GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) testing method of residual quantity of cyantraniliprole
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A GC-NCI-MS and cyantraniliprole technology, which is applied in the field of GC-NCI-MS determination of cyantraniliprole residues, can solve the problems of low sensitivity of anti-interference ability, achieve matrix interference avoidance, good repeatability, and easy operation easy effect
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Problems solved by technology
Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometers (GC-MS), and are generally equipped with negative chemical ion sources (NCI). Now many types of pesticides contain electronegative groups, organochlorines and pseudo Pyrethrin pesticide molecules mostly contain strong electronegative groups such as -F, -Cl, -Br or -COO-; organophosphorus pesticide molecules mostly contain =S, -OR, -P, -O-, -Cl, or -P=O and other electronegative groups; and most of the new pesticides developed in recent years contain -F groups. Therefore, the use of GC-NCI-MS can facilitate the multi-residue analysis of various pesticides. Compared with MS, it can obtain better anti-interference ability, lower sensitivity and better selectivity. Cytraniliprole is an electronegative compound, but so far no GC- According to the report of the NCI-MS detection method, 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, the establishment of gas chromatography-negative chemistry Ion source-mass spectrometry (GC-NCI-MS) is of great significance for the qualitative and quantitative analysis of cyantraniliprole residues in grains and animal-derived foods
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Embodiment 1
[0036] Example 1: Detection of cyantraniliprole residues in beef
[0037] (1) Sample pretreatment
[0038] extract
[0039] Weigh 5g of beef sample that has been thoroughly mixed into a 50mL centrifuge tube, add 5mL of water to mix, let 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.
[0040] purify
[0041] 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 el...
Embodiment 2
[0067] Example 2: Detection of cyantraniliprole residues in wheat
[0068] (1) Sample pretreatment
[0069] extract
[0070] 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.
[0071] purify
[0072] 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...
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Abstract
The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) testing method of residual quantity of cyantraniliprole. The method is mainly used for testing the content of cyantraniliprole remained in complex matrix food agricultural products such as cereal grains and animal-origin food. The method comprises the following steps: homogenously extracting cyantraniliprole remained in samples by using acetonitrile or acetonitrile solutions containing 1 percent of acetic acid; purifying and condensing by using a C18 / PSA solid-phase extraction column; detecting by GC-NCI-MS; building a corrected standard curve by using vehicle solutions which do not contain pesticides to be detected; and quantifying by using an external standard method. The method has the average recycling rate of 93.4-97.7 percent, the average relative standard deviation (RSD) of 4.0-7.3 percent and the detection limit of lower than 2.89 microgram / kg, has the advantages of convenience and quickness in operation, good impurity removal effect, high sensitivity, high property, high repeatability and accurate quantitativeness and qualitativeness, and can meet the technical requirement of uniform limit, namely 0.01 mg / kg maximum residue limit of corresponding food security detection, in America, Canada, European Union, Japan and the like, so that powerful technical support is provided for guaranteeing food security of people and healthy development of export trade in China.
Description
technical field [0001] The present invention relates to a kind of GC-NCI-MS determination method of residual amount of cyantraniliprole, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) qualitative and quantitative determination grain, pork, beef The invention discloses a method for residual cyantraniliprole content in animal and plant-derived foods with complex matrices such as animal muscles and products such as mutton and chicken, and belongs to the technical field of determination of pesticide residues. Background technique [0002] Cyantraniliprole, also known as cyantraniliprole (cyantraniliprole), is a second-generation ryanodine receptor inhibitor insecticide successfully developed by DuPont after chlorantraniliprole. Formed from various polar groups on the benzene ring, compared with chlorantraniliprole, it has a wider spectrum of insecticidal activity, excellent control effect on piercing-sucking pests, and has b...
Claims
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