GC-MS/MS (gas chromatography-tandem mass spectrometry) determining method of penthiopyrad residual quantity
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A technology for penthiopyrad and a determination method, which is applied in the field of GC-MS/MS determination of penthiopyrad residues, can solve the problems of high price, relatively long system consumption, etc., achieves easy operation, avoids matrix interference, repeats good effect
Inactive Publication Date: 2016-05-04
郭庆龙
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[0006] At this stage, there are few studies on the determination methods of penthiopyram residues, and the detection methods reported are mainly the detection methods of penthiopyram residues in vegetables and fruits. These detection methods all use liquid chromatography tandem mass spectrometry (LC-MS / MS) is a detection method for the determination of penthiopyram residues in vegetables and fruits. 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 and enterprises Or the scientific research institute has not configured this instrument or the number of equipment is small. Since 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. The time to balance the system restricts the application of LC-MS / MS to some extent
The use of gas chromatography-tandem mass spectrometry (GC-MS / MS) to analyze pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, high sensitivity, and strong selectivity. It can achieve multi-residue analysis of hundreds of pesticides, but so far no food and agricultural products In the report of the GC-MS / MS detection method of penthiopyram residues, due to the complex matrix of food and agricultural products such as grains and animal-derived foods, it is necessary to establish a sample pretreatment method and instrument analysis conditions with good purification effects to meet the detection requirements. Therefore, it is of great significance to establish a gas chromatography-tandem mass spectrometry (GC-MS / MS) detection method for the qualitative and quantitative analysis of penthiopyrad residues in grains and animal-derived foods
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Embodiment 1
[0035] Example 1: Detection of Penthiopyrad Residues in Wheat
[0036] (1) Sample pretreatment
[0037] extract
[0038]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 8 mL of acetonitrile extract and rotate it at 40 °C or blow it with nitrogen until it is nearly dry, add 1 mL of acetonitrile and vortex it, and wait for purification.
[0039] purify
[0040] 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 tran...
Embodiment 2
[0068] Example 2: Detection of Penthiopyrad Residues in Pork
[0069] (1) Sample pretreatment
[0070] extract
[0071] 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.
[0072] purify
[0073] 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, receive all the ...
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Abstract
The invention discloses a GC-MS/MS (gas chromatography-tandem mass spectrometry) determining method of penthiopyrad residual quantity. The method is a method mainly used for determining the residual penthiopyrad content in agricultural products of complicated matrix food such as cereal grains and animal derived food. Acetonitrile or an acetonitrile solution containing one-percent acetic acid is used for performing homogeneous extraction of the residual penthiopyrad in samples; after C<18>/PSA (primary secondary amine) solid phase extraction column purification and concentration, GC-MS/MS detection is performed; a corrected standard work curve is built by using a blank matrix solution not containing pesticide to be detected; an external reference method is used for quantification. The GC-MS/MS determining method has the advantages that the average recovery rate is 86.4 percent to 95.3 percent; the average RSD (relative standard deviation) is 5.0 percent to 8.7 percent; the detection limit is lower than 0.25mug/kg; the operation is simple, convenient and fast; the impurity removal effect is good; the sensitivity is high; the characteristic performance is high; the repeatability is good; the qualitative and quantitative analysis is accurate. The technical requirements of countries such as America, European Union and Japan on corresponding product safety detection can be met; powerful technical support is provided for guaranteeing the food safety of Chinese people and healthy development of export abroad trade.
Description
technical field [0001] The present invention relates to a kind of GC-MS / MS determination method of penthiopyram residual amount, more specifically adopts gas chromatography tandem mass spectrometry (GC-MS / MS) to qualitatively and quantitatively measure grain, pork, beef, mutton, chicken The invention discloses a method for residual penthiopyram content in animal and plant-derived foods with complex matrices such as animal muscles and products, and belongs to the technical field of determination of pesticide residues. Background technique [0002] Penthiopyrad (Penthiopyrad) is a novel amide fungicide developed by Mitsui Chemicals, Japan. Its English common name is penthiopyrad, its test code is MTF-753, and its trade name is Afetofluapro. CAS registration number: 183675-82-3, chemical name is (RS)-N-[2-(1,3-dimethylbutyl)-3-thienyl]-methyl-3-(trifluoromethyl )-1H-pyrazole-4-carboxamide, the chemical structural formula is: [0003] [0004] Penthiopyrad has a different b...
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