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Method for measuring and analyzing content of chiral isomers in epichlorohydrin

A technology for epichlorohydrin and chiral isomers, applied in the field of medicine, can solve the problems of difficulty in direct determination, specificity, sensitivity, method precision and repeatability, and inability to provide reliable analysis results.

Pending Publication Date: 2022-06-28
SHANGHAI AOBO PHARMTECH INC LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is difficult to directly measure it by gas phase, liquid chromatography, etc.
[0008] At present, the method for determining the content of chiral isomers of epichlorohydrin adopts the classic optical rotation method or gas chromatography, which has great defects in specificity, sensitivity, method precision and repeatability, and cannot provide reliable analysis results.

Method used

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  • Method for measuring and analyzing content of chiral isomers in epichlorohydrin
  • Method for measuring and analyzing content of chiral isomers in epichlorohydrin
  • Method for measuring and analyzing content of chiral isomers in epichlorohydrin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Instruments and Conditions:

[0039] High performance liquid chromatograph: Agilent 1260infinity, DAD detector.

[0040] Chromatographic column: DAICEL Chiralpak IC, 5μm, 250*4.6mm

[0041] Flow rate: 1.0 mL / min. Column temperature: 20°C. Mobile phase A: 0.1% diethylamine n-hexane solution, mobile phase B: ethanol, injection volume: 10 μL, UV wavelength: 250 nm. Elute according to the following gradient program.

[0042] time / min Mobile phase A / % Mobile phase B / % 0.0 96 4 15 96 4 15.1 70 30 30 70 30 30.1 96 4 50 96 4

[0043] Experimental steps:

[0044] 1) Diluent: use chromatographic grade ethanol as the diluent.

[0045] 2) Derivative solution: quantitatively prepare 2.5 mg / mL mercaptopyridine solution with diluent.

[0046] 3) Sensitivity stock solution: Accurately weigh 10.0 mg R-epichlorohydrin and 10.0 mg S-epichlorohydrin, accurately weigh them in a 10 mL volumetric flask, dissolve with diluent, and se...

Embodiment 2

[0051] Instruments and Conditions:

[0052] High performance liquid chromatograph: Agilent 1260infinity, DAD detector.

[0053] Chromatographic column: DAICEL Chiralpak IC, 5μm, 250*4.6mm

[0054] Flow rate: 1.0 mL / min. Column temperature: 20°C. Mobile phase A: 0.1% diethylamine n-hexane solution, mobile phase B: ethanol, injection volume: 10 μL, UV wavelength: 250 nm. Elute according to the following gradient program.

[0055] time / min Mobile phase A / % Mobile phase B / % 0.0 96 4 15 96 4 15.1 70 30 30 70 30 30.1 96 4 50 96 4

[0056] Experimental steps:

[0057] 1) Diluent: use chromatographic grade ethanol as the diluent.

[0058] 2) Derivative solution: quantitatively prepare 2.5 mg / mL mercaptopyridine solution with diluent.

[0059] 3) R-epichlorohydrin sample solution: accurately weigh 10.0 mg of R-epichlorohydrin in a 10.0 ml volumetric flask, and dilute to the mark with diluent. Dissolve 500 μL of diluent and 500...

Embodiment 3

[0061] Instruments and Conditions:

[0062] High performance liquid chromatograph: Agilent 1260infinity, DAD detector.

[0063] Chromatographic column: DAICEL Chiralpak IC, 5μm, 250*4.6mm

[0064] Flow rate: 1.0 mL / min. Column temperature: 20°C. Mobile phase A: 0.1% diethylamine n-hexane solution, mobile phase B: ethanol, injection volume: 10 μL, UV wavelength: 250 nm. Elute according to the following gradient program.

[0065] time / min Mobile phase A / % Mobile phase B / % 0.0 96 4 15 96 4 15.1 70 30 30 70 30 30.1 96 4 50 96 4

[0066] Experimental steps:

[0067] 1) Diluent: use chromatographic grade ethanol as the diluent.

[0068] 2) Derivative solution: quantitatively prepare 2.5 mg / mL mercaptopyridine solution with diluent.

[0069] 3) S-epichlorohydrin stock solution: accurately weigh 10.0 mg of S-epichlorohydrin to be tested in a 10.0 mL volumetric flask, and dilute to the mark with diluent.

[0070] 4) R-epichl...

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Abstract

The invention discloses a method for determining and analyzing the content of chiral isomers in epoxy chloropropane. According to the method, chemical derivation is combined with a high performance liquid chromatography-photodiode array detector to determine the content of trace chiral isomers in R-epoxy chloropropane. Compared with the prior art, the analysis method has the characteristics of good reproducibility, high sensitivity, suitability for microanalysis and the like.

Description

technical field [0001] The invention relates to the determination of the content of trace chiral isomers in epichlorohydrin by chemical derivatization combined with a high-efficiency gas chromatography headspace-hydrogen flame ion detector. The method can better control the content of trace chiral isomers in epichlorohydrin, provides quality assurance for pharmaceutical raw materials, and belongs to the technical field of medicine. [0002] technical background [0003] Epichlorohydrin, chemical name 1-chloro-2,3-epoxypropane. [0004] Epichlorohydrin is an organic compound with the chemical formula C 3 H 5 ClO, a colorless liquid, an organic compound with a chloroform-like odor, is an important organic synthesis raw material and intermediate. It is often used as a common raw material for pharmaceutical and chemical products. Because its molecular structure contains a chiral center, it contains chiral isomers. [0005] The structure of epichlorohydrin is as follows: [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74G01N2030/324
Inventor 祝广山邱学艳顾虹安建国胡素招黄文静张丽娟张南南于波谭越王秋峰陈茜
Owner SHANGHAI AOBO PHARMTECH INC LTD