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Method for detecting pesticide residues in rice and rice stems

A technology for pesticide residues and detection methods, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as difficult simultaneous quantitative detection of rice

Inactive Publication Date: 2019-08-20
SHANGHAI ACAD OF AGRI SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The technical problem to be solved by the present invention is to overcome the difficulty in simultaneously quantitatively detecting propamocarb, chlorantraniliprole, thiabendazole, oxadiazone, pyraclostrobin, and cyhalofop in rice and rice stems in the prior art and emamectin and other 7 kinds of pesticide residue defects, and provide a detection method for pesticide residues in rice and rice stems

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  • Method for detecting pesticide residues in rice and rice stems
  • Method for detecting pesticide residues in rice and rice stems
  • Method for detecting pesticide residues in rice and rice stems

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0113] Embodiment 1 methodological verification

[0114] 1 Materials and methods

[0115] 1.1 Materials and reagents

[0116] Rice samples were collected from the suburbs of Shanghai;

[0117] Pesticide standard samples were purchased from Shanghai Anpu Experimental Technology Co., Ltd., and the prepared concentration was 1000mg / L standard solution;

[0118] GCB adsorbent (graphitized carbon black) and PSA adsorbent (ethylenediamine-N-propylsilane) were purchased from Shanghai Anpu Experiment Technology Co., Ltd.;

[0119] Sodium chloride, anhydrous magnesium sulfate, sodium citrate and disodium citrate, analytically pure, purchased from Shanghai Anpu Experiment Technology Co., Ltd.;

[0120] Acetonitrile, methanol, formic acid, chromatographically pure, purchased from Tedia, USA;

[0121] Polytetrafluoroethylene (PTFE) (hydrophilic / hydrophobic) and 0.22 μm nylon filter membrane were purchased from Shanghai Anpu Experimental Technology Co., Ltd.;

[0122] Ultrapure water ...

Embodiment 2

[0183] By using QuEChERS-UPLC-MS / MS to detect 10 rice samples purchased from the market (purchased from the Shanghai Agricultural Products Central Wholesale Market), the results showed that the three pesticides acetamiprid, azoxystrobin and indoxacarb had samples detected respectively. Among them, the detected concentration of acetamiprid was 1.33 μg·kg -1 , the detection concentration of 1 sample of azoxystrobin was 1.10 μg·kg -1 , the detected concentrations of the two samples of indoxacarb were 2.21 and 10.46 μg·kg respectively -1 , no pesticides were detected in other samples; at the same time, the pesticide residues in 10 forage grasses with rice stalks as raw materials were screened, and the results showed that the detected concentrations of the two samples of Daobunling were 15.18 and 14.66 μg·kg respectively -1 , the detection concentration of 1 sample of indoxacarb was 17.25 μg·kg -1 , the detected concentrations of the two samples of pymetrozine were 9.58 and 17.73...

Embodiment 3

[0185] Take 3 parts of rice from a rice production base in Shanghai, and process it according to the following steps:

[0186] 1) Sample preparation

[0187] The paddy samples were dehulled, ground and pulverized in a high-speed pulverizer, and passed through a 40-mesh sieve.

[0188] 2) Extraction and purification

[0189] Extraction: Weigh 5.0g of rice evenly into a 50mL centrifuge tube, add 10mL of distilled water, vortex and mix well, at the same time add ceramic beads with a diameter of 4mm, add 10mL of acetonitrile, and vortex again for 30 seconds to mix. Add QuEChERS extraction reagent (anhydrous MgSO 4 5.5g, NaCl 1.5g, disodium citrate 0.5g and sodium citrate 1.0g), mix quickly, put in a shaker, shake at high speed for 10min, and then shake at 4000r·min -1 , Centrifuge at 4°C for 5 minutes and wait for purification.

[0190] Purification: Take 10 mL of the centrifuged supernatant, add purification reagent (PSA 0.1 g, anhydrous MgSO 4 0.6g). Shake at high speed fo...

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Abstract

The invention discloses a method for detecting pesticide residues in rice and / or rice stems. The method includes the following steps that: a to-be-detected sample is pretreated; and after the to-be-detected sample is pretreated, a to-be-detected sample solution is detected through liquid chromatography, the mobile phase A of the liquid chromatography is 0.1% formic acid aqueous solution, and the mobile phase B of the liquid chromatography is methanol, and a percentage refers to a volume percentage. The pretreatment of the to-be-detected sample further includes the following two steps that: (1)mixing and extraction are performed on the to-be-detected sample, water, an organic solvent and a reagent A, so that an organic phase extract solution can be obtained; and (2) the organic phase extract solution in the step (1) is mixed with a reagent B, so that the to-be-detected sample solution is obtained. With the method of the invention adopted, 42 kinds of pesticide residues including propamocarb, chlorantraniliprole, thiabendazole, oxadiazon, pyraclostrobin, cyhalofop-butyl and emamectin benzoate which are contained in the rice and / or rice stems can be quantitatively detected at the same time; and a new technical means can be provided for the safety monitoring of the quality of the rice and rice stems.

Description

technical field [0001] The invention relates to a method for detecting pesticide residues in rice and rice stems. Background technique [0002] As an important staple food source, rice has made important contributions to the nutrition and health of Chinese people. At the same time, rice stalks play an economic role as fodder. However, due to the excessive use and abuse of insecticides, fungicides and herbicides in rice, the pesticide residues in rice and rice stems exceed the standard, which poses a threat to human health. Therefore, it is of great significance to establish a simple, fast and efficient detection technology for multi-residue pesticides in rice and rice stems, and to strengthen the monitoring of pesticide residues. [0003] At present, the pretreatment methods for the detection of pesticide residues in rice and rice stems include liquid-liquid extraction, solid phase extraction, gel permeation chromatography, and QuEChERS. It is not conducive to the rapid s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 姚春霞周佳欣李亚辉宋卫国杨海锋王玉双
Owner SHANGHAI ACAD OF AGRI SCI
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