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Method for determining enantiomer impurity in alogliptin crude drug and preparation by virtue of HPLC

A technology of enantiomers and raw materials, applied in the field of pharmaceutical analysis, can solve problems such as ineffectiveness, isomer impurity detection methods that have not yet been patented and reported in literature, and harmful

Active Publication Date: 2015-07-01
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With chiral drugs, one isomer may be effective while the other may be ineffective or even harmful
From the 1950s to the early 1960s, the incident of Thalidomide, a drug used to treat early morning sickness in pregnant women, occurred. Thalidomide entered the market in 1956 and was withdrawn from the market in 1962, killing 12,000 seals. For children with limb deformities, the main reason is that the R type of Thalidomide has a good sedative and emetic effect, but the S type has a strong teratogenic effect.
[0008] The chiral drug alogliptin benzoate is a new drug that has been on the market in recent years, and the detection method of its isomer impurities has not yet been patented or reported in the literature

Method used

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  • Method for determining enantiomer impurity in alogliptin crude drug and preparation by virtue of HPLC
  • Method for determining enantiomer impurity in alogliptin crude drug and preparation by virtue of HPLC
  • Method for determining enantiomer impurity in alogliptin crude drug and preparation by virtue of HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] Instrument: AgiLent1100 high performance liquid chromatography, 1100 UV detector;

[0105] Chromatographic column: CHIRALPAK AS-H (150×4.6mm, 5μm);

[0106] Mobile phase A: n-hexane (containing 0.3% diethylamine v / v);

[0107] Mobile phase B: ethanol (containing 0.3% diethylamine v / v);

[0108] See the table below for gradient elution;

[0109] time (minutes)

Mobile Phase A(%)

Mobile phase B(%)

0

75

25

3

75

25

20

25

75

25

25

75

26

75

25

32

75

25

[0110] Flow rate: 0.4mL / min

[0111] Detection wavelength: 278nm

[0112] Column temperature: 25°C

[0113] Injection volume: 10μL

[0114] Thinner: ethanol

[0115] experiment procedure:

[0116] Separation test solution: Accurately weigh 5.12mg of alogliptin benzoate racemate (a mixture of alogliptin benzoate R type and S type about 1:1) into a 100mL volumetric flask, add an appropriate amount of ethanol,...

Embodiment 2

[0127] Instrument: AgiLent1100 high performance liquid chromatography, 1100 UV detector;

[0128] Chromatographic column: CHIRALPAK AS-H (150×4.6mm, 5μm);

[0129] Mobile phase A: n-hexane (containing 0.2% diethylamine v / v);

[0130] Mobile phase B: ethanol (containing 0.2% diethylamine v / v);

[0131] See the table below for gradient elution;

[0132] time (minutes)

Mobile Phase A(%)

Mobile phase B(%)

0

75

25

3

75

25

20

25

75

25

25

75

26

75

25

32

75

25

[0133] Flow rate: 0.4mL / min

[0134] Detection wavelength: 278nm

[0135] Column temperature: 25°C

[0136] Injection volume: 10μL

[0137] Thinner: ethanol

[0138] experiment procedure:

[0139] Separation test solution: Accurately weigh 5.23 mg of alogliptin racemate (about 1:1 mixture of alogliptin R type and S type) into a 10mL volumetric flask, add an appropriate amount of ethanol, dissolve it by ultr...

Embodiment 3

[0143] Instrument: AgiLent1100 high performance liquid chromatography, 1100 UV detector;

[0144] Chromatographic column: CHIRALPAK AS-H (150×4.6mm, 5μm);

[0145] Mobile phase A: n-hexane (containing 0.4% diethylamine v / v);

[0146] Mobile phase B: ethanol (containing 0.4% diethylamine v / v);

[0147] See the table below for gradient elution;

[0148] time (minutes)

Mobile Phase A(%)

Mobile phase B(%)

0

75

25

3

75

25

20

25

75

25

25

75

26

75

25

32

75

25

[0149] Flow rate: 0.4mL / min

[0150] Detection wavelength: 278nm

[0151] Column temperature: 25°C

[0152] Injection volume: 10μL

[0153] Thinner: ethanol

[0154] experiment procedure:

[0155] Separation test solution: Accurately weigh 5.45 mg of alogliptin racemate (about 1:1 mixture of alogliptin R type and S type) into a 10mL volumetric flask, add an appropriate amount of ethanol, dissolve it by ultr...

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Abstract

The invention discloses a method for determining an enantiomer impurity in an alogliptin crude drug and a preparation by virtue of HPLC. The method comprises the step of carrying out gradient elution by selecting a silica gel coated with amylose-tri((S)-alpha-phenethyl carbamate on the surface as a stationary phase, and taking a mixed solvent of n-hexane and ethanol containing triethylamine or diethylamine respectively as a mobile phase. With the adoption of the method, alogliptin or the salt thereof can be separated from the enantiomer of alogliptin, and the masses of the alogliptin crude drug and the preparation thereof can be effectively controlled. According to the detection method, the specificity is high, the precision and the accuracy are high, the tolerance is good, the operation is convenient, and medicine quality can be effectively controlled.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to the detection of enantiomer impurities in alogliptin bulk drug and preparations thereof. Background technique [0002] Chiral drug refers to a pair of enantiomers that are real objects and mirror images obtained after introducing a chiral center into the molecular structure of a drug. The absorption, distribution, metabolism and excretion of chiral drugs in the organism are all In addition to stereoselectivity, different isomers of chiral drugs often display different pharmacological and toxicological properties, as well as different pharmacokinetic properties. [0003] Enantiomers are a lot like your left and right hands, they look very similar, but not identical. With chiral drugs, one isomer may be effective, while the other may be ineffective or even harmful. From the 1950s to the early 1960s, the incident of Thalidomide, a drug used to treat early morning sickness ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 夏艳开崔健钱丽娜
Owner WATERSTONE PHARMA WUHAN
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