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An ion chromatography method for the simultaneous determination of main component mepiperium and its impurity n-methylpiperidine in pesticides

A technology of methylpiperidine and methylpiperium, applied in the field of analytical chemistry, can solve the problems of inability to use liquid chromatography ultraviolet detectors for detection, distinction, and inability to achieve qualitative analysis, and achieves the effect of meeting process control requirements

Active Publication Date: 2016-01-06
ANHUI WAYEE SCI & TECH CO LTD
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  • Abstract
  • Description
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Problems solved by technology

[0003] The existing measuring method of mepiperium and N-methylpiperidine is gravimetric titration, but because the structure of mepiperium and N-methylpiperidine is very similar, there is only a methyl difference in the structure, so weight Titration cannot distinguish between these two substances, that is, qualitative analysis cannot be achieved, so it is urgent to find a means to solve the qualitative problem of mepiperium and N-methylpiperidine, and chromatography is a method for qualitative and quantitative analysis of known substances. An ideal means of quantification, because there is no chromogenic group in the structure of mepiperium and N-methylpiperidine, it cannot be detected by liquid chromatography with a UV detector; under acidic conditions, mepiperium and N-methylpiperidine Pyridine binds hydrogen ions in solution to form a positively charged cation with a conductance response

Method used

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  • An ion chromatography method for the simultaneous determination of main component mepiperium and its impurity n-methylpiperidine in pesticides
  • An ion chromatography method for the simultaneous determination of main component mepiperium and its impurity n-methylpiperidine in pesticides
  • An ion chromatography method for the simultaneous determination of main component mepiperium and its impurity n-methylpiperidine in pesticides

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Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: Optimization of chromatographic conditions

[0035] When a single 2mmol / L methanesulfonic acid solution was used as the eluent, it was found that N-methylpiperidine and Mg 2+ , Ca 2+ Inseparable from mepiperium, which cannot be resolved by increasing or decreasing the concentration of the methanesulfonic acid solution. Therefore, it is necessary to add an organic solvent to adjust the interaction between N-methylpiperidine and mepiperium and the chromatographic column filler, so as to realize that N-methylpiperidine and Mg 2+ , Ca 2+ Separation from methylpiperium. It is found through experiments that after adding 1.0mmol / L crown ether in the 2mmol / L methanesulfonic acid eluent, N-methylpiperidine and Mg 2+ , Ca 2+ Baseline separated from mepiperium, see figure 1 .

Embodiment 2

[0036] Embodiment 2: Analysis of N-methylpiperidine and mepiperium mixed standard solution

[0037] (1) Repeatability

[0038] The standard mixed solution of the same concentration was continuously injected 6 times to obtain the chromatograms of N-methylpiperidine and mepiperium (see figure 2 ), and the relative standard deviations of their peak areas were 0.81% and 0.80%, respectively.

[0039] (2) Linear relationship

[0040] For the prepared linear solution of N-methylpiperidine and mepiperium, perform injection analysis according to the injection sequence from low concentration to high concentration, and obtain the peak areas of N-methylpiperidine and mepiperium at different concentrations , taking the concentration (mg / L) of the ion to be measured as the abscissa respectively, and taking its peak area as the ordinate to plot, obtain the working curve of N-methylpiperidine and mepiperium, attach respectively image 3 with Figure 4 .

Embodiment 3

[0041] Embodiment 3: the mensuration of the content of N-methylpiperidine and mepiperium in the pesticide

[0042] Under the selected chromatographic conditions, the actual sample is detected to obtain the chromatogram of the simultaneous detection of N-methylpiperidine and mepiperium, see the attached Figure 5 , N-methylpiperidine and mepiperium in the actual sample were quantified according to the external standard method, and the contents of N-methylpiperidine and mepiperium in the pesticide were obtained, as shown in Table 1. In the sample, N-methylpiperidine and mepiperium-0.1 and 5.0mg / L standard solutions were added respectively, and the recovery rate test was carried out by the method of adding standard. The recovery rate results are attached in Table 1.

[0043] The content detection result of table 1N-methylpiperidine and mepiperium

[0044]

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Abstract

The invention discloses an ion chromatography method for simultaneously detecting mepiquat as a main component and N-methylpiperidine as an impurity in a pesticide. The ion chromatography method comprises the following steps of (1) setting the temperature of a column oven to be 45 DEG C; (2) setting the sample injection amount to be 25 microliters; (3) setting applied suppression current to be 15mA; (4) preparing leacheate; (5) preparing a standard solution; (6) analyzing a mixed standard solution with the N-methylpiperidine and the mepiquat; (7) diluting a liquid sample by 10,000 times as a sample solution for later use; (8) filtering a post-treated sample through a disposable needle type filter, putting the sample into an ion chromatography for analysis to measure the contents of negative N-methylpiperidine and mepiquat ions. The method disclosed by the invention is quick, simple and accurate, is suitable for quality control in pesticide production and can meet a requirement on technical control in a pesticide production process.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a method for quantitatively determining the contents of mepiperium, conventional cations and impurity N-methylpiperidine in pesticides, in particular to a chromatographic method for determining cations in pesticides. Background technique [0002] Methylpiperium, also known as benzedramine, is produced by high-pressure hydrogenation of pyridine under an aluminum-nickel alloy catalyst to produce hexahydropyridine (piperidine), and then reacting with formaldehyde and formic acid to obtain N-methylpiperidine , and further salted with methyl chloride under pressure to obtain mepiperium, namely N, N-dimethylpiperidine. [0003] The existing measuring method of mepiperium and N-methylpiperidine is gravimetric titration, but because the structure of mepiperium and N-methylpiperidine is very similar, there is only a methyl difference in the structure, so weight Titration cannot distingu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 焦霞盖学武赵春华
Owner ANHUI WAYEE SCI & TECH CO LTD
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