Gas chromatographic measurement method for 2-isopropyl-6-methyl-4-hydroxy pyrimidine in intermediate

A technology of hydroxypyrimidine and gas chromatography, which is applied in the field of gas chromatography determination of 2-isopropyl-6-methyl-4-hydroxypyrimidine in intermediates, can solve the problem of poor reproducibility and accuracy of determination, chromatographic Solve problems such as unsuitable conditions for column use, achieve the effect of fast and convenient method, stable and accurate data

Inactive Publication Date: 2018-08-28
JIANGSU TAIJIE INSPECTION TECH
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Problems solved by technology

Regarding the analysis of hydroxypyrimidine, some literatures use ultraviolet spectrophotometry to measure its content, but due to the interference of raw material mechanism, the reproducibility and accuracy of determination are poor; there are literatures that use gas chromatography, but due to the relatively high boiling point of hydroxypyrimidine , while the use conditions of the chromatographic column do not meet the conditions

Method used

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  • Gas chromatographic measurement method for 2-isopropyl-6-methyl-4-hydroxy pyrimidine in intermediate
  • Gas chromatographic measurement method for 2-isopropyl-6-methyl-4-hydroxy pyrimidine in intermediate
  • Gas chromatographic measurement method for 2-isopropyl-6-methyl-4-hydroxy pyrimidine in intermediate

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Experimental program
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Embodiment

[0040] 1 Instruments and reagents

[0041] 1. The instrument is as follows:

[0042] Gas chromatograph: HP-6890GC produced by Agilent, USA, hydrogen flame ion detector;

[0043] Chromatographic column: HP-FFAP (Crosslinked FFAP), 25m*0.32mm*0.52um;

[0044] Microsyringe: 10 μL.

[0045] 2. The reagents are as follows:

[0046] 2-isopropyl-6-methyl-4-hydroxypyrimidine standard substance, content 99%, Shanghai Merrill Chemical Technology Co., Ltd.;

[0047] Internal standard: triphenylmethane, 99%, Aladdin;

[0048] Methanol: analytically pure; (Sinopharm Group).

[0049] 2 Instrument debugging and determination of methods and control parameters

[0050] 1. Selection of methods and instruments

[0051] After repeated tests and screening, it is determined that the content of hydroxypyrimidine is determined by gas chromatography, which can quickly and accurately determine the content of hydroxypyrimidine in intermediates. At the same time, the analysis room has various spec...

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Abstract

The invention discloses a gas chromatographic measurement method for 2-isopropyl-6-methyl-4-hydroxy pyrimidine in an intermediate. According to the gas chromatographic measurement method, the intermediate is dissolved with a methanol solvent, and triphenylmethane is used as an internal standard substance, so that the 2-isopropyl-6-methyl-4-hydroxy pyrimidine is subjected to accurately quantitativedetection and analysis by using an HP-FFAP capillary column and a gas chromatograph with a hydrogen flame ionization detector and adopting an internal standard method; data are stable and accurate, and the method is quick and convenient. A variable coefficient of the method is 0.42%, the recycling rate is 99.22 to 100.32%, and the retention time is 2.306 min.

Description

technical field [0001] The invention belongs to the field of gas chromatography determination, in particular to a gas chromatography determination method of 2-isopropyl-6-methyl-4-hydroxypyrimidine in an intermediate. Background technique [0002] Hydroxypyrimidine is white powder, slightly soluble in water, relatively soluble in alcohol, ester, benzene and other organic solvents, and is an intermediate of organophosphorus pesticide diazinon and pharmaceutical products. Regarding the analysis of hydroxypyrimidine, some literatures use ultraviolet spectrophotometry to measure its content, but due to the interference of raw material mechanism, the reproducibility and accuracy of determination are poor; there are literatures that use gas chromatography, but due to the relatively high boiling point of hydroxypyrimidine , but the conditions of use of the chromatographic column do not meet the conditions. The invention adopts the HP-FFAP capillary column to directly analyze by ga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/60G01N30/68
CPCG01N30/02G01N30/60G01N30/68
Inventor 周树华林新艳
Owner JIANGSU TAIJIE INSPECTION TECH
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