Method for measuring sitagliptin-related matters by means of separation

A technology related to substances and impurities, applied in the field of drug analysis and detection, can solve the problems of low sensitivity and inaccuracy, and achieve the effect of good separation effect, fast speed and high detection rate

Active Publication Date: 2016-11-16
上海柏狮生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Aiming at the above-mentioned technical problems in the prior art, the invention provides a kind of method for separating and measuring sitagliptin related substances, and the method for separating and measu

Method used

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  • Method for measuring sitagliptin-related matters by means of separation
  • Method for measuring sitagliptin-related matters by means of separation
  • Method for measuring sitagliptin-related matters by means of separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1 system practicability

[0049] Instrument: Agilent1260;

[0050]Chromatographic column: Luna 5μC18(2)100A 250×4.6mm, Guangzhou Philome Scientific Instruments Co., Ltd.

[0051] The mobile phase flow rate is 1.0mL / min;

[0052] The temperature of the chromatographic column is 30°C;

[0053] The injection volume is 10 μL;

[0054] The detection wavelength is 210nm;

[0055] Mobile phase A is 0.5 mol / L potassium dihydrogen phosphate buffer solution, adjusted to Ph=6.2 with 2 mol / L potassium hydroxide; mobile phase B is acetonitrile. The gradient of the mobile phase was set as follows:

[0056] t(min)

A

B

0

82

18

6

82

18

7

69

31

18

69

31

20

30

70

30

30

70

[0057] Reference solution (a): Weigh 25mg of sitagliptin standard substance, accurately weigh it in a 50mL volumetric flask, dilute to the mark with diluent, and mix well. (Sitagliptin concentration: 0.5mg / mL) ...

Embodiment 2

[0072] Example 2 Specificity

[0073] Experimental conditions, liquid chromatography method and solution preparation are as in Example 1.

[0074] Method specificity studies examine peak identification and selectivity. Inject blank solution, impurity localization solution and resolution solution respectively, and record the chromatograms.

[0075] The results are shown in Table 2, and the spectrum is shown in figure 1 ,2,3,4,5.

[0076] Table 2 Specificity

[0077]

[0078]

[0079] The results show that good separation can be achieved between each substance and main component of sitagliptin, and between all related substances.

Embodiment 3

[0080] Embodiment 3 detection limit and quantitative limit

[0081] Experimental conditions, liquid chromatography method and solution preparation are as in Example 1.

[0082] For known potential impurities, the limit of detection (LOD) and limit of quantitation (LOQ) were determined based on the signal-to-noise ratio method. Dilute the impurity stock solution of known concentration to the sample with the lowest concentration, detect the signal-to-noise ratio S / N-10 to determine the LOQ of the system, and determine the LOD of the system according to S / N-3. For unknown impurities, use sitagliptin samples instead to investigate the detection limit and quantification limit of a single unknown impurity.

[0083] The test results are shown in Tables 3, 4, 5, and 6.

[0084] Table 3 impurity II-2 detection limit and limit of quantitation determination result

[0085]

[0086] Table 4 unknown impurity detection limit and limit of quantitation assay results

[0087]

[0088...

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Abstract

The invention discloses a method for measuring sitagliptin-related matters by means of separation. The method adopts a high performance liquid chromatograph, takes a PhenomenexLunaC18 (2) 100A column as a chromatographic column and uses acetonitrile and a phosphate buffer solution with a pH (Potential of Hydrogen) value of 6.2 as flowing phases to perform gradient elution under the condition that a wavelength is 210nm. The method is rapid in analysis speed, good in separation effect and low in cost, and can be used for measuring and checking matters related to sitagliptin crude drug. The method is high in detection rate of related matters, high in accuracy and good in repeatability and recovery rate; furthermore, the method is verified to be used for routine analysis and quality control of the sitagliptin crude drug and preparation.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, and relates to a method for quality control of sitagliptin crude drug, in particular to a method for separating and measuring related substances of sitagliptin. Background technique [0002] With the improvement of residents' living standards, the incidence of type Ⅰ and type Ⅱ diabetes is increasing year by year. Diabetes has become a major social problem that threatens people's health, which has attracted the attention and attention of governments and health departments around the world. DPP-4 inhibitor can promote the secretion of insulin and inhibit the secretion of glucagon by inhibiting the inactivation of incretin GLP-1, and it is a new drug for the treatment of type Ⅱ diabetes. DPP-4 inhibitors are safe to use and have less gastrointestinal reactions. Low risk of hypoglycemia, no weight gain and other advantages, has become a research hotspot in recent years. Sitagliptin phosp...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 潘仙华李勤勤王亚萍于万盛曹阳
Owner 上海柏狮生物科技有限公司
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