An ultra-high performance liquid chromatography detection method for terlipressin and its impurities

A terlipressin and ultra-high performance liquid chromatography technology, which is applied in the field of ultra-high performance liquid chromatography detection of terlipressin and its impurities, can solve the problems of difficulty in completely effective separation, waste of human and material resources, and the like

Active Publication Date: 2017-01-04
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The above compounds can be separated and detected separately when using different chromatographic conditions, but there is a great waste of manpower and material resources when using multiple chromatographic conditions for separate detection
[0019] The above impurities and terlipressin are very similar in structure, but from the perspective of polarity, some impurities and terlipressin have a large polarity difference. Therefore, each component can be obtained on the same column The fully efficient separation of

Method used

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  • An ultra-high performance liquid chromatography detection method for terlipressin and its impurities
  • An ultra-high performance liquid chromatography detection method for terlipressin and its impurities
  • An ultra-high performance liquid chromatography detection method for terlipressin and its impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Flow rate: 0.4mL / min

[0059] Column temperature: 50°C

[0060] Column pressure: 6000psi

[0061] Injection volume: 5μL

[0062] Mobile phase A: 0.01M phosphoric acid-triethylamine aqueous solution (adjust pH=6.5 with ammonia water): acetonitrile=90:10;

[0063] Mobile phase B: 0.01M phosphoric acid-triethylamine aqueous solution (adjust pH=6.5 with ammonia water): acetonitrile=40:60;

[0064] The gradient of mobile phase A and mobile phase B is shown in Table 4 below.

[0065] Table 4

[0066]

[0067] Weigh 100 mg of terlipressin, 10 mg of impurity A, 10 mg of impurity B, 10 mg of impurity C, 10 mg of impurity D, 10 mg of impurity E and 10 mg of impurity F, and dissolve them with the mobile phase A described in this example, in the same manner as in the comparative example Prepare the test sample solution and filter it with a Φ0.45 μm filter membrane. The concentration of terlipressin in the sample is 10 mg / mL, and the concentration of each impurity is 1 mg / mL...

Embodiment 2

[0072] Flow rate: 0.5mL / min

[0073] Column temperature: 50°C

[0074] Column pressure: 6000psi

[0075] Injection volume: 5μL

[0076] Mobile phase A: 0.01M phosphoric acid-triethylamine aqueous solution (phosphoric acid adjusts pH=3.0): acetonitrile=90:10;

[0077] Mobile phase B: 0.01M phosphoric acid-triethylamine aqueous solution (phosphoric acid to adjust pH=3.0): acetonitrile=40:60,

[0078] The gradient of mobile phase A and mobile phase B is the same as in Table 2.

[0079] Weigh 100 mg of terlipressin, 10 mg of impurity A, 10 mg of impurity B, 10 mg of impurity C, 10 mg of impurity D, 10 mg of impurity E and 10 mg of impurity F, and dissolve them with the mobile phase A described in this example, in the same manner as in the comparative example The test sample was prepared and filtered with a Φ0.45 μm filter membrane. The concentration of terlipressin in the sample was 10 mg / mL, and the concentration of each impurity was 1 mg / mL. Set the flow rate to 0.5mL / min, ...

Embodiment 3

[0084] Flow rate: 0.6mL / min

[0085] Column temperature: 50°C

[0086] Column pressure: 6000psi

[0087] Injection volume: 5μL

[0088] Mobile phase A: 0.01M phosphoric acid-triethylamine aqueous solution (phosphoric acid adjusts pH=3.2): acetonitrile=90:10;

[0089] Mobile phase B: 0.01M phosphoric acid-triethylamine aqueous solution (phosphoric acid to adjust pH=3.2): acetonitrile=40:60,

[0090] The gradient of mobile phase A and mobile phase B is shown in Table 7 below.

[0091] Table 7

[0092]

[0093] Weigh 100 mg of terlipressin, 10 mg of impurity A, 10 mg of impurity B, 10 mg of impurity C, 10 mg of impurity D, 10 mg of impurity E and 10 mg of impurity F, and dissolve them with the mobile phase A described in this example, in the same manner as in the comparative example The test sample was prepared and filtered with a Φ0.45 μm filter membrane. The concentration of terlipressin in the sample was 10 mg / mL, and the concentration of each impurity was 1 mg / mL. Se...

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Abstract

The invention provides an ultra-high performance liquid chromatogram detection method for segregation analysis of terlipressin and impurities thereof. The method comprises the step of and carrying out gradient elution on the terlipressin and the impurities thereof by taking a mobile phase A and a mobile phase B which are prepared from a buffer solution and an organic solvent in different proportions as moving phases in an ultra-high performance liquid chromatograph, thereby realizing rapid segregation analysis of the terlipressin and the impurities thereof.

Description

technical field [0001] The invention relates to a method for separating and analyzing terlipressin and its impurities by using ultra-high performance liquid chromatography. Background technique [0002] The structure of Terlipressin is [0003] Gly-Gly-Gly-c[Cys-Tyr-Phe-Gln-Asn-Cys]-Pro-Lys-Gly-NH 2 (SEQ ID NO: 1), it is a kind of artificially synthesized long-acting vasopressin preparation, as a kind of prodrug, it is inactive in itself, and it is detached by aminopeptidase in the body through the action of aminopeptidase. After a glycyl residue, the active lysine vasopressin is slowly "released", which can contract visceral vascular smooth muscle and reduce visceral blood flow (such as reducing blood flow in the mesentery, spleen, uterus, etc.), thereby It reduces portal blood flow and portal pressure, and also acts on smooth muscles such as the esophagus and uterus. On the other hand, terlipressin can also reduce plasma renin concentration, thereby reducing the product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 康旭刘建马亚平袁建成
Owner HYBIO PHARMA
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