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Free hydrazine detection method and application thereof in sitagliptin phosphate bulk drug impurity detection

A detection method and detector technology, which are applied in the field of analytical chemistry, can solve the problems of inability to perform quantitative determination, acetone toxicity, unfavorable environmental protection, etc., and achieve the effects of effective detection, short time and strong method specificity.

Inactive Publication Date: 2019-04-26
TONGHUA DONGBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the need for derivatization, this method is cumbersome to operate and takes a long time; and acetone has certain toxicity, which is not good for environmental protection
[0012] (4) Fluorescent probe technology: the Chinese invention patent with publication number CN106431986B discloses a method for detecting free hydrazine using fluorescent probe molecules, but this method can only achieve qualitative detection and cannot be quantitatively determined
[0014] However, in the prior art, there are also relevant reports on the detection of a very small amount of free hydrazine in the sitagliptin phosphate crude drug

Method used

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  • Free hydrazine detection method and application thereof in sitagliptin phosphate bulk drug impurity detection
  • Free hydrazine detection method and application thereof in sitagliptin phosphate bulk drug impurity detection
  • Free hydrazine detection method and application thereof in sitagliptin phosphate bulk drug impurity detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] Example 1 Choice of mobile phase

[0088] The purpose of this example is to investigate the influence of methanesulfonic acid as mobile phase, its concentration and elution procedure on the separation and detection of free hydrazine.

[0089] Except mobile phase, present embodiment all adopts following chromatographic conditions

[0090] Ion chromatograph: Thermo Dionex Aquion ion chromatograph;

[0091] Chromatographic column: Thermo Dionex IonPac CS12A (4mm*250mm);

[0092] Guard column: Thermo Dionex IonPac CG12 (4mm*50mm);

[0093] Flow rate: 1.0ml / min;

[0094] Column temperature: 28-35°C;

[0095] Cation suppressor CERS (4mm);

[0096] Detector: conductivity detector;

[0097] Injection volume: 25 μl.

[0098] Present embodiment all adopts hydrazine sulfate reference substance solution to measure, and the preparation method of hydrazine sulfate reference substance solution is:

[0099] Precisely measure an appropriate amount of hydrazine sulfate, dissolv...

Embodiment 2

[0156] Example 2 Methodological research on the free hydrazine detection method of the present invention

[0157] On the basis of Example 1, the detection method of free hydrazine has been established, specifically:

[0158] I. Chromatographic conditions:

[0159] Ion chromatograph: Thermo Dionex Aquion ion chromatograph;

[0160] Chromatographic column: Thermo Dionex IonPac CS12A (4mm*250mm);

[0161] Guard column: Thermo Dionex IonPac CG12 (4mm*50mm);

[0162] Mobile phase: 5mmol / L methanesulfonic acid (prepared with ultrapure water)

[0163] Flow rate: 0.8-1.3ml / min, preferably 1.0ml / min;

[0164] Column temperature: 28-35°C, preferably 32°C;

[0165] Cation suppressor CERS (4mm);

[0166] Detector: conductivity detector;

[0167] Injection volume: 25 μl.

[0168] II. Preparation of reference substance solution:

[0169] Precisely measure an appropriate amount of hydrazine sulfate, dissolve it with ultrapure water and dilute it to a solution containing about 0.9 ...

Embodiment 3

[0209] Example 3 Use method of the present invention to measure 6 batches of sitagliptin phosphate

[0210] The specific measurement results are as follows:

[0211] Weigh an appropriate amount of sitagliptin phosphate bulk drug, add ultrapure water to dissolve and dilute to make a solution containing about 60mg per 1ml, as the reference solution; accurately measure an appropriate amount of hydrazine sulfate, and dilute it to about 60mg per 1ml with ultrapure water. A solution containing 0.9 μg was used as a control solution. Under the chromatographic conditions described in Example 2, accurately measure 25 μl of the reference substance solution, inject it into an ion chromatograph, and adjust the sensitivity of the instrument so that the chromatographic peak height of the main component is 10%-20% of the full scale. Then accurately measure 25 μl each of the test solution and the reference solution, inject samples into the ion chromatograph, record the chromatogram to 5 tim...

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Abstract

The invention provides a detection method for free hydrazine on the basis of ion chromatography. According to the chromatographic conditions, a chromatography column is a Thermo Dionex IonPac CS12A chromatography column with the specification being 250mm*4mm; a protective column is a Thermo Dionex IonPac CS12A chromatography column with the specification being 4 mm*50mm; the specification of a positive ion inhibitor CERS is 4 mm; a detector is an electric conduction detector; a moving phase is 5 mmol / l loprazolam; the flow speed is 0.8-1.3 ml / min; the column temperature is 28-35 DEG C; the sampling size is 25 microliters. According to the detection method, the minimum linear detection concentration is 0.18 microgram / ml, and the minimum detection concentration is 0.05 microgram / ml. The invention further provides application of the detection method in sitagliptin phosphate bulk drug impurity detection.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a detection method for free hydrazine and its application in the detection of impurities in sitagliptin phosphate crude drug. Background technique [0002] Diabetes mellitus is a chronic comprehensive disease mainly characterized 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 (Version 8) released by the International Diabetes Federation shows that the global prevalence of diabetes (20-79 years old) was about 8.8% in 2017, and there were about 425 million adults with diabetes. By 2045, this figure may reach 629 million. [0003] China is the country with the largest number of diabetic patients, accounting for about a quarter of the world's total. Diabetes mellitus is a high-incidence chronic disease with ...

Claims

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Application Information

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IPC IPC(8): G01N30/96G01N30/64G01N30/06G01N30/04G01N30/86
CPCG01N30/04G01N30/06G01N30/64G01N30/8634G01N30/96G01N2030/047G01N2030/645G01N2030/965
Inventor 冷春生王广祁宁科权王健盛永强
Owner TONGHUA DONGBAO PHARMA
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