Method for processing onion sample containing several pesticide residues before determination
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A treatment method and sample technology, applied in the field of determination of organophosphorus and pyrethroid pesticide residues, can solve the problems of acute poisoning, achieve the effects of low matrix interference, high stability and reliability, and simple treatment process
Inactive Publication Date: 2011-07-13
CENT LAB TIANJIN ACADEMY OF AGRI SCI
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However, vegetable farmers in some areas still use highly toxic and highly toxic pesticides such as methamidophos and methyl par
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Embodiment 1
[0035] (1) Microwave treatment: Peel the onion layer by layer and cut into 4cm 2 The slices were placed in a 650W microwave oven for 20s at high heat, crushed and mixed to prepare a uniform sample;
[0036] (2) Weigh 10g sample, add 15mL acetonitrile and 20mL distilled water, shake and extract for 30min, then filter;
[0037] (3) Wash the residue with 20 mL of acetonitrile, add 8 g of sodium chloride after filtering the washing liquid, shake for 1 min, let stand to separate layers, and dry with anhydrous sodium sulfate;
[0038] (4) Wash anhydrous sodium sulfate with acetonitrile, combine the acetonitrile phases, concentrate to dryness under reduced pressure, add 2 mL of acetone / n-hexane with a volume ratio of 1 / 1, vortex for 10 s, transfer to a sample injection vial for determination by GC-MS. Wherein the recovery rate: 109.9%, the relative standard deviation is 1.49%.
Embodiment 2
[0040] Microwave processing: Peel the onion layer by layer and cut into about 6cm 2 The slices were placed in a microwave oven at 650W (medium heat) for 40s, crushed and mixed to prepare a uniform sample.
[0041] Weigh 10g sample, add 30mL acetonitrile and 10mL distilled water, shake and extract for 30min, then filter into a 500mL separatory funnel, wash the residue with 20mL acetonitrile, and filter the washing liquid into a separatory funnel. Add 8 g of sodium chloride, shake for 1 min, let stand to separate layers, discard the lower aqueous phase, take the upper organic phase per anhydrous sodium sulfate, wash anhydrous sodium sulfate with 20 mL of acetonitrile for several times, combine the acetonitrile phases, and concentrate to dryness under reduced pressure , add 2mL of acetone / n-hexane (V / V, 1 / 1), vortex for 10s, transfer to the injection vial for testing.
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Abstract
The invention discloses a method for processing an onion sample containing organophosphorus and synthetic pyrethroid pesticide residues before determination, comprising the following steps: processing the onion in a microwave oven for 40 seconds; stirring, mixing and obtaining an even sample; then adding 30ml of acetonitrile and 10ml of distilled water; after oscillating and extracting for 30 minutes, filtering into a separating funnel of which the volume is 500ml; washing residues by 20ml of acetonitrile; filtering a washing liquid into the separating funnel; adding 8g of sodium chloride; oscillating for 1 minute; standing and layering; abandoning a lower-layer aqueous phase; taking an upper-layer organic phase, and processing the upper-layer organic phase by anhydrous sodium sulfate; washing the anhydrous sodium sulfate for several times by 20ml of acetonitrile; combining the acetonitrile phases; reducing pressure and concentrating to be dry; adding 2ml of acetone/ normal hexane (V/V, 1/1); eddying for 10 seconds; transferring to a sample introduction flasket; and determining by a gas chromatography and mass spectrometry. With the method for processing an onion sample before determination in the invention, impurity interference can be greatly lowered, and the method has high sensitivity.
Description
Technical field: [0001] The invention belongs to the technical field of measuring pesticide residues, and relates to a method for measuring residues of organophosphorus and pyrethroid pesticides. In particular, the invention relates to a method for treating onion samples containing organophosphorus and pyrethroid pesticides before determination. Background technique: [0002] Pesticide residues refer to the phenomenon that a part of pesticides directly or indirectly remain in grains, vegetables, fruits, livestock products, aquatic products, soil and water after pesticides are applied in agricultural production. The problem of pesticide residues arises with the mass production and widespread use of pesticides. Some of the currently used pesticides can be biodegraded into harmless substances in a relatively short period of time, while some organochlorine pesticides are difficult to degrade and are pesticides with strong residues. Vegetable pesticide residues exceeding the st...
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