Determination method for organophosphorus in scallion, garlic and products thereof

A method for determination, organophosphorus technology, applied in the field of determination of pesticide residues in food, can solve the problems of unsatisfactory sensitivity and selectivity of single-stage mass spectrometry, cumbersome processing process of liquid chromatography-mass spectrometry, and difficult removal, etc., to achieve high sensitivity , good reproducibility, no effect of matrix interference

Inactive Publication Date: 2015-12-02
RIZHAO ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have certain limitations in the detection of special matrices, such as spicy samples such as onions, which will release sulfides during the chopping process and produce special odors [8-10] , these sulfides are similar to the organophosphorus in the detection, and are not easy to remove, and it is easy to cause false positives when detected by the FPD detector
However, the sensitivity and selectivity of single-stage mass spectrometry are not ideal, and the pretreatment process of liquid chromatography-mass spectrometry is cumbersome, costly, and polluted
A gas chromatography / tandem triple quadrupole mass spectrometry method capable of simultaneously detecting five organophosphorus residues in onions, garlic, and their products has not yet been developed. See the report

Method used

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  • Determination method for organophosphorus in scallion, garlic and products thereof
  • Determination method for organophosphorus in scallion, garlic and products thereof
  • Determination method for organophosphorus in scallion, garlic and products thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1.1 Instruments and reagents

[0057] Agilent7000B gas chromatography / tandem triple quadrupole mass spectrometer (GC-MS / MS); homogenizer; 1.0mL syringe; 50mL centrifuge tube; nitrogen blowing apparatus; 150mL conical flask; 50mL nitrogen blowing tube.

[0058] Detect fresh onion samples, fresh onions, fresh garlic samples, garlic sprouts samples, frozen onion products, frozen boiled onion slice products, frozen garlic sprouts, dehydrated onion samples, and dehydrated garlic slices that do not contain the above-mentioned organophosphorus pesticide residues.

[0059] PSA (ethylenediamine-N-propylsilane); aminopropyl powder; NaCl; ceramic homogeneous.

[0060] Acetonitrile: chromatographically pure; acetone: chromatographically pure; n-hexane: chromatographically pure; ethyl acetate: chromatographically pure; phorate: certified reference material; methamidophos: certified reference material; Fenthion: certified reference material; parathion: certified reference material; ...

Embodiment 2

[0095] 1.1 Extraction and purification

[0096] Weigh 20.04g (accurate to 0.01g) of frozen onion products, add 1.0ug / mL methamidophos or other organic phosphorus standard solution 200uL, place in a 100mL centrifuge tube, add 40.0mL acetonitrile:ethyl acetate (1+1) accurately To the solution, add 0.2g PSA, 0.2g aminopropyl powder, 5gNaCl and ceramic homogenate, vortex for 3min and then centrifuge at 10000r / min for 3min. After the organic phase and the aqueous phase are separated, accurately pipette 20mL of the organic phase into a 50mL nitrogen blowpipe, blow it in a 45°C water bath with nitrogen until it is nearly dry, and accurately add 1.0mL of acetone + n-hexane (30+70, v / v) to dissolve the residue. Through the 0.22um filter membrane on the machine to measure.

[0097] 1.2 Chromatographic conditions

[0098] GC / MS / MS: Chromatographic column: HP-5MS (30m×0.25mmi.d., 0.25μm) elastic quartz capillary column; carrier gas: high-purity helium (99.999%); collision gas: high-purity...

Embodiment 3

[0101] 1.1 Extraction and purification

[0102] Weigh 20.02g (accurate to 0.01g) fresh onion sample, add 200uL of organic phosphorus standard solution such as 1.0ug / mL methamidophos, put it in a 100mL centrifuge tube, add 40.0mL acetonitrile: ethyl acetate (1+1) accurately The solution was stored at -18°C for 30 minutes. After taking it out, add 0.2g PSA, 0.2g aminopropyl powder, 5gNaCl and ceramic homogenate, vortex for 3min and then centrifuge at 10000r / min for 3min. After the organic phase and the aqueous phase are separated, accurately pipette 20mL of the organic phase into a 50mL nitrogen blowpipe, blow it in a 45°C water bath with nitrogen until it is nearly dry, and accurately add 1.0mL of acetone + n-hexane (30+70, v / v) to dissolve the residue. Through the 0.22um filter membrane on the machine to measure.

[0103] 1.2 Chromatographic conditions

[0104] GC / MS / MS: Chromatographic column: HP-5MS (30m×0.25mmi.d., 0.25μm) elastic quartz capillary column; carrier gas: hi...

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Abstract

The invention provides a determination method for organophosphorus in scallion, garlic and products thereof. The method comprises the following steps: weighing scallion, garlic and products thereof, placing the weighed scallion, garlic and products thereof into a centrifuge tube, adding an acetonitrile-ethyl acetate solution or acetone-ethyl acetate solution in a volume ratio of 1: 1; then adding PSA, aminopropyl powder, NaCl and ceramic homogenization proton and carrying out centrifugation; after layering of an organic phase and a water phase, accurately transferring the organic phase into a nitrogen blowpipe, adding acetone + hexane (30 + 70, v/v) to dissolve residue after the organic phase is almost dried under blowing of nitrogen, carrying out filtering with a filter membrane and then carrying out determination on an instrument; and carrying out detection, wherein gas chromatography/triple-quadrupole tandem mass spectrography is used for determining methamidophos, thimet, monocrotophos, baytex and parathion in purified liquid obtained in the previous step. The method is simple to operate and almost free of interference by matrix, has high sensitivity, good repeatability and qualitative and quantitative accuracy and can be extensively applied to detection of residual of methamidophos, thimet, monocrotophos, baytex and parathion in scallion, garlic and products thereof.

Description

technical field [0001] The invention relates to a method for determining pesticide residues in food, in particular to a method for determining methamidophos, phorate, monocrotophos, fenthion and parathion in onions, garlic and their products. Background technique [0002] Methamidophos, phorate, monocrotophos, fenthion, and parathion are broad-spectrum insecticides and acaricides, widely used in vegetables and fruits, and the use of such pesticides is large [1] . However, these drug residues pass through the food chain and accumulate in the human body to cause teratogenic, carcinogenic and mutagenic [2] . Poisoning incidents of organophosphorus pesticides such as phorate occur from time to time. Therefore, it is necessary to strictly control the amount of organophosphorus pesticides used on vegetables, fruits and other crops [3] . my country's requirements for such pesticide residues in domestic and imported and exported vegetables and fruits are that they must not be de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 高尧华刘冰宋卫得孙灿李林杰王凯
Owner RIZHAO ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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