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Method for detecting purity of 3-methylamino-1,2-propylene glycol with capillary column method

A capillary column and methylamine-based technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low recovery rate, undetectable content, narrow detection range and other problems of standard addition test, and achieve wide detection range and short detection time. Short, easy-to-use effects

Inactive Publication Date: 2016-10-12
青岛惠国新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) 3-methylamino-1,2-propanediol products contain 2-methylamino-1,3-propanediol, 1,3-dimethylamino-propanol, N,N-(2,3- Dihydroxypropyl) methylamine [structural formula CH 3 N(CH 2 CHOHCH 2 Oh) 2 ], glycerin, polymerized glycerol (generally the degree of polymerization is 2), and other impurities, the content of these five impurities cannot be detected at all in the analysis and detection methods provided by the prior art;
[0006] (2) The existing analytical methods are not linear when doing linear equations, the recovery rate of the standard addition test is low, the detection range is narrow, and the detection precision is poor;
[0007] (3) The prior art uses trifluoroacetic anhydride to derivatize the sample first, and then conducts detection and analysis. It takes at least 50-60 minutes from sampling to obtaining the chromatographic detection results. The detection time is long and the work efficiency is low.

Method used

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  • Method for detecting purity of 3-methylamino-1,2-propylene glycol with capillary column method
  • Method for detecting purity of 3-methylamino-1,2-propylene glycol with capillary column method
  • Method for detecting purity of 3-methylamino-1,2-propylene glycol with capillary column method

Examples

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Embodiment 1

[0033] Example 1 The method for detecting the purity of 3-methylamino-1,2-propanediol by capillary column method

[0034] Include the following steps:

[0035] 1. Sample preparation

[0036] Dissolve about 0.1 mL of 3-methylamino-1,2-propanediol in 2 mL of chromatographically pure methanol, fully dissolve and set aside.

[0037] 2. Setting of chromatographic conditions

[0038] (1) Chromatograph (FL9790 produced in Wenling, Zhejiang);

[0039] (2) Detector (FID), hydrogen flame ionization detector;

[0040] (3) Agilent gas chromatography column, DB-1701 (30m×0.32mm×0.5um) quartz capillary column;

[0041] (4) Column temperature, 240°C; injection volume 0.2µL, split injection, split ratio 18:1; carrier gas nitrogen, flow rate 42mL / min; air flow rate 455 mL / min; hydrogen 43mL / min;

[0042] (5) Temperature of vaporization chamber, 283°C;

[0043] (6) Detector temperature, 282°C.

[0044] 3. Detection operation

[0045] Turn on the power of the chromatograph and turn it on...

Embodiment 2

[0051] Example 2 The method for detecting the purity of 3-methylamino-1,2-propanediol by capillary column method

[0052] Adopt the method of embodiment 1, only change column temperature and vaporization chamber temperature, change to:

[0053] Column temperature: 265°C;

[0054] Vaporization chamber temperature: 315°C.

[0055] Table 2 adopts the detection result corresponding to the detection method of embodiment 2

[0056]

[0057]In Table 2, according to the retention time, peak number 1 is 1,3-dimethylamino-propanol, or 2-methylamino-1,3-propanediol, or 1,3-dimethylamino-propanol Mixture with 2-methylamino-1,3-propanediol; peak number 2 is 3-methylamino-1,2-propanediol; peak number 3 is glycerol or glycerol and N,N-( A mixture of 2,3-dihydroxypropyl)methylamine; peak number 4 is a mixture of polymerized glycerol (generally, the degree of polymerization is 2) or polymerized glycerol and N,N-(2,3-dihydroxypropyl)methylamine;

[0058] As can be seen from Table 2, the ...

Embodiment 3

[0059] Example 3 Method for detecting the purity of 3-methylamino-1,2-propanediol by capillary column method

[0060] Adopt the method of embodiment 2, only change the flow rate of carrier gas, the flow rate of carrier gas is reduced from 42mL / min to 33ml / min.

[0061] Table 3 adopts the detection result corresponding to the detection method of embodiment 3

[0062]

[0063] Among them, in Table 3, peak number 2 is 3-methylamino-1,2-propanediol; due to poor separation effect, peak number 1 is 1,3-dimethylamino-propanol, or 2-methylamino -1,3-propanediol, or a mixture of 1,3-dimethylamino-propanol and 2-methylamino-1,3-propanediol; after adjusting the operating conditions, the three substances with high boiling points were completely separated, and the peak No. 3 is N,N-(2,3-dihydroxypropyl)methylamine; peak No. 4 is glycerol at 3.892min; peak No. 5 is polymerized glycerin (the degree of polymerization is generally 2);

[0064] It can be seen from Table 3 that the three co...

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Abstract

The invention provides a method for detecting purity of 3-methylamino-1,2-propylene glycol with a capillary column method. The method comprises steps of sample preparation and chromatographic condition setting, wherein for the chromatographic condition setting, the temperature of a detector is 282-310 DEG C. According to the analysis method, the content of impurities such as 2-methylamino-1,3-propylene glycol, 1,3-dimethylamino-propyl alcohol, N,N-(2,3-dihydroxypropyl) methylamine, glycerol, polyglycerol (with polymerization degree of 2 generally) and the like generated in synthesis of 3-methylamino-1,2-propylene glycol can be detected while the content of 3-methylamino-1,2-propylene glycol is detected in the industry for the first time. The analysis method is wide in detection range, and the linearity is good when the detected content of 3-methylamino-1,2-propylene glycol is in a range of 10-50 mg; a recovery rate experiment is performed on the detection method, and the average recovery rate is 99.5%-99.6%.

Description

technical field [0001] The invention relates to a method for detecting the purity of 3-methylamino-1,2-propanediol by a capillary column method, and belongs to the technical field of product instrument analysis. Background technique [0002] 3-Methylamino-1,2-propanediol is an important raw material for the synthesis of low-osmotic non-ionic contrast agent iopromide, and its purity, quantity and content of impurities directly affect the purity and clinical application of the final product iopromide . In the synthesis reaction of iopromide, if the impurity content of 3-methylamino-1,2-propanediol is too high or the impurity components are more, it will react with the intermediate 3-(2-methoxy)acetamido]-5 -(2,3-Dihydroxy-n-propylcarbamoyl)-2,4,6-triiodobenzoyl chloride undergoes a variety of side reactions to produce a variety of complex products with different structures or unknown structures, which may cause allergies when injected into the body Symptoms vary in severity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025
Inventor 郭祥荣翟浩桐王璀庄青张恭孝杨荣华刘梅王芳汪海孟宪锋
Owner 青岛惠国新材料科技有限公司