GC-NCI-MS determination method for determining residual amount of chlorantraniliprole
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A GC-NCI-MS, chlorantraniliprole technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity and anti-interference ability, and achieve the advantages of avoiding matrix interference, good repeatability and easy operation. Effect
Active Publication Date: 2015-04-08
SHENZHEN SINO ASSESSMENT GRP
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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-interfer
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Embodiment 1
[0037] Example 1: Detection of Chlorantraniliprole Residues in Wheat
[0038] (1) Sample pretreatment
[0039] extract
[0040] Weigh 5g of wheat 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.
[0041] purify
[0042] 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 colum...
Embodiment 2
[0069] Example 2: Detection of Chlorantraniliprole Residues in Pork
[0070] (1) Sample pretreatment
[0071] extract
[0072] 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.
[0073] purify
[0074] 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, an...
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Abstract
The invention discloses a GC-NCI-MS determination method for determining residual amount of chlorantraniliprole, which is mainly used for determining content of residual chlorantraniliprole in complex matrix food agricultural products such as cereal grains and animal derived foods. The GC-NCI-MS determination method comprises the following steps: extracting the residual chlorantraniliprole in a sample by adopting acetonitrile or acetonitrile solution containing 1% of acetic acid in a homogenizing manner; purifying and concentrating by adopting a C18/PSA solid phase extraction column, performing gas chromatography-negative chemical ionization-mass spectrum (GC-NCI-MS) detection, establishing a correcting standard curve by adopting a blank matrix solution which does not contain pesticides, and quantifying by adopting an external standard method. With the adoption of the GC-NCI-MS determination method, the average recovery rate is 86.8%-96.9%, the average relative standard deviation (RSD) is 4.0-9.7%, the detection limit is 1.41 microg/kg; the GC-NCI-MS determination method has the advantages of simplicity and convenience in operation, rapidness, good impurity removal effect, high sensitivity, strong characteristic feather, good repeatability, and accuracy in qualitative and quantitative effect; the 0.01mg/kg residual limit for corresponding food safety detection by countries including America, Japan, European Union and Canada, namely, the technical requirement of uniform limit, is met, and therefore, powerful technical support is provided for guaranteeing food safety of Chinese people and healthy development of export trade.
Description
technical field [0001] The present invention relates to a kind of GC-NCI-MS determination method of residual amount of chlorantraniliprole, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure grain, pork The invention discloses a method for residual chlorantraniliprole content in animal and plant-derived foods with complex matrices such as animal muscle and products such as beef, mutton, chicken, etc., and belongs to the technical field of determination of pesticide residues. Background technique [0002] Chlorantraniliprole (Chlorantraniliprole), trade name Kang Kuan, is a new type of o-formamidobenzamide insecticide developed by DuPont. Mothidae, Fruit Mothidae, Leaf Rolleridae, Melydidae, Plutella Plutella, Graciidae, Thymothidae, etc. all have very good control effects, and can also control Coleoptera Weevilidae and Chromophyidae; Muscidae; Bemisia tabaci and other non-Lepidopt...
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