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Detection method for epichlorohydrin and application thereof

A technology of epichlorohydrin and a detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as inapplicability, and achieve the effect of simple operation and high detection accuracy

Inactive Publication Date: 2019-05-14
WUHAN CONFORM PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by this invention is to overcome the defect that the detection method of epichlorohydrin in the prior art is not suitable for the detection of the content of epichlorohydrin in the mixture containing propranolol hydrochloride and epichlorohydrin, Thereby providing a kind of detection method and application of epichlorohydrin

Method used

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  • Detection method for epichlorohydrin and application thereof
  • Detection method for epichlorohydrin and application thereof
  • Detection method for epichlorohydrin and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1. Instruments: Agilent 7890B gas chromatograph, FID detector, Agilent 7697A headspace sampler, electronic balance

[0052] 2. Sample configuration

[0053] Accurately weigh the appropriate amount of epichlorohydrin, and dilute it with water to an epichlorohydrin solution containing 1.74 μg of epichlorohydrin per 1 mL;

[0054] Precisely pipette 5mL into a 20mL headspace bottle, seal it with a gland, and use it as a control solution;

[0055] Accurately weigh 0.5 g of propranolol hydrochloride raw material, put it in a 20 mL headspace bottle, accurately pipette 5 mL of epichlorohydrin reference solution, press the cap and shake well, and use it as the test solution.

[0056] 3. Experimental conditions

[0057] The chromatographic column is DB-624 (30m×0.32mm×1.8μm);

[0058] The carrier gas is nitrogen and the flow rate is 3mL / min;

[0059] The air flow rate is 300mL / min;

[0060] The hydrogen flow rate is 30mL / min;

[0061] Injection port 200°C;

[0062] FID detec...

Embodiment 2

[0082] Referring to the operation of Example 1, the only difference is that the headspace equilibrium temperature is 58° C., and the equilibrium time is 10 minutes. See attached chromatogram image 3 ~ attached Figure 4 .

[0083] The chromatographic data of the contrast solution are shown in Table 3 below:

[0084] table 3

[0085]

[0086] Peak number 1 represents epichlorohydrin.

[0087] The chromatographic data of the test solution are shown in Table 4 below:

[0088] Table 4

[0089]

[0090] Peak number 1 represents epichlorohydrin.

[0091] The results show that in this method, the limit concentration of epichlorohydrin responds well, and the recovery rate of epichlorohydrin in the test solution is 89% calculated by the external standard method.

Embodiment 3

[0093] Referring to the operation of Example 1, the only difference is that the headspace equilibrium temperature is 62° C., and the equilibrium time is 10 minutes.

[0094] See attached chromatogram Figure 5 ~ attached Image 6 .

[0095] The chromatographic data of contrast solution are shown in table 5 below:

[0096] table 5

[0097]

[0098] Peak number 1 represents epichlorohydrin.

[0099] The chromatographic data of the test solution are shown in Table 6 below:

[0100] Table 6

[0101]

[0102] Peak number 1 represents epichlorohydrin.

[0103] The results show that in this method, the limit concentration of epichlorohydrin responds well, and the recovery rate of epichlorohydrin in the test solution is 80% calculated by the external standard method.

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Abstract

The invention discloses a detection method for epichlorohydrin and application thereof. The detection method is characterized in that a sample containing propranolole hydrochloride and epichlorohydrinis detected by a headspace gas chromatography method, wherein in the headspace gas chromatography method, the headspace balance temperature is 55 to 62 DEG C, and the headspace balance time is 5 to 15 minutes. The detection method is easy to operate, stable and effective, does not need excessive samples, has high detection accuracy for the content of the epichlorohydrin in a propranolole hydrochloride raw material containing the epichlorohydrin, and is suitable for controlling the quality of the propranolole hydrochloride raw material in industrial production.

Description

technical field [0001] The invention relates to a detection method and application of epichlorohydrin. Background technique [0002] Propranolol hydrochloride, as shown in the following formula, has a chemical name of 1-isopropylamino-3-(l-naphthyloxy)-2-propanol hydrochloride, which is a non-selective beta-receptor blocker, Block myocardial β receptors, and have antagonistic effects on both β1 and β2 receptors. It is clinically used to treat diseases such as hypertension, angina pectoris and arrhythmia, and the drug effect is good. [0003] [0004] The synthetic technique of propranolol hydrochloride mainly takes 1-naphthol and epichlorohydrin as starting raw materials at present, through intermediate 1-naphthyl glycidyl ether, and then through intermediate 1-isopropylamino-3 -(1-naphthyloxy)-2-propanol reacts with hydrochloric acid to generate propranolol hydrochloride. Among them, epichlorohydrin is likely to be introduced into the finished product as a starting ma...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/68
Inventor 周小顺牟东升余雪峰李进贺容丽别彤
Owner WUHAN CONFORM PHARMA CO LTD
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