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Detection method of pyrethroid pesticide remained in rice

A technology for pyrethroids and pesticide residues is applied in the field of detection of pesticide residues in grains. less demanding effects

Inactive Publication Date: 2010-12-15
王冬群 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the extraction method are: less extraction time, lower extraction rate, more loss of pyrethroid pesticides in the purification process, complicated gas chromatography column temperature rise program, difficult operation, high operation requirements, time-consuming and labor-intensive, and complicated operation steps. , with low quantitative recovery
"Determination of 13 organophosphorus and pyrethroid pesticide residues in rice by capillary gas chromatography" by Zhao Yu et al., Modern Scientific Instruments, 2006, 3, disclosed that rice was soaked in water for 30 minutes, added acetonitrile to homogenize for 2 minutes, and the filtrate Use sodium chloride to stand and separate the phases for 10 minutes, and blow the organic phase to near dryness at 75-78°C with nitrogen; dissolve the organic phase with n-hexane to obtain an extract, and use the mixed solvent of n-hexane-acetone in order to purify the extract on a Florisil column Rinse and purify three times, each eluate was blown dry with nitrogen on a 40°C water bath and concentrated to less than 4mL, then fixed the bath with n-hexane to 4mL, mixed to obtain a purified solution for gas spectrometry; gas chromatographic conditions: DB-17 column Or HP-17 column, the column temperature is 150°C (2min), the temperature is programmed to 270°C at a rate of 6°C / min (retained for 25min), the inlet temperature is 200°C, the detector temperature is 320°C, and the flow rate is split; There is no specific injection volume and the way of purging with nitrogen gas after injection time. Although the extraction process is simplified, the extraction rate is also low, the gas chromatography conditions are still complicated, the operation is difficult, the operation requirements are high, and the quantitative recovery rate is also lower

Method used

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  • Detection method of pyrethroid pesticide remained in rice

Examples

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Embodiment 1

[0017] A method for detecting pyrethroid pesticide residues in rice, taking 25 grams of crushed rice into a 125ml reagent bottle, adding permethrin, cypermethrin, bifenthrin, and cyhalothrin with a concentration of 1mg / kg The mixed standard solution prepared by pesticides such as fenvalerate, fenvalerate, deltamethrin and fenpropathrin, the addition level is 0.05mg·kg -1 For rice, the above-mentioned pesticide standard samples were all provided by the Environmental Protection Scientific Research and Monitoring Institute of the Ministry of Agriculture, with a concentration of 100mg / kg, prepared with chromatographically pure n-hexane and diluted to the required concentration. Then add 50 milliliters of acetonitrile, use a homogenizer to homogenize at high speed for 2 minutes, stand for extraction for 4 hours, add 15 milliliters of ultra-pure water to shake and let stand for 30 minutes, filter, and pour the filtrate into a centrifuge tube with 4 grams of sodium chloride In the me...

Embodiment 2

[0019]It is basically the same as in Example 1, except that the concentration of each pyrethroid pesticide is 0.1mg / kg, and the DB-1701 chromatographic column is replaced by an HP-5 chromatographic column, and the detection time can be shortened to 13min, obtaining the following: figure 2 The chromatogram of pyrethroid pesticide shown, can make the qualitative of pesticide according to the retention time after separation, from figure 2 It can be seen that the retention time of bifenthrin 1 is 6.209min, the retention time of fenpropathrin 2 is 6.322min, the retention time of cyhalothrin 3 is 7.041min, and the retention time of permethrin 4 is 8.039min min, the retention time of cypermethrin 5 is 9.197-9.548min, the retention time of fenvalerate 6 is 11.025-11.522min, and the retention time of deltamethrin 7 is 12.993min; repeat this embodiment three times, obtain according to the surface area The average quantitative recoveries are shown in Table 1.

Embodiment 3

[0021] It is basically the same as Example 2, except that the concentration of each pyrethroid pesticide is 0.5 mg / kg.

[0022] In the actual detection application, it is operated according to the method of the present invention, without adding the above-mentioned pesticide standard sample, and the specific detection method is the same as in Example 1 or Example 2, and the examples are no longer listed here.

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Abstract

The invention discloses a detection method of pyrethroid pesticide remained in rice. The method comprises the following steps of: fully extracting pyrethroid pesticide with acetonitrile for 4 h; vibrating with ultra-pure water and then standing still for 30 min so that the pyrethroid pesticide is separated very well; centrifugally splitting the phase of the pyrethroid pesticide for 6 min to have better split phases and higher extraction rate; leaching and cleaning with hexane and acetone (in a ratio of 90 to 10) to better remove the pyrethroid pesticide; and increasing a column temperature to 260 DEG C at a programmed temperature rise rate of 40 DEG C / min and keeping both a sampling temperature and a detector temperature at 260 DEG C. The gas chromatograph is simple and convenient to operate, finishes the separation and the detection of the pyrethroid pesticide in a shorter time and has simple and rapid gas chromatography conditions and more accurate measuring value. Accordingly, the detection method of the pyrethroid pesticide remained in rice has higher extraction rate, simple and rapid gas chromatography conditions, lower operation requirement and higher quantitative recovery rate.

Description

technical field [0001] The invention relates to a detection method for pesticide residues in grains, in particular to a detection method for pyrethroid pesticide residues in rice. Background technique [0002] Rice is the main food we eat daily, and its quality and safety are closely related to people's physical and mental health. Pesticide residues in rice include organophosphorus and pyrethroids, etc. Pyrethroid pesticides include permethrin, cypermethrin, bifenthrin, cyhalothrin, fenvalerate, deltamethrin and fenvalerate permethrin etc. The detection method of pyrethroids such as "method for the determination of various pyrethroid pesticide residues in imported and exported foods", ST / T1157-2008, just discloses the use of sodium chloride, water and n-hexane-acetone (1+1) for rice. Mixed solvent immersion, homogenization and centrifugal extraction, the extraction conditions are: first add sodium chloride and water to soak for 0.5h, then add n-hexane-acetone (1+1) mixed s...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 王冬群吴华新韩敏辉
Owner 王冬群
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