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A rapid detection method for pyridine pesticides in plant extracts

A plant extract and detection method technology, applied in the field of detection of harmful substances, can solve the problems of long cycle, high cost, complicated process, etc., and achieve the effects of simple operation, low detection limit and low detection cost.

Inactive Publication Date: 2017-07-25
陕西出入境检验检疫局检验检疫技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a rapid detection method for pyridine pesticides in plant extracts, which solves the problem that the sample pretreatment in the existing detection method needs to be purified by solid phase extraction column or gel permeation chromatography, the process is complicated and the cost is high , the problem of long cycle

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  • A rapid detection method for pyridine pesticides in plant extracts
  • A rapid detection method for pyridine pesticides in plant extracts
  • A rapid detection method for pyridine pesticides in plant extracts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Weigh 0.5g of Lycium barbarum extract (accurate to 0.01g) into a 50mL glass centrifuge tube, add 10ng of standard substance to mix the standard, add 10mL of ethyl acetate and 0.2mL of ammonia water, vortex and mix, ultrasonically extract for 20min, and centrifuge at 4000r / min 10min. Take 8 mL of the supernatant, concentrate to dryness, add 1 mL of methanol-0.1% formic acid water (1+9) to constant volume, and pass through a 0.22 μm organic microporous membrane to obtain the extracted and concentrated plant extract sample, which is ready to be injected.

[0076] Using TF-LC-MS / MS method to detect pyridine pesticide residues in plant extracts, TF detection parameters: TF purification column: Cyclone TM -P: 0.5×50mm; mobile phase: A is methanol, B is 0.1% formic acid in water; see Table 3 for gradient elution program and flow rate. Liquid phase detection parameters: Hypersil GOLD aQ C18 (column length 50mm, column inner diameter 2.1mm, packing particle size 3μm), or equiva...

example 2

[0081] Weigh 1g of Lycium barbarum extract (accurate to 0.01g) into a 50mL glass centrifuge tube, add 20ng of standard substance to mix the standard, add 30mL of ethyl acetate, 0.3mL of ammonia water, vortex and mix, ultrasonically extract for 25min, and centrifuge at 5000r / min for 6min . Take 10 mL of the supernatant, concentrate to dryness, add 1 mL of methanol-0.1% formic acid water (1+9) to constant volume, and pass through a 0.22 μm organic microporous membrane to obtain the extracted and concentrated plant extract sample, which is ready to be injected.

[0082] Using TF-LC-MS / MS method to detect pyridine pesticide residues in plant extracts, TF detection parameters: TF purification column: Cyclone TM -P: 0.5×50mm; mobile phase: A is methanol, B is 0.1% formic acid water; gradient elution program and flow rate are shown in Table 4. Liquid phase detection parameters: Hypersil GOLD aQ C18 (column length 50mm, column inner diameter 2.1mm, packing particle size 3μm), or equi...

example 3

[0086] Weigh 2g of Lycium barbarum extract (accurate to 0.01g) into a 50mL glass centrifuge tube, add 40ng of standard substance to mix the standard, add 20mL of ethyl acetate, 0.4mL of ammonia water, vortex and mix, ultrasonically extract for 30min, and centrifuge at 6000r / min for 4min . Take 15 mL of the supernatant, concentrate to dryness, add 1 mL of methanol-0.1% formic acid water (1+9) to constant volume, and pass through a 0.22 μm organic microporous membrane to obtain the extracted and concentrated plant extract sample, which is ready to be injected.

[0087] Using TF-LC-MS / MS method to detect pyridine pesticide residues in plant extracts, TF detection parameters: TF purification column: Cyclone TM -P: 0.5×50mm; mobile phase: A is methanol, B is 0.1% formic acid water; gradient elution program and flow rate are shown in Table 5. Liquid phase detection parameters: Hypersil GOLD aQ C18 (column length 50mm, column inner diameter 2.1mm, packing particle size 3μm), or equi...

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Abstract

The invention discloses a rapid detection method of pyridine pesticides in a plant extract. The method specifically comprises steps as follows: firstly, the plant extract and a solvent are mixed for pretreatment, and a plant extract sample after extraction and concentration is obtained; then pyridine pesticide residues in the plant extract are detected with the high performance liquid chromatography-tandem mass spectrometry. According to the detection method, the pretreatment method is simple and convenient to operate, the solid phase extraction or gel permeation purification process in the traditional method is omitted, the sample pretreatment time is shortened by more than 2 times, only 1 hour is taken to detect one sample completely, the detection limit can reach 10 mu g / kg, the detection period is short, the detection cost is low, the detection limit is low, the repeatability is good, and the method is suitable for product quality detection by production enterprises and management departments.

Description

technical field [0001] The invention belongs to the technical field of harmful substance detection and relates to a rapid detection method for pyridine pesticides in plant extracts. Background technique [0002] Pyridine pesticides have the characteristics of high biological activity, low toxicity, strong systemic property, and good selectivity. They are a new class of compounds obtained by replacing the benzene ring with pyridine. Acetamiprid and imidacloprid belong to the neonicotinoid insecticides, which have the characteristics of broad-spectrum insecticidal, high activity and long duration. Highly active and selective pyridine herbicide; boscalid is a new type of nicotinamide fungicide, mainly used for various rot and powdery mildew, etc. It has a strong ability to inhibit the germination of spores, and it is compatible with other Fungicides have no cross-resistance. Pyridine pesticides are often used in plants and Chinese medicinal materials due to their remarkable e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 孔祥虹刘开何强张璐邹阳付骋宇李莹
Owner 陕西出入境检验检疫局检验检疫技术中心