Unlock instant, AI-driven research and patent intelligence for your innovation.

An LC-MS/MS method for the analysis of three phenoxycarboxylic acid herbicide residues in tobacco

A phenoxycarboxylic acid and LC-MS technology, which is applied in the direction of analyzing materials, measuring devices, and material separation, can solve the problems of underestimating the actual concentration, etc., and achieve the effects of reducing matrix effect, improving accuracy, and increasing adsorption

Active Publication Date: 2015-12-30
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
View PDF5 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ordinary pretreatment methods mostly directly use acidifying reagents to extract target compounds, and phenoxycarboxylic acid herbicides usually exist in the form of free acids, salts, or esters, and the detection of only acidifying reagents will eventually underestimate their actual concentration

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • An LC-MS/MS method for the analysis of three phenoxycarboxylic acid herbicide residues in tobacco
  • An LC-MS/MS method for the analysis of three phenoxycarboxylic acid herbicide residues in tobacco
  • An LC-MS/MS method for the analysis of three phenoxycarboxylic acid herbicide residues in tobacco

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0037] 1. Instruments and reagents:

[0038] Standards of 2,4,5-T, 2,4-D, dicamba and their methyl ester derivatives were purchased from Dr. Eh laboratory in Germany; deuterated 2,4,5-T, deuterated 2,4- D and deuterated dicamba standard products were purchased from Canadian CDN company.

[0039] Methanol (Pesticide Residue Grade, Korea DUKSAN Company); Dichloromethane (Pesticide Residue Grade, American J.T.Baker Company); Glacial Acetic Acid (HPLC Grade, American TEDIA Company); C18 (American Agilent Company); Anhydrous Magnesium Sulfate (Tianjin City Kemiou Chemical Reagent Co., Ltd.), should be burned at 650 ° C for 4 hours before use, and stored in a desiccator for later use; sodium hydroxide (Tianjin Chemical Reagent No. 3 Factory); concentrated sulfuric acid (Luoyang Haohua Chemical Reagent Co., Ltd.).

[0040] Liquid chromatography-tandem mass spectrometry (API4000, American AB Company); desktop high-speed refrigerated centrifuge (3-30k, American SIGMA Company); vortex...

example 2

[0056] As described in Example 1, another tobacco sample B was selected, and the measured contents of the three pesticide targets in the sample are shown in Table 4.

[0057] Table 4 Detection results of pesticide targets in sample B

[0058] serial number Chinese common name The content of pesticide target in the sample (mg / kg) 1 2,4,5-T 0.16 2 2,4-D not detected 3 Dicamba not detected

example 3

[0060] As described in Example 1, another tobacco sample C was selected, and the measured contents of the three pesticide targets in the sample are shown in Table 5.

[0061] table 5 Detection results of pesticide targets in sample C

[0062] serial number Chinese common name The content of pesticide target in the sample (mg / kg) 1 2,4,5-T not detected 2 2,4-D 0.34 3 Dicamba not detected

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
recovery rateaaaaaaaaaa
Login to View More

Abstract

An LC-MS / MS method for analyzing the residual amounts of three phenoxycarboxylic acid herbicides in tobacco is characterized in that: the analysis and determination are carried out by the following method: after the sample is infiltrated and hydrolyzed by NaOH solution, acidified with H2SO4, added Dichloromethane and internal standard were then vortex extracted, the extract was dehydrated with anhydrous MgSO4, purified with C18, and the supernatant was taken for determination by liquid chromatography-tandem mass spectrometry. The method of the invention improves the existing sample processing method, provides a cleaner upper solution, and reduces the maintenance of the instrument during use. Compared with the prior art, the method has the following excellent effects: "wetting the sample with water" is changed to "wetting the sample with NaOH aqueous solution", and the purpose of hydrolysis is achieved while infiltrating. Adding H2SO4 solution to adjust the pH value can convert all phenoxycarboxylates and esters into free acid forms for detection, which improves the accuracy of detection. Choosing dichloromethane as the extraction agent is more targeted than acetonitrile extraction and improves the extraction effect.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection in tobacco, and in particular relates to an LC-MS / MS method for analyzing the residual amount of three phenoxycarboxylic acid herbicides in tobacco. NaOH solution is added to tobacco samples and hydrolyzed by lye The process converts all phenoxycarboxylic acid herbicides in different forms such as acid, salt and ester into the form of salt, and then converts them all into free acid form by adjusting the pH value with sulfuric acid, and then extracts with dichloromethane, C18 Sorbent purification and determination by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Background technique [0002] Phenoxycarboxylic acid herbicides are by far the second largest selective herbicides in the world, and also the largest herbicides against broadleaf weeds in the world. Phenoxycarboxylic acid herbicides belong to low-toxic herbicides, but they have endocrine disrupting effects....

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 刘珊珊边照阳杨飞李中皓范子彦张洪非王颖张艳革唐纲岭胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT