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A method for detecting aminopyralid pesticide residues in barley

A technology of aminopyridine and a detection method, which is applied in the abbreviated process field of pesticide residues, and can solve the problems of long duration of the chemicals and the like

Inactive Publication Date: 2015-11-25
NANTONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF THE PEOPLES REPUBLIC OF CHINA
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Aminopyralid (aminopyralid), whose chemical name is 4-amino-3,6-dichloropyridine-2-carboxylic acid, is a synthetic hormone-type herbicide of pyridine carboxylic acid, widely used in mountains, grasslands, planting Weed control in land and non-cultivated land, long-lasting agent; in the new version of "National Food Safety Standard Food Maximum Residue Limits of Pesticides GB2763-2014", aminopyralid is one of the 65 newly added pesticides. (barley, barley, oats, triticale) the maximum residue limit is 0.1mg / kg, this standard has been implemented since August 1, 2014, after searching, there is no standard and literature report on the detection of this pesticide

Method used

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  • A method for detecting aminopyralid pesticide residues in barley
  • A method for detecting aminopyralid pesticide residues in barley
  • A method for detecting aminopyralid pesticide residues in barley

Examples

Experimental program
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preparation example Construction

[0029] 1. Preparation, extraction, purification and concentration of barley samples:

[0030] Grind the barley through a 40-mesh sieve, weigh 4.00 g of the sample, add 40 ml of chromatographic-grade pure methanol as the extract (for recovery detection, the total amount of standard solution and methanol used is 40 ml), vortex mix for 5 min, and take Clear liquid 20ml, use HR-XA (3ml, 200mg) solid phase extraction cartridge to purify and concentrate according to the following steps:

[0031] (1), column activation: 5ml chromatographic grade pure methanol, 5ml water (do not let the extraction column evaporate);

[0032] (2), sample loading: add the supernatant to the extraction column under vacuum;

[0033] (3), column cleaning: sequentially add 2.5ml of sodium acetate aqueous solution with a concentration of 50mmol / L, 2.5ml of chromatographic grade pure methanol, and dry the extraction column with nitrogen;

[0034] (4), elution: use 5ml chromatographic grade pure methanol to ...

Embodiment

[0051] Example: Detection of aminopyralid in barley

[0052] To draw a standard curve:

[0053] Use chromatographic grade pure methanol as the solvent to prepare the mass concentration of 0.005, 0.010, 0.020, 0.050, 0.10mg / L aminopyralid standard solution, with 100% acetonitrile as A phase, 5mmol ammonium acetate aqueous solution as B phase, A phase and Phase B is mixed at a volume ratio of 60:40 as the mobile phase, using an anion exchange column (DIONEX AcclaimMix-ModeWAX-1), with a flow rate of 500 μl / min and an injection volume of 25 μl; using Selected Reaction Monitoring Mode (SRM) (mass spectrometry conditions: electrospray Ion source, negative ion ionization (ESI-) mode, ion source temperature 300°C, capillary voltage 3000V, sheath gas flow rate 40L / min, auxiliary gas flow rate 15L / min, capillary temperature 350°C, collision energy 18ev); m / z161.1 is the quantitative ion, and the reference retention time of aminopyralid is 15.5min (attached figure 1 ).

[0054] Treat...

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Abstract

The invention discloses a method for detecting aminopyralid pesticide residues in barley. The method comprises the following steps: preparing a sample, extracting, purifying and concentrating, obtaining a standard curve under a certain chromatographic condition and a certain mass spectrum condition and performing final detection. In the method, with methanol as an extracting solution, a small strongly-polar SPE (solid phase extraction) column is selected for purification; liquid chromatography-tandem triple quadrupole mass spectrometry is used for detection, state requirements on quality control during pesticide residue analysis can be met in aspects of accuracy, precision and recycling rate; the detection limit in the method can meet aminopyralid supervising requirements of GB 2763-2014.

Description

technical field [0001] The invention relates to an abbreviation process for pesticide residues, in particular to a detection method for aminopyralid pesticide residues in barley. Background technique [0002] Aminopyralid (aminopyralid), whose chemical name is 4-amino-3,6-dichloropyridine-2-carboxylic acid, is a synthetic hormone-type herbicide of pyridine carboxylic acid, widely used in mountains, grasslands, planting Weed control in land and non-cultivated land, long-lasting agent; in the new version of "National Food Safety Standard Food Maximum Residue Limits of Pesticides GB2763-2014", aminopyralid is one of the 65 newly added pesticides. (barley, barley, oats, triticale) the maximum residue limit is 0.1mg / kg, the standard has been implemented since August 1, 2014, after searching, there is no standard and literature report on the detection of this pesticide. When aminopyralid is used on the land where crops are planted, it is often sprayed on the crops to a greater or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 张文国黄键赵炜施锦辉郭桂萍葛卜峰王金娟
Owner NANTONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF THE PEOPLES REPUBLIC OF CHINA