Method for extracting and purifying glyphosate residue in vegetable oil

A technology for glyphosate and vegetable oil, which is applied in the field of pretreatment for the determination of pesticide residues, can solve the problems of lack of fluorescent and chromophoric groups, long pretreatment time, and long reaction time, so as to reduce the types of reagents, shorten the time, The effect of reducing dosage

Pending Publication Date: 2022-07-12
ZHEJIANG FORESTRY ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Because glyphosate is highly polar, insoluble in most organic solvents, difficult to volatilize, and lacks fluorescence and chromophoric groups, this pretreatment method changes the chromatographic behavior of glyphosate in the gas and liquid phases through derivatization reactions Only by improving the response value of the detector can it be detected normally, but the derivatization reaction requires a wide variety of reagents and a long reaction time, which leads to problems such as long time-consuming pretreatment, high cost and troublesome operation.

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  • Method for extracting and purifying glyphosate residue in vegetable oil
  • Method for extracting and purifying glyphosate residue in vegetable oil
  • Method for extracting and purifying glyphosate residue in vegetable oil

Examples

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Effect test

Embodiment 1

[0039] A kind of extraction and purification method of glyphosate residue in vegetable oil, such as figure 1 shown, including the following steps:

[0040] (1) Mix the Camellia oleifera seed oil sample evenly, accurately weigh 1.00g of Camellia oleifera seed oil sample in a 10mL centrifuge tube;

[0041] (2) Add 2 mL of dichloromethane (chromatographically pure) to the centrifuge tube;

[0042] (3) Add 5 mL of ultrapure water to the centrifuge tube;

[0043] (4) Seal the centrifuge tube and place it on a vortex shaker for high-speed vortex mixing and extraction for 40s;

[0044](5) place the centrifuge tube after the vortex extraction in the centrifuge, and centrifuge at high speed (centrifugal force 10000×g) for 3 minutes to quickly stratify the organic layer and the water layer;

[0045] (6) Absorb the supernatant liquid (that is, the aqueous solution of glyphosate), pass it through a Florisil column (the specification of the Florisil cartridge is 1000 mg, 6 mL) to purify...

Embodiment 2

[0064] Compared with Example 1, the difference between this example is that in this example, 1000 mg / L high-concentration glyphosate standard solution was added to the Camellia oleifera seed oil sample to form a glyphosate concentration of 5.0 mg / kg and 3.0 mg. / kg and 1.0mg / kg camellia seed oil spiked samples, respectively accurately weighed three glyphosate concentrations of camellia seed oil spiked samples 1.00g in three 10mL centrifuge tubes, and according to Example 1 (2 (2) The steps of )-(6) carry out pretreatment analysis, and the equipment and chromatographic conditions are consistent with those in Example 1.

[0065] The detection method of the ion chromatograph is the prior art, which will not be repeated here. The purified solution after three kinds of camellia seed oil spiked samples with different glyphosate concentrations are put into the injection bottle and detected by the ion chromatograph to obtain Glyphosate was detected in camellia seed oil spiked samples ...

Embodiment 3

[0067] Compared with Example 1, the difference between this example is that in this example, a high-concentration glyphosate standard solution is added to the camellia seed oil sample to form a camellia seed oil spiked sample with a glyphosate concentration of 1.0 mg / kg. , after mixing evenly, accurately weigh 1.00g of Camellia oleifera seed oil spiked sample in a 10mL centrifuge tube, and carry out pretreatment analysis according to the steps of (2)-(6) in Example 1. Instruments and chromatographic conditions and examples If 1 is consistent, measure the recovery rate, repeat twice, and take the average value of the recovery rate to avoid accidental errors.

[0068] The detection method of the ion chromatograph is the prior art, which will not be repeated here. The purified solution of the camellia seed oil spiked sample is put into a sample injection bottle and detected by the ion chromatograph to obtain the camellia seed oil spiked sample. The chromatogram of glyphosate dete...

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Abstract

The invention relates to the technical field of pesticide residue determination pretreatment, and discloses a method for extracting and purifying glyphosate residue in vegetable oil, which comprises the following steps: 1, sample preparation: uniformly mixing a vegetable oil sample, and weighing the vegetable oil sample in a centrifuge tube; step 2, extracting: adding the extracting solution into a centrifugal tube, carrying out vortex oscillation and then centrifuging to obtain a target solution dissolved with glyphosate, and taking out the target solution to wait for purification; and step 3, purification: sucking the target solution, passing through a solid-phase extraction small column for purification to obtain a purified solution, sucking the purified solution into a sample introduction bottle, and waiting for determination and analysis by an ion chromatograph. The extraction and purification method provided by the invention establishes a method which does not need derivation and concentration and can be used for conveniently and rapidly performing accurate quantitative determination on the glyphosate content in the vegetable oil; meanwhile, the requirement of GB2763 on the detection limit of the glyphosate in the vegetable oil is met.

Description

technical field [0001] The invention relates to the technical field of pretreatment for determination of pesticide residues, in particular to a method for extracting and purifying glyphosate residues in vegetable oil. Background technique [0002] Vegetable oil is an indispensable and important food material in people's daily life, and its quality and safety have also attracted much attention. In recent years, spraying and weeding has become the main way of planting and tending oil farmers. The use of glyphosate is increasing year by year, especially glyphosate. Although the use of glyphosate reduces costs, increases production, and brings short-term benefits, the resulting safety issues have become the focus of attention. my country's food safety standard GB2763 clearly stipulates the residues of glyphosate in oils and fats. The maximum residue limit of glyphosate in cottonseed oil is 0.05mg / kg, and the detection method GB / T23750-2009 or SN / T1923-2007 is indicated. , this sta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/16
CPCG01N30/02G01N30/06G01N30/16G01N2030/062G01N2030/065G01N2030/167
Inventor 杨柳王衍彬方燕朱杰丽吴翠蓉欧菊芳柴振林陆军王家瑶马子恒黄忆婷
Owner ZHEJIANG FORESTRY ACAD
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