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A method suitable for detecting the content of organophosphate flame retardants in various foods
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A detection method and food technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of no OPFRs application research reports, achieve high selectivity and sensitivity, shorten analysis time, and fast analysis speed
Active Publication Date: 2019-12-24
RES INST OF ZHEJIANG UNIV TAIZHOU
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Problems solved by technology
However, there are still no reports on the application of this method to OPFRs in food samples.
Method used
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Embodiment 1
[0068] 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.
[0070] Take the same amount of fish, chicken, pork, vegetables, and milk, each 10g, mix and homogenize fully;
[0071] Step (2): Extract
[0072] 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 20μL internal standardmixed solution (1000ng·ml -1 ), A1-A7 and B1-B7 were added with 4ml of 0.5% formic acid-acetonitrile, vortexed for 1min, and ultrasonically extracted for 10-15min. Take another 10ml centrifuge tube, numbered C1-C7, add 4ml of acetonitrile containing 0.5% formic acid, vortex mix for 1min, and ultrasonically extract for 10-15min.
[0073] Step (3): Purification ...
Embodiment 2
[0093] This example is the application of the present invention to the detection of OPFRs in chicken meat.
[0095] Take 5g of washed chicken breast, and fully homogenize;
[0096] Step (2): Extract
[0097] 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 standardmixed solution (1000 ng·ml -1 ), add 4ml of 0.5% formic acid-acetonitrile, vortex mix for 1min, and ultrasonically extract for 10-15min.
[0098] Step (3): Purification
[0099] Add 300mg anhydrous NaCl and 300mg anhydrous MgSO to parallel samples 4 , vortexed for 1 min. At 3000r·min -1 Centrifuge for 5 minutes, and transfer the supernatant to a corresponding new centrifuge tube. After the original centrifuge tube was rinsed with 2 ml of 0.5% formic acid-acetonitrile, it was centrifuged again to obtain the supernatant, and the two supernatants were combined. Add 40mg PSA, ...
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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 quadrupolemassspectrometer (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 phosphateflame retardants, and relates to a simultaneous rapid determination method for multiple organic phosphate flame retardants applicable to different food matrices. Background technique [0002] Organophosphateflame 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.) due to environmental safety and other reasons, OPFRs, as an excellent substitute, its social needs and 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 ...
Claims
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