Method for measuring residual amounts of pirimicarb and mtabolites thereof in cabbage

A determination method, the technology of pirimicarb, which is applied in the field of determination of pesticide residues, can solve the problem of simultaneous detection of pirimicarb compound residues, etc., and achieve low cost, high speed, high stability and reliability Effect

Inactive Publication Date: 2011-10-19
CENT LAB TIANJIN ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the methods at home and abroad are to detect the parent body of pirimicarb, and there are also reports on the simultaneous detection of pirimicarb and desmethyl-pirimicarb, but no simultaneous detection of pirimicarb, desmethyl-pirimicarb and desmethyl-pirimicarb Report on Residues of Three Formamide-based Pirimicarb Compounds

Method used

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  • Method for measuring residual amounts of pirimicarb and mtabolites thereof in cabbage
  • Method for measuring residual amounts of pirimicarb and mtabolites thereof in cabbage
  • Method for measuring residual amounts of pirimicarb and mtabolites thereof in cabbage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Establish a standard curve

[0041] The blank solution of cabbage that does not contain pirimicarb and its metabolites is treated with the pretreatment method of this determination method, and the mixed standard working solution of pirimicarb and its metabolites is prepared with a series concentration of 5, 2.5, 0.5, 0.1, 0.025 and 0.01 μg / mL, inject 5 μL respectively, take the injection concentration as the abscissa, and the peak area as the ordinate to make a standard curve. The linear equation of pirimicarb is y = 766637x - 11407, and the correlation coefficient is r = 0.998; the linear equation of demethylformamide-based pirimicarb is y = 35820x - 1681.8, and the correlation coefficient is r = 0.998.

[0042] (2) Pre-processing

[0043] Weigh 10g of the sample (accurate to 0.01g), add 20mL of water and 30mL of acetonitrile to shake for 30min, filter to the separatory funnel, add 20mL of acetonitrile to wash the residue, filter the washing liquid into the separ...

Embodiment 2

[0062] The accuracy, precision and sensitivity test of this method

[0063] Select a cabbage sample that does not contain pirimicarb and its metabolites as the background, add the standard working solution of pirimicarb and its metabolites to the cabbage sample, and then process and measure it according to the method in the above examples. Each concentration was repeated 5 times, and the final recoveries and relative standard deviations are shown in Table 2.

[0064] Table 2 Added recovery results

[0065]

[0066] It can be seen from the above table that the recovery rate is 70-100%, and the relative standard deviation is within 10%, indicating that the method has high accuracy and good precision. The minimum quantitative limit of the method of the present invention: pirimicarb is 0.005 mg / kg; demethylpirimicarb is 0.005 mg / kg; demethylformamido-pirimicarb is 0.05 mg / kg. The sensitivity of the method is good.

Embodiment 3

[0068] Application of the method in real sample detection

[0069] Representative samples of cabbage were taken from supermarkets and farmers’ markets in Tianjin, and this method was used to detect anti-pirimicarb and its metabolites. The results are shown in Table 3.

[0070] Table 3 Test results

[0071]

[0072] 20 batches of representative cabbage samples were taken from supermarkets and farmer's markets in Tianjin. The results showed that neither pirimicarb nor its metabolites were detected, indicating that pirimicarb is safe to use on cabbage.

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Abstract

The invention discloses a method for measuring the residual amounts of pirimicarb and mtabolites thereof in a cabbage. The method comprises the following steps of: weighing 10 grams of sample accurately to 0.01 gram, adding 20 milliliters of water and 30 milliliters of acetonitrile, performing oscillation for 30 minutes, filtering the oscillated solution into a separating funnel, adding 20 milliliters of acetonitrile to wash residues, filtering washing liquid into the separating funnel, adding 10 grams of sodium chloride, performing the oscillation for 2 minutes, standing the oscillated solution for 5 minutes, discarding a water phase on a lower layer after the oscillated solution is demixed, concentrating an acetonitrile phase on an upper layer under reduced pressure until dryness, adding 2 milliliters of methanol, performing whirling for 1 minute, causing the solution to pass through a filtration membrane of 0.22 mu m, transferring the filtered solution into a small sample introduction bottle, and finally performing detection by adopting ultra performance liquid chromatography-tandem mass spectrum (UPLC / MS / MS). The method for measuring the residual amounts of the pirimicarb and the mtabolites thereof in the cabbage is put forward for the first time, and has the characteristics of high speed, low cost, high accuracy, high stability and high reliability.

Description

technical field [0001] The invention belongs to the technical field of determination of pesticide residues, and in particular relates to a method for determining the residues of pirimicarb and its metabolites (desmethylpirimicarb and desmethylformamide-based pirimicarb) in cabbage. Background technique [0002] Kale is a cruciferous vegetable that people eat frequently and in large quantities. Japanese scientists believe that the anti-aging and anti-oxidation effects of cabbage are at a higher level than that of asparagus and cauliflower. The nutritional value of cabbage is almost the same as that of Chinese cabbage, and the content of vitamin C is about twice as high. Cabbage can improve human immunity and prevent colds. Among anti-cancer vegetables, cabbage ranks fifth. [0003] Aphids are one of the main pests in cabbage planting. Aphids reproduce quickly, and they often live on the shrunken parts of the heart leaves and leaf backs of cabbage. They suck plant juice, cau...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/14
Inventor 邵辉
Owner CENT LAB TIANJIN ACADEMY OF AGRI SCI
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