Method applicable to simultaneous and rapid determination of organic phosphate fire retardants (OPFRs) in different food sample matrixes

A detection method and food technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of no OPFRs application research report, etc., and achieve the effects of high selectivity and sensitivity, shortened analysis time, and fast analysis speed.

Active Publication Date: 2017-10-27
RES INST OF ZHEJIANG UNIV TAIZHOU
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method applicable to simultaneous and rapid determination of organic phosphate fire retardants (OPFRs) in different food sample matrixes
  • Method applicable to simultaneous and rapid determination of organic phosphate fire retardants (OPFRs) in different food sample matrixes
  • Method applicable to simultaneous and rapid determination of organic phosphate fire retardants (OPFRs) in different food sample matrixes

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Experimental program
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Embodiment 1

[0067] This embodiment focuses on the matrix effect of the analytical method, the recovery rate of standard addition and the production of a standard working curve.

[0068] Step (1): Mixed sample processing

[0069] Take the same amount of fish, chicken, pork, vegetables, and milk, each 10 g, mix and homogenize fully;

[0070] Step (2): Extract

[0071] Accurately weigh 1.0 g of the homogenate into 10 ml stoppered glass centrifuge tubes, numbered A1-A7, B1-B7 respectively, and add 50 μL of different concentrations (1, 5, 10, 50, 100, 500, 1000 ng ml -1 ) standard substance mixed solution and 20 μL internal standard mixed solution (1000 ng·ml -1 ), A1-A7 and B1-B7 were added with 4 ml 0.5% formic acid-acetonitrile, vortexed for 1 min, and ultrasonically extracted for 10-15 min. Take another 10 ml centrifuge tube, numbered C1-C7, add 4 ml of acetonitrile containing 0.5% formic acid, vortex mix for 1 min, and ultrasonically extract for 10-15 min.

[0072] Step (3): Purifica...

Embodiment 2

[0092] This example is the application of the present invention to the detection of OPFRs in chicken meat.

[0093] Step (1): Chicken sample processing

[0094] Take 5 g of washed chicken breast, and fully homogenize;

[0095] Step (2): Extract

[0096] Accurately weigh 1.0 g of chicken homogenate in 3 parts, respectively, into 10 ml stoppered glass centrifuge tubes, and add 20 μL of internal standard mixed solution (1000 ng·ml -1 ), add 4 ml of 0.5% formic acid-acetonitrile, vortex mix for 1 min, and ultrasonically extract for 10-15 min.

[0097] Step (3): Purification

[0098] Add 300mg anhydrous NaCl and 300mg anhydrous MgSO to parallel samples 4 , vortexed for 1 min. at 3000 rpm -1 Centrifuge for 5 min, and transfer the supernatant to a corresponding new centrifuge tube. After rinsing the original centrifuge tube with 2 ml of 0.5% formic acid-acetonitrile, centrifuge again to get the supernatant, and combine the two supernatants. Add 40 mg PSA, 40 mg C18, 200 mg an...

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Abstract

The invention relates to a method applicable to simultaneous and rapid determination of organic phosphate fire retardants (OPFRs) in different food sample matrixes. The method is characterized in that residues of the OPFRs in the foods are extracted and purified by an improved QuEChERS method, the matrix interference of a target compound is effectively eliminated, and the matrix effect is 92.3%-116.1% (except triphenylmethyl phosphate is 65.9%). the method has the advantages that the selectivity and the stability are good, the average recovery rate is 78.6%-127.3%, and the relative standard deviation is 3.1%-9.7%; an ultra-high performance liquid chromatography-tandem quadrupole mass spectrometer (UPLC-MS/MS) is adopted for qualitative and quantitative detection, the sensitivity is good and the quantification limit is 0.05-0.42ng.g-1; and synchronous and rapid detection of multiple residues of trace OPFRs in complex matrixes of different food sample types is realized and the technical defects in the current field are made up.

Description

technical field [0001] The invention belongs to the field of analysis and detection of organic phosphate flame retardants, and relates to a simultaneous rapid determination method for multiple organic phosphate flame retardants applicable to different food matrices. Background technique [0002] Organophosphate flame retardants (Organophosphate flame retardants, OPFRs) have good flame retardant properties, and have multiple functions such as plasticization and lubrication, and are widely used. With the continuous expansion of the global flame retardant market and the restricted use of halogenated flame retardants (such as polybrominated diphenyl ethers, etc.) The output showed a rapid growth trend. my country is a big producer of OPFRs, with an annual production capacity of more than 100,000 tons, and the usage is also growing rapidly. The vast majority of OPFRs are used in different materials (furniture, building materials, textiles, and electronic products, etc.) in the ...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 丁锦建邓童庆王燕飞丁佳敏杨方星
Owner RES INST OF ZHEJIANG UNIV TAIZHOU
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