Determination method of pesticides including ethoprophos in Xinhui tangerine peels and products of Xinhui tangerine peels

A technology for eliminating line phosphorus and tangerine peel, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems affecting the export competitiveness and product reputation of Xinhui tangerine peel and its products, the health risks of residue detection operators, and the pesticide residues in Xinhui tangerine peel. Pollution and other problems, to achieve the effect of strong resistance to matrix interference, low harm to human health, and high recovery rate

Active Publication Date: 2016-06-22
新会出入境检验检疫局综合技术服务中心
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the food safety risks faced by Xinhui tangerine peel and its products are very serious. In recent years, there have been reports of pesticide residues in Xinhui tangerine peel, which not only affects human health and damages the interests of consumers, but also affects the export competitiveness and products of Xinhui tangerine peel and its products. reputation
[0003] In my country's existing pesticide testing standards, redistilled acetone is widely used in sample pretreatment, and acetone is extremely harmful to human liver, kidney and pancreas.
Moreover, the re-distillation and use of dichloromethane and acetone have certain risks to the health of the residue detection operators.

Method used

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  • Determination method of pesticides including ethoprophos in Xinhui tangerine peels and products of Xinhui tangerine peels
  • Determination method of pesticides including ethoprophos in Xinhui tangerine peels and products of Xinhui tangerine peels
  • Determination method of pesticides including ethoprophos in Xinhui tangerine peels and products of Xinhui tangerine peels

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: sample determination

[0032] 1.1 Preparation of standard stock solution: Accurately absorb 100.0 μg of methimen, fetophos, terbufos, monocrotophos, methyl parathion, fenitrothion, isofenphos-methyl and isocarbophos respectively / mL standard solution 1.000mL to a 25mL brown volumetric flask, dilute with chromatographically pure ethyl acetate and make up to the mark, respectively prepare standard stock solutions with a mass concentration of 4.000μg / mL, store at 4°C for later use.

[0033] 1.2 Preparation of standard working solution: Accurately draw 0.0050mL, 0.0125mL, 0.050mL, 0.50mL and 5.0mL of standard stock solution respectively, place them in 10mL brown volumetric flasks, dilute with chromatographically pure ethyl acetate and make up to the mark. Shake well to prepare standard working solutions with mass concentrations of 0.0020 μg / mL, 0.0050 μg / mL, 0.020 μg / mL, 0.20 μg / mL, and 2.0 μg / mL, and store at 4 °C for later use.

[0034] 1.3 Draw a standar...

Embodiment 2

[0044] Embodiment 2: the selection of extraction solvent

[0045] In this example, the preparation of the standard stock solution and the standard working solution, the purification of the sample and the chromatographic conditions are the same as in Example 1. The extraction method of the sample is as follows: Weigh 2.00 g of negative Xinhui tangerine peel powder and place it in a 50 mL centrifuge tube, add 0.20μg / mL standard solution, add 2mL water, vibrate and sonicate, and extract twice with 5mL petroleum ether, methanol and ethyl acetate respectively. The experimental results are shown in Table 1.

[0046]

[0047]

[0048] From the comparative analysis of the standard addition recoveries extracted by different organic solvents in Table 1, it can be seen that the recovery obtained by ethyl acetate as the extraction solvent is higher and stable, and is most suitable for extracting the pesticide residues in Xinhui tangerine peel and its products described in the prese...

Embodiment 3

[0049] Embodiment 3: the selection of solid-phase extraction column filler type

[0050] Because some volatile oils, flavonoids, alkaloids and other chemical components unique to Xinhui tangerine peel are not easy to remove by conventional methods, and there are also components such as protein, fat, sugar and organic acids, these impurities will seriously interfere with the determination of target analytes. At the same time, the service life of the chromatographic column will be greatly shortened, so the sample needs to be pre-purified. The SPE column with a single filler is not effective in removing impurities.

[0051] The C18 filler has a high adsorption capacity for impurities such as protein, fat, and vitamins, but it can also firmly adsorb the target compound, which affects the recovery rate of the standard addition. PSA filler can effectively adsorb impurities such as flavonoids, alkaloids, sugars, phenols, fatty acids, organic acids and pigments, and MWNTs can effec...

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Abstract

The invention provides a determination method of pesticides including ethoprophos and the like in Xinhui tangerine peels and products of the Xinhui tangerine peels. The pesticides comprise the ethoprophos, sulfotep, terbufos, monocrotophos, methy-parathion, fenitrothion, isofenphos-methyl and isocarbophos. The method comprises the following steps: manufacturing a standard curve, extracting a sample, purifying the sample and determining the sample. The determination method has the advantages of simplicity and rapidness in operation, high sensitivity and strong matrix interference resistance capability, and is suitable for qualitative and quantitative analysis of pesticide residues in the Xinhui tangerine peels and the products of the Xinhui tangerine peels.

Description

technical field [0001] The invention relates to the technical field of detection of pesticide residues, in particular to a method for determining pesticides such as phenmetphos in Xinhui tangerine peel and products. Background technique [0002] Xinhui tangerine peel is a rare local specialty that has the same source of medicine and food, and is excellent in food and nutrition. It is one of the top ten authentic Chinese medicinal materials in Guangdong and the first treasure of "Guangdong three treasures" (tangerine peel, ginger, and straw grass) And Qing court tribute. However, the food safety risks faced by Xinhui tangerine peel and its products are very serious. In recent years, there have been reports of pesticide residues in Xinhui tangerine peel, which not only affects human health and damages the interests of consumers, but also affects the export competitiveness and products of Xinhui tangerine peel and its products. reputation. [0003] In my country's existing pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 彭晓俊梁伟华蔡璇庞晋山李蓉
Owner 新会出入境检验检疫局综合技术服务中心
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