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Method for separating and detecting components in permethrin

A technology for permethrin and cis-permethrin, which is applied in the field of separation and detection of components in permethrin, can solve the problems of separation, separation of cis-permethrin and trans-permethrin, etc., and achieves a stable separation state , Accuracy, repeatability, and specificity

Active Publication Date: 2021-05-25
上海汉维生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2013, permethrin (Permethrin25:75) was included in European Pharmacopoeia 8.5, but its related substance detection method did not separate cis-permethrin from trans-permethrin, nor did it separate other known impurities Construct separation, there is room for further improvement

Method used

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  • Method for separating and detecting components in permethrin
  • Method for separating and detecting components in permethrin
  • Method for separating and detecting components in permethrin

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Embodiment

[0026] The method for separating and detecting each component in permethrin in this embodiment adopts gas chromatography for separation and detection, and uses 100% concentration of dimethylpolysiloxane as a capillary chromatographic column of the stationary liquid, and the capillary chromatographic column is J&W HP-5MS Model, the inner diameter is 0.25mm, the length is 30m, the film thickness is 0.25μm, or a chromatographic column with equivalent performance. The detector is a hydrogen flame ionization detector, the inlet temperature is 250°C, the detector temperature is 270°C, the injection volume is 1 μl, the split ratio is 15:1, the carrier gas is nitrogen, and the nitrogen flow rate is 3.0ml / min , the diluent is methanol.

[0027] Heating program: the initial column temperature is 125°C, maintained for 2 minutes, then raised to 235°C at a rate of 10°C / min, maintained for 15 minutes,

[0028] Solution preparation:

[0029] The test solution (5mg / ml): Take homemade permet...

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Abstract

The invention relates to a method for separating and detecting components in permethrin. The permethrin comprises the following components: cis-permethrin, trans-permethrin, an impurity B, an impurity C and an impurity G, the impurity B is methyl dichlorochrysantheate, the impurity C is m-phenoxybenzyl alcohol, the impurity G is 3-(phenoxy phenyl) methyl-(1RS, 2RS)-2-(chloroethynyl)-3, 3-dimethyl cyclopropyl-1-carboxylic acid ester. According to the method, a gas chromatographic method is adopted for separation and detection, a capillary chromatographic column with 100% concentration of dimethyl polysiloxane as a stationary liquid is used, and the heating procedure of the capillary chromatographic column is as follows: the initial column temperature is 125 DEG C and maintained for 2 min, then the temperature is raised to 235 DEG C at the rate of 10 DEG C / min and maintained for 15 min, a detector is a hydrogen flame ionization detector, the temperature of a sample inlet is 230-270 DEG C, and the detection time is 30-50 min. The temperature of a detector is 250-290 DEG C, and the diluent is methanol. The method for separating and detecting the components in the permethrin can well separate the components in the permethrin, and has the advantages of high sensitivity, strong specificity, stable separation state and the like.

Description

technical field [0001] The invention relates to a method for separating and detecting components in permethrin, belonging to the technical field of chemical analysis. Background technique [0002] Permethrin, also known as dichlorophenyl ether, insecticide, permethrin, is a low-toxic broad-spectrum insecticide. In 1949, the American Carbon Chemical Company put into production and commercialized the first generation of pyrethroid insecticides. Elliott Michael (1976, twice awarded the Queen's Award in 1980) solved the problem of the instability of the first generation of pyrethrins to light, and completed the first generation of pyrethrins (only for indoor pest control, livestock ectoparasites and stored grain pests) Shift to second-generation pyrethrins for agricultural and forestry pests. Permethrin is the main species of the second-generation pyrethroids, and its chemical name is (1R,S)-cis,trans-2,2-dimethyl-3-(2,2-dichlorovinyl )-cyclopropanecarboxylic acid-3-phenoxybe...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/68
CPCG01N30/02G01N30/68G01N2030/025Y02A50/30
Inventor 韩志宏朱颐雯霍丽萍
Owner 上海汉维生物医药科技有限公司
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