Detecting method of ethene diamine and method for detecting ethene diamine in sitagliptin phosphate intermediate XG-SM2

A technology of XG-SM2 and detection method, which is applied in the field of analytical chemistry, can solve problems such as the detection of ethylenediamine that have not been seen before, and achieve the effect of good quality, high sensitivity and strong operability

Active Publication Date: 2019-04-19
TONGHUA DONGBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] So far, there have been no reports on the detection of ethylenediamine in sitagliptin phosphate intermediate XG-SM2 by ion chromatography

Method used

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  • Detecting method of ethene diamine and method for detecting ethene diamine in sitagliptin phosphate intermediate XG-SM2
  • Detecting method of ethene diamine and method for detecting ethene diamine in sitagliptin phosphate intermediate XG-SM2
  • Detecting method of ethene diamine and method for detecting ethene diamine in sitagliptin phosphate intermediate XG-SM2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Example 1: Selection of mobile phase

[0086] The purpose of this example is to investigate the influence of methanesulfonic acid as the mobile phase, its concentration and the elution procedure on the separation and detection of ethylenediamine.

[0087] Except for the mobile phase, the following chromatographic conditions were used in this example

[0088] Ion chromatograph: Thermo Dionex Aquion type ion chromatograph;

[0089] Chromatographic column: Thermo Dionex IonPac CS12A cation column (4mm*250mm);

[0090] Guard column: Thermo Dionex IonPac CG12 guard column (4mm*50mm);

[0091] Flow rate: 1.0ml / min;

[0092] Column temperature: 28-35℃;

[0093] Detector: Conductivity detector

[0094] Injection volume: 25μl.

[0095] In this embodiment, the ethylenediamine reference substance solution is used for determination. The preparation method of the ethylenediamine reference substance solution is as follows:

[0096] Accurately measure an appropriate amount of ethylenediamine, dissolv...

Embodiment 2

[0138] Example 2 Methodological study of the ethylenediamine detection method of the present invention

[0139] On the basis of Example 1, a detection method for ethylenediamine was established, specifically:

[0140] I. Chromatographic conditions:

[0141] Ion chromatograph: Thermo Dionex Aquion type ion chromatograph;

[0142] Chromatographic column: Thermo Dionex IonPac CS12A cation chromatographic column (4mm*250mm);

[0143] Guard column: Thermo Dionex IonPac CG12 guard column (4mm*50mm);

[0144] Mobile phase: 40mmol / L methanesulfonic acid (prepared with ultrapure water)

[0145] Flow rate: 0.7-1.4ml / min, preferably 1.0ml / min;

[0146] Column temperature: 28-35℃;

[0147] Detector: Conductivity detector

[0148] Injection volume: 25μl.

[0149] II. Preparation of reference solution:

[0150] Accurately measure an appropriate amount of ethylenediamine, dissolve it with ultrapure water and dilute it to a solution containing about 2μg ethylenediamine per 1ml, and get it;

[0151] Preparatio...

Embodiment 3

[0194] Example 3 Use the method of the present invention to determine two batches of sitagliptin phosphate intermediate XG-SM2

[0195] The specific measurement results are as follows:

[0196] Weigh appropriate amount of sitagliptin phosphate intermediate XG-SM2, dissolve and dilute with ultrapure water to make a solution containing about 1mg per 1ml, as a reference solution; accurately measure an appropriate amount of ethylenediamine and dilute with ultrapure water As a control solution, a solution containing about 2μg per 1ml. Under the chromatographic conditions described in Example 2, 25 μl of the reference solution was accurately measured and injected into the ion chromatograph to adjust the sensitivity of the instrument so that the chromatographic peak height of the main component was 10%-20% of the full scale. Then accurately measure 25μl each of the test solution and the reference solution, inject the samples separately, inject into the ion chromatograph, record the chr...

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Abstract

The invention provides a detecting method of ethene diamine based on ion chromatography. A chromatogram condition is characterized in that a chromatographic column is a Thermo Dionex IonPac CS12A cation chromatographic column, 250mm*4mm; a detector is a conductivity detector; a mobile phase is 40mmol/l methane sulfonic acid; the flow velocity is 0.7ml/min - 1.4ml/min; the column temperature is 28-35 DEG C; and the sample entering amount is 25 ul. The lowest linear detection concentration of the detecting method is 0.4[mu]g/ml. The lowest detection concentration of the method with a signal-to-noise ratio of 3:1 is 0.06 [mu]g/ml. The invention further provides application of the detecting method in sitagliptin phosphate intermediate XG-SM2 impurity detection.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a method for detecting ethylenediamine and a method for detecting ethylenediamine in sitagliptin phosphate intermediate XG-SM2. Background technique [0002] Diabetes mellitus is a chronic comprehensive disease dominated by glucose metabolism disorders, including insulin-dependent diabetes (type I diabetes), non-insulin-dependent diabetes (type II diabetes, accounting for 90%) and gestational diabetes. The Global Diabetes Map (8th edition) released by the International Diabetes Federation shows that the global prevalence of diabetes (20-79 years old) in 2017 is about 8.8%, and there are about 425 million adult diabetic patients. By 2045, this number may reach 629 million. [0003] China has the largest number of diabetic patients, accounting for about a quarter of the world's total. Diabetes, as a high-incidence chronic disease, has the characteristics of irreversible di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/96G01N30/06
CPCG01N30/02G01N30/06G01N30/96
Inventor 冷春生王广祁宁科权王健盛永强
Owner TONGHUA DONGBAO PHARMA
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