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Detection method for twelve kinds of pyrethroids pesticide residues in capsanthin

A technology for pyrethroids and detection methods, which is applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as matrix interference, complex matrix, and inability to achieve effective detection, and achieves high accuracy, reduced interference, and easy mass production. The effect of sample detection

Active Publication Date: 2013-01-23
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because capsanthin contains a lot of pigments and the matrix is ​​complex, the above-mentioned detection method for pyrethroids in food is directly used, the matrix interference is very large, and effective detection cannot be achieved

Method used

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  • Detection method for twelve kinds of pyrethroids pesticide residues in capsanthin
  • Detection method for twelve kinds of pyrethroids pesticide residues in capsanthin
  • Detection method for twelve kinds of pyrethroids pesticide residues in capsanthin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: The specific implementation steps of the detection method of twelve pyrethroid pesticide residues in the capsicum red are as follows:

[0021] (1) Standard curve: Twelve kinds of pyrethroid pesticide residue standard stock solutions are accurately measured respectively, and they are gradually diluted with Fisher chromatographic pure hexane to the mass concentrations of 0.01, 0.05, 0.1, 0.2, 0.5, 1.0 mg, respectively / L series of standard solutions were injected and determined under the above test conditions, and the peak area Y of the twelve pyrethroid pesticide residues was plotted against the mass concentration X.

[0022] (2) Sample extraction: accurately weigh 1.0g (accurate to 0.0001g) =200 capsicum sample in a 25mL volumetric flask, add 12.5mL cyclohexane-ethyl acetate mixed solvent with a volume ratio of 50:50, sonicate for 15min, 2 times, cool to room temperature, add 50:50 volume ratio The volume of cyclohexane-ethyl acetate mixed solvent is constant. T...

Embodiment 2

[0031] Example 2: The specific implementation steps of the method for detecting twelve pyrethroid pesticide residues in the capsicum red are as follows:

[0032] (1) Standard curve: the same as in Example 1.

[0033] (2) Sample extraction: accurately weigh 0.5g (accurate to 0.0001g) =50 Capsicum sample in a 10mL volumetric flask, add 10mL cyclohexane-ethyl acetate mixed solvent with a volume ratio of 50:50, sonicate for 10min, cool to room temperature, add cyclohexane-acetic acid with a volume ratio of 50:50 Constant volume of ethyl ester mixed solvent. The extract was transferred to a centrifuge tube, centrifuged at 4000 r / min at 5°C for 5 min, the supernatant was taken and filtered with a 0.45 μm filter membrane, and the filtrate was transferred to a GPC loading bottle.

[0034] (3) GPC purification treatment: The GPC detection wavelength is 254nm, the mobile phase is a cyclohexane-ethyl acetate mixed solvent with a volume ratio of 50:50, and the flow rate is 5.0 mL / min. Load 2....

Embodiment 3

[0039] Example 3: The specific implementation steps of the method for detecting twelve pyrethroid pesticide residues in the capsicum red are as follows:

[0040] (1) Standard curve: the same as in Example 1.

[0041] (2) Sample extraction: accurately weigh 1.5g (accurate to 0.0001g) =50 Capsicum sample in a 25mL volumetric flask, add 25mL cyclohexane-ethyl acetate mixed solvent with a volume ratio of 50:50, ultrasonicate for 30min, 3 times, cool to room temperature, add a 50:50 volume ratio ring The hexane-ethyl acetate mixed solvent is constant volume. The extract was transferred to a centrifuge tube, centrifuged at 10000 r / min at 5°C for 10 min, the supernatant was taken and filtered with a 0.45 μm filter membrane, and the filtrate was transferred to a GPC loading bottle.

[0042] (3) GPC purification treatment: The GPC detection wavelength is 254nm, the mobile phase is a cyclohexane-ethyl acetate mixed solvent with a volume ratio of 50:50, and the flow rate is 5.0 mL / min. Load ...

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Abstract

The invention discloses a detection method for twelve kinds of pyrethroids pesticide residues in capsanthin. The detection method comprises the following steps of: ultrasonically extracting the capsanthin with an extracting solvent and then separating an extract liquor to obtain a supernatant liquor; purifying the supernatant liquor by using a gel permeation chromatography, collecting target eluant, concentrating the target eluant until dry and then making the volume constant to obtain a sample solution; and measuring the sample solution by adopting a gas chromatography-tandem mass spectrum in a selected ion monitoring mode and quantifying with an external standard method. The method is used for processing the capsanthin by adopting a GPC (gel permeation chromatography) technology, so that most of macromolecular pigment matters are moved, interference of sample matrixes on measurement is lowered greatly; and the detection method is high in accuracy and strong in applicability for the capsanthin. The detection is carried out by adopting the gas chromatography-tandem mass spectrum and selecting the ion monitoring mode, so that the method has the advantages of high sensitivity and high automation degree, is easy and fast and is capable of detecting large batches of samples easily; and generated waste liquid can be recycled and reused so as to reduce the detection cost and reduce the environmental pollution.

Description

Technical field [0001] The invention relates to a method for detecting pesticide residues in food additives, in particular to a method for detecting twelve pyrethroid pesticide residues in capsicum red. Background technique [0002] Paprika is a deep red oily liquid pigment obtained by extracting the fruit of red pepper as a raw material. It is a natural coloring agent with nutritional strengthening effect, and its main component is carotenoids. Due to the high food safety and physiological activity of natural pigments, paprika is more and more popular. [0003] Pepper is the raw material for the production of red pepper. In order to ensure and promote the normal growth of pepper, farmers will apply various pesticides that kill insects, sterilize, and kill harmful animals (or weeds), resulting in widespread pesticide residues in pepper. These pesticide residues are continuously concentrated and enriched during the extraction and processing of pepper, leading to potential safety ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
Inventor 高伟吉桂珍杜精精程淑君
Owner CHENGUANG BIOTECH GRP CO LTD
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