPM spiked recovery is 82%-105%)

Embodiment 2

[0020] Example 2: For a matrix containing part of oil and part of water, the implementation steps: take a sample of 1.0g, dissolve it with 1-2mL of n-hexane, then extract twice with 4mL of acetonitrile, centrifuge, collect all the acetonitrile layer, and pour it into a purification tube. Fully shake, centrifuge at 4000r / min for 5min. The supernatant was analyzed (1PPM spiked recovery rate was 80%-94%).

Embodiment 3

[0021] Example 3: For pure oil products, the implementation steps: 0.5g sample, fully shake or vortex mixed with 4mL acetonitrile, centrifuge, collect the upper layer (acetonitrile layer), and then extract once with 4ML acetonitrile, pour all into the purification tube, fully shake, Centrifuge at 4000r / min for 5min, and take the supernatant for analysis (1PPM spiked recovery rate is 87%-96%, diphenyl ester 76%).

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PUM

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Abstract

The invention provides a matrix dispersion purification tube for phthalate ester detection, and relates to development of a pretreatment purification tube for detecting various phthalate esters in different matrixes. A purification process of the tube comprises: (1) based on different matrixes, placing a filler in an empty purification tube according to a ratio regulated by a requirement; (2) selecting appropriate extraction solvents to extracted various phthalate esters according to the different matrixes; (3) pouring the extracted phthalate ester solutions into an extraction tube; and (4) after completely mixing, purifying the filler, removing interferents, centrifugating for 5 min at a speed of 4000 r / min, taking the supernatant, and analyzing. With the matrix dispersion purification tube, the phthalate esters in various matrixes can be rapidly and cheaply purified, characteristics of economy, environmental protection and stability are provided, GPC instrument purification is not required, and analysis accuracy and no damage on the instrument are ensured.

Description

Technical field: [0001] The invention relates to the development of a pretreatment purification tube for detecting various phthalate esters in different matrices, in particular to a matrix dispersion purification tube for detecting phthalate esters. Background technique: [0002] Phthalates are chemical products that are widely used in the plastics industry, packaging materials, pharmaceutical auxiliary materials and other industries. At the same time, phthalates are environmental hormones. If they exceed a certain level in food and drinking water, Concentrations will affect the fertility of men and the development of women, so the European Union has long introduced limits for phthalates in food, drinking water, and toys for infants and young children. [0003] China issued GB / T 21911-2008-Method for the determination of phthalates in foods in 2008, especially for the detection of phthalates in oily substances, the pre-treatment method uses GPC to remove oil However, the GPC instr...

Claims

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Application Information

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IPC IPC(8): G01N1/38
Inventor 吴刚强维严晨斌江晨舟
Owner SHANGHAI ANPEL SCI INSTR
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