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Polar pesticide determination using chromatography

A chromatographic method and pesticide technology, applied in the field of anionic polar pesticides and polar pesticides

Inactive Publication Date: 2019-10-25
WATERS TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Risk factors for public health from pesticide residues from the use of plant protection products on crops used in food or feed production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] The methods of the present disclosure were used to determine polar pesticides in orange juice. Tested for the following polar pesticides: glyphosate, AMPA, glufosinate, perchlorate, ethephon, aluminum triethronate, maleic hydrazide, phosphonic acid, and chlorate. Table 2 shows the MS conditions for each of these polar pesticides. Orange juice samples were extracted using the QuPPe extraction method. A 10 mL aliquot of the sample was acidified using 10 mL of 1% formic acid in MeOH. The mixture was shaken for 10 minutes and centrifuged at 4000 rpm for 5 minutes. The mixture was then filtered using a 0.45 micron filter. Filtered sample extracts were spiked with approximately 250 ppb of each pesticide before introduction to the chromatographic system.

[0088] Table 2: Example 1MS Conditions

[0089]

[0090]

[0091] Chromatographic systems include commercially available from Waters Corporation, Milford, MA, USA. system. Columns are commercially available f...

Embodiment 2

[0101] Initial conditions and analytical methods for the analysis of polar pesticides in extracted food matrices are described.

[0102] Column Equilibration: Before installing the column, the LC system can be acid washed to remove metal ions. When the column is initially received, the column can be flushed for 50 column volumes in 50% acetonitrile / 50% (LCMS grade water). For example, for a 3.0 mm x 150 mm column, 1 column volume equals 1.06 mL. At a flow rate of 0.45 mL / min, it takes 2.35 min to fill one column volume. Equilibration may include initial mobile phase conditions for 20 column volumes before the first injection is performed.

[0103] LC conditions can be the same as those used in Example 1. Exemplary gradients are provided in Table 5.

[0104] Table 5: Example 2 gradient conditions

[0105]

[0106]

[0107] LC conditions can be the same as those used in Example 1. Gradients can be as provided in Table 5. The sample may include various polar pestic...

Embodiment 3

[0122] Samples of onions and spinach labeled organic were purchased from retail outlets, homogenized, and extracted using the EURL polar pesticide rapid extraction method.

[0123] Table 8: Example 3, Liquid Chromatography System

[0124] LC system ACQUITY UPLC I-Class Chromatographic column Torus DEA 2.1×100mm mobile phase A 50mM ammonium formate pH 2.9 mobile phase B 0.9% formic acid in acetonitrile strong wash 10:90 acetonitrile: water weak wash 90:10 acetonitrile: water Column temperature 50℃ Sample temperature 10℃ Injection volume 10 μL flow rate 0.5mL / min operation hours 20 minutes

[0125] Table 9: Example 3 MS instrument settings

[0126]

[0127]

[0128] The mobile phase gradients used are listed in Table 10. The gradient was held at 320 μL.

[0129] Table 10: Example 3 mobile phase gradient

[0130] Time (Min) The first solvent (%) Second solvent (%) cu...

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Abstract

The present disclosure relates to the determination of pesticides, e.g., polar pesticides, in a sample using chromatography. The present disclosure can provide direct analysis of polar pesticides, including anionic polar pesticides, using high performance liquid chromatography. The polar pesticides are sufficiently retained and resolved to allow for multiple polar pesticide determinations in a single analysis.

Description

[0001] Cross References to Related Applications [0002] This application claims U.S. Provisional Application No. 62 / 468,700, filed March 8, 2017, entitled "Polar Pesticide Determination Using Chromatography," and the filed November 6, 2017, entitled "Polar Pesticide Determination Using Chromatography." The benefit and priority of U.S. Provisional Application No. 62 / 582,237, "Pesticide Determination Using Chromatography," the contents of each of which are incorporated herein by reference in their entirety. technical field [0003] The present disclosure relates to the determination of pesticides, such as polar pesticides, in a sample using chromatography. The present disclosure may provide for direct analysis of polar pesticides, including anionic polar pesticides, using, for example, liquid chromatography and / or high performance liquid chromatography. Background technique [0004] Pesticide residues from the use of plant protection products on crops used for food or feed p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884G01N33/184G01N30/72G01N30/74G01N30/8631G01N2030/027
Inventor D.D.沙赫J.N.费尔蔡尔德E.罗斯B.伍伊茨
Owner WATERS TECH CORP
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