HPLC detecting method for tenofovir alafenamide and isomer thereof

A technology for tenofovir alafenamide and a detection method is applied in the field of HPLC detection of tenofovir alafenamide and its isomers, and can solve the problem of long running time and inability to tenofovir alafenamide. The separation of amine and its isomers impurities, the complex mobile phase preparation and other problems, to achieve the effect of accurate results and good resolution

Active Publication Date: 2018-02-02
厦门蔚扬药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In Method 1, the chromatographic column adopts a chiral chromatographic column, and the price is 4 to 5 times that of ordinary C18, and the mobile phase used in the elution process is an organic phase, and the separation cost is high; in Method 2, the preparation of the mobile phase is complicate

Method used

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  • HPLC detecting method for tenofovir alafenamide and isomer thereof
  • HPLC detecting method for tenofovir alafenamide and isomer thereof
  • HPLC detecting method for tenofovir alafenamide and isomer thereof

Examples

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Effect test

Embodiment 1

[0042] A method for separating and determining tenofovir alafenamide and its isomers, specifically comprising the steps of:

[0043] 1) Column: Kromstar C 18 (4.6×250 mm×5 µm);

[0044] 2) Column temperature: 30°C;

[0045] 3) Wavelength: 260nm;

[0046] 4) Injection volume: 5 µL;

[0047] 5) Flow rate: 1.0 mL / min;

[0048] 6) Isocratic elution: methanol: 0.1% phosphoric acid aqueous solution = 40:60.

[0049] see results figure 1 , figure 1 The chromatographic peak at 19.892 min is the chromatographic peak of the isomers of tenofovir alafenamide, and the chromatographic peak at 21.863 min is the chromatographic peak of tenofovir alafenamide. The separation degree of the two was 1.83, meeting the requirements of the Chinese Pharmacopoeia.

Embodiment 2

[0051] A method for separating and determining tenofovir alafenamide and its isomers, specifically comprising the steps of:

[0052] 1) Column: Kromstar C 18 (4.6×250 mm×5 µm);

[0053] 2) Column temperature: 30°C;

[0054] 3) Wavelength: 260nm;

[0055] 4) Injection volume: 5 µL;

[0056] 5) Flow rate: 1.0 mL / min;

[0057] 6) Isocratic elution: methanol: 0.1% formic acid aqueous solution = 40:60.

[0058] see results figure 2 , figure 2 The chromatographic peak at 29.038 min is the chromatographic peak of the isomers of tenofovir alafenamide, and the chromatographic peak at 31.850 min is the chromatographic peak of tenofovir alafenamide. The separation degree of the two is 2.13, meeting the requirements of the Chinese Pharmacopoeia.

Embodiment 3

[0060] A method for separating and determining tenofovir alafenamide and its isomers, specifically comprising the steps of:

[0061] 1) Column: Kromstar C 18 (4.6×250 mm×5 µm);

[0062] 2) Column temperature: 30°C;

[0063] 3) Wavelength: 260nm;

[0064] 4) Injection volume: 5 µL;

[0065] 5) Flow rate: 1.0 mL / min;

[0066] 6) Isocratic elution: Methanol: 0.1% trifluoroacetic acid aqueous solution = 40:60.

[0067] see results image 3 , image 3The chromatographic peak at 33.892 min is the chromatographic peak of the isomers of tenofovir alafenamide, and the chromatographic peak at 36.342 min is the chromatographic peak of tenofovir alafenamide. The separation degree of the two is 1.62, meeting the requirements of the Chinese Pharmacopoeia.

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Abstract

The invention relates to a fractionation detection method for tenofovir alafenamide and isomer thereof, and belongs to the technical field of fractionation detection. The detection method comprises the following steps: taking a chromatographic column filled with octadecylsilane chemically bonded silica; and carrying out isocratic elution by taking methanol and an acidic aqueous solution as mobilephases under certain conditions. By the method, the tenofovir alafenamide and the isomer thereof can be effectively detected in a fractionation manner, the peak pattern of chromatographic peaks is good, the appearance time is short, and the degree of fractionation is good.

Description

technical field [0001] The invention relates to an HPLC detection method for tenofovir alafenamide and its isomers, belonging to the technical field of drug detection. Background technique [0002] Tenofovir alafenamide is a novel nucleotide reverse transcriptase inhibitor and a prodrug of tenofovir. The drug is an improved version of Gilead's marketed drug Viread®, which has been approved by the United States for the treatment of adults with uncompensated chronic hepatitis B. Compared with Viread®, the clinical dosage of tenofovir alafenamide is smaller, it only needs 1 / 10 of Viread® to have equivalent antiviral efficacy, better safety, and can improve renal function and Bone safety parameters. [0003] The structure of tenofovir alafenamide is shown in the following formula (1): [0004] (1). [0005] In the preparation process of tenofovir alafenamide, the racemate is first synthesized and then transformed, so the synthesized tenofovir alafenamide may have isomer im...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 蔡惠坚顾世海
Owner 厦门蔚扬药业有限公司
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