GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of fluoride ether bacterium amide
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A technology of GC-NCI-MS and fluoxybactam, which is applied in the field of GC-NCI-MS determination of fluoxibactil residues, achieves high sensitivity, easy operation, and the effect of ensuring people's food safety
Active Publication Date: 2015-05-27
广东唯诺冠动漫食品股份有限公司
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[0006] So far, there have been no domestic and foreign reports on the detection method of fluoxetin residues in food and agricultural products. Gas chromatography-mass spectrometry (GC-NCI-MS) equipped with a negative chemical ionization source has great advantages in the analysis of pesticide residues in food and agricultural products. Negative chemical ion source (NCI source) is called the "soft ionization source" of mass spectrometry. It has high selectivity and high sensitivity for analytes containing electronegative groups. Due to its strong characteristics, matrix interference Rarely, the qualitative and quantitative analysis of the target can be carried out very accurately
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Embodiment 1
[0035] Example 1: Detection of Fluorysin Residues in Rice
[0036] (1) Sample pretreatment
[0037] extract
[0038] Weigh 5g of rice sample that has been thoroughly mixed into a 50mL centrifuge tube, add 5mL of water to mix, let it stand for 30min, add 20mL of acetonitrile accurately, 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.
[0039] purify
[0040] Pre-wash C with 5 mL of acetonitrile18 / 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,...
Embodiment 2
[0065] Example 2: Detection of fluoxetin residues in pork
[0066] (1) Sample pretreatment
[0067] extract
[0068] Weigh 5g of pork 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.
[0069] purify
[0070] 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...
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Abstract
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of fluoride ether bacterium amide. The method is mainly used for determining the residual amount of fluoride ether bacterium amide in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual fluoride ether bacterium amide in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-NCI-MS detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 85.0%-91.1%, the average relative standard deviation (RSD) is 4.1%-6.6%, the detection limit is lower than 0.35mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.
Description
technical field [0001] The invention relates to a GC-NCI-MS method for determining the residual amount of fluoxyrhizobactin, more specifically, it uses gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure grains, pork, The invention relates to a method for the content of fluoxetin 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] Fluorobactylamide (LH-2010A) is a new type of fluorine-containing benzamide fungicide innovatively synthesized by Shandong United Pesticide Industry Co., Ltd. in 2010. The chemical name is: N-(3-chloro-5-(tri Fluoromethyl)pyridine-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide, the structural formula is: [0003] [0004] The structural formula of fluoxetin contains 7 fluorine atoms. The C...
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