GC-EI-MS measurement method for cyenopyrafen residual amount
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A GC-EI-MS and pyrazafen technology, which is applied in the field of GC-EI-MS determination of pyraclofen residue, can solve the problems of complexity, high price, and restrictions on the application of LC-MS/MS, and achieve Easy to operate, high sensitivity, and the effect of avoiding matrix interference
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Problems solved by technology
[0006] So far, only one patent "a method for the determination of pyrimidin residues" has been retrieved, which establishes a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of pyrimidin in vegetables, fruits and tea. The detection method of ester residues, the use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of fast, simple, and high sensitivity. However, due to its high price, many testing institutions, enterprises or research institutes have not equipped this instrument or configuration The number of units is small, because when different compounds are detected by LC-MS / MS, different mobile phases or chromatographic columns need to be used, which requires constant replacement of chromatographic columns and mobile phases and takes a long time to balance the system. Restricts the application of LC-MS / MS
Gas chromatography-mass spectrometry (GC-EI-MS) equipped with electron bombardment ionization source has great advantages in analyzing pesticide residues in food and agricultural products. Since electron bombardment ionization source mass spectrometry is a universal detector, it can realize multi-residue analysis of hundreds of pesticides. It can be qualitative and quantitative at the same time, and the price is moderate. Therefore, various testing institutions and enterprises are equipped with gas chromatography-electron bombardment ion source-mass spectrometer (GC-EI-MS) to detect pesticide residues in food and agricultural products, but so far no See the report on the GC-EI-MS detection method of pyrazafen residues in food and agricultural products. Due to the complex matrix of food and agricultural products such as grains and animal-derived foods, a sample pretreatment method with good purification effect must be established to meet the detection requirements. Therefore, it is of great significance to establish a gas chromatography-mass spectrometry (GC-EI-MS) detection method for the qualitative and quantitative analysis of pyrazafen residues in grains and animal-derived foods
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Embodiment 1
[0034] Embodiment 1: detection of the residual amount of pyrifenin in pork
[0035] (1) Sample pretreatment
[0036] extract
[0037]Weigh 5g of fully mixed pork sample into a 50mL centrifuge tube, add 5mL of water to mix, let stand for 30min, accurately add 20mL of acetonitrile, extract homogeneously for 2min, add 3g of anhydrous magnesium sulfate and 2g of sodium chloride, and vortex for 1min , 7000r / min centrifugal 5min. After centrifugation, take 8 mL of the acetonitrile extract at 40°C for rotary steaming or nitrogen blowing to about 1 mL for purification.
[0038] purify
[0039] Pre-wash C with 5 mL of acetonitrile 18 / PSA solid phase extraction column, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetonitrile, and transfer the washing liquid into the SPE column, when the solution reaches the top of the adsorbent, add Add 4mL of acetonitrile to the column for elution, all...
Embodiment 2
[0064] Embodiment 2: the detection of pyrazafen residue in wheat
[0065] (1) Sample pretreatment
[0066] extract
[0067] Weigh 5g of wheat sample (ground into flour) that has been thoroughly mixed into a 50mL centrifuge tube, add 20mL of water to resuscitate for 30min, then accurately add 20mL of acetonitrile solution containing 1% acetic acid, shake and extract for 20min, ultrasonically extract for 5min, add 3g of anhydrous Magnesium sulfate and 2g sodium acetate, after vortexing for 1min, centrifuge at 7000r / min for 5min. After centrifugation, take 8mL of the extract solution at 40°C by rotary steaming or blowing with nitrogen until it is nearly dry, add 1mL of acetonitrile and vortex, and wait for purification.
[0068] purify
[0069] Pre-wash C with 5 mL of acetonitrile 18 / PSA solid phase extraction column, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetonitrile, and t...
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Abstract
The invention discloses a GC-EI-MS (gas chromatograph-electron ionization-mass spectrometry) measurement method for a cyenopyrafen residual amount. The method is mainly used for measuring the content of cyenopyrafen retained in complicated matrix food agricultural products such as grains and animal derived food. The method comprises the steps of extracting the cyenopyrafen retained in a sample by homogenizing acetonitrile or an acetonitrile solution with 1 percent of acetic acid, performing purification and concentration by a C18/PSA solid-phase extraction column, performing GC-EI-ES detection, building a corrected standard curve for a blank matrix solution without pesticide to be detected, and carrying out quantification by an external standard method. According to the method, the average recycling rate is 81.9-89.0 percent, the average relative standard deviation (RSD) is 4.7-6.5 percent, and the detection limit is lower than 0.73 [mu]g/kg; the method has the advantages of simplicity and convenience in operation, quickness, good impurity removal effect, high sensitivity, high repetitiveness and accuracy in qualification and quantification. The technical requirement of 'uniform limit' on the 0.01 mg/kg residue limit of corresponding food safety detection of the countries such as Japan, European Union and Korea can be met.
Description
technical field [0001] The present invention relates to a kind of GC-EI-MS determination method of the residual amount of pyraclofen, more specifically, it adopts gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively measure grain, pork, The invention relates to a method for the content of pyrifenin residues in animal and plant-derived foods with complex matrices such as beef, mutton, chicken and other animal muscles and products, and belongs to the technical field of determination of pesticide residues. Background technique [0002] Cyenopyrafen (Cyenopyrafen) is a new type of pyrazole acaricide developed by Nissan Chemical Company in 2009. It is mainly used to control harmful mites such as red spider mites on fruit trees, vegetables and green peppers. The chemical name is (E)-2- (4-tert-butylphenyl)-2-cyano-1-(1,3,4-trimethylpyrazol-5-yl)enyl 2,2-dimethylpropionate, English Chemistry The name is (E)-2-(4-tert-b...
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