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Method for separating and detecting insulin degludec side chains and enantiomers thereof

A technique for insulin degludec and its enantiomers, which is applied in the field of analytical chemistry and can solve problems such as not containing the side chain of insulin degludec

Pending Publication Date: 2021-10-12
DONGGUAN HEC BIOPHARMACEUTICAL R&D CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, "United States Pharmacopoeia" USP, "European Pharmacopoeia" EP, "Japanese Pharmacopoeia" JP, and "Chinese Pharmacopoeia" Ch.P. do not include the separation and detection methods for the side chain of insulin degludec and its enantiomers. In order to more accurately control the impurities in the product and ensure the quality of the API, it is necessary to study the analytical method suitable for the side chain of insulin degludec and its enantiomers

Method used

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  • Method for separating and detecting insulin degludec side chains and enantiomers thereof
  • Method for separating and detecting insulin degludec side chains and enantiomers thereof
  • Method for separating and detecting insulin degludec side chains and enantiomers thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Instruments and Conditions

[0064] Chromatographic column: CHIRALPAK IE, 4.6x250mm, 5μm;

[0065] Detector: DAD (ultraviolet detector), detection wavelength 210nm;

[0066] Flow rate: 0.6mL / min;

[0067] Column temperature: 35°C;

[0068] Injection volume: 4μL;

[0069] Mobile phase A: n-hexane;

[0070] Mobile phase B: ethanol: methanol: TFA = 90:10:0.3 (V:V:V);

[0071] Elution ratio: phase A:phase B=25:75(V:V);

[0072] Running time: 30min;

[0073] Diluent / blank solution: isopropanol: acetic acid = 1:1 (V:V);

[0074] Experimental procedure

[0075] Take 25.28mg of insulin degludec side chain sample, 6.07mg of insulin degludec side chain enantiomer, accurately weighed into a 10mLEP tube, add 4mL of diluent, dissolve, shake well, as insulin degludec side chain spike solution .

[0076] Take the blank solution and insulin degludec side chain spiked solution, carry out high-performance liquid chromatography analysis according to the above conditions, record ...

Embodiment 2

[0081] Instruments and Conditions

[0082] Chromatographic column: CHIRALPAK IE, 4.6x250mm, 5μm;

[0083] Detector: DAD (ultraviolet detector), detection wavelength 210nm;

[0084] Flow rate: 0.6mL / min;

[0085] Column temperature: 40°C;

[0086] Injection volume: 4μL;

[0087] Mobile phase A: n-hexane;

[0088] Mobile phase B: ethanol: methanol: TFA = 90:10:0.3 (V:V:V);

[0089] Elution ratio: phase A:phase B=25:75(V:V);

[0090] Running time: 30min;

[0091] Diluent / blank solution: isopropanol: acetic acid = 1:1 (V:V);

[0092] Experimental procedure

[0093] Take 25.28mg of insulin degludec side chain sample, 6.07mg of insulin degludec side chain enantiomer, accurately weighed into a 10mL EP tube, add 4mL diluent, dissolve, shake well, as insulin degludec side chain spike solution.

[0094] Take the blank solution and insulin degludec side chain spiked solution, carry out high-performance liquid chromatography analysis according to the above conditions, record the...

Embodiment 3

[0098] Instruments and Conditions

[0099] Chromatographic column: CHIRALPAK IE, 4.6x250mm, 5μm;

[0100] Detector: DAD (ultraviolet detector), detection wavelength 210nm;

[0101] Flow rate: 0.6mL / min;

[0102] Column temperature: 25°C;

[0103] Injection volume: 4μL;

[0104] Mobile phase A: n-hexane;

[0105] Mobile phase B: ethanol: methanol: TFA = 90:10:0.3 (V:V:V);

[0106] Elution ratio: phase A:phase B=25:75(V:V);

[0107] Running time: 30min;

[0108] Diluent / blank solution: isopropanol: acetic acid = 1:1 (V:V);

[0109] Experimental procedure

[0110] Take 25.28mg of insulin degludec side chain sample, 6.07mg of insulin degludec side chain enantiomer, accurately weighed into a 10mL EP tube, add 4mL diluent, dissolve, shake well, as insulin degludec side chain spike solution.

[0111] Take the blank solution and insulin degludec side chain spiked solution, carry out high-performance liquid chromatography analysis according to the above conditions, record the...

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Abstract

The invention relates to a method for separating and detecting the insulin degludec side chains and enantiomers thereof, and belongs to the field of analytical chemistry. According to the method, a chromatographic column with a polysaccharide derivative as a filler is adopted, a mobile phase is divided into a phase A and a phase B, the phase A is n-hexane or n-heptane, and the phase B is a mixed solution of ethanol, methanol and trifluoroacetic acid. The method is simple, rapid and accurate.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and detecting side chains of insulin degludec and its enantiomers. Background technique [0002] Insulin degludec was developed by NovoNordisk and launched in Japan in October 2012, approved for the treatment of type 1 and type 2 diabetes. On September 25, 2015, the US FDA approved the launch of the new drug Insulin Degludec injection of Novo Nordisk, Denmark, with the trade name Tresiba. Insulin degludec is a new generation of basal insulin analogues, which form multi-hexamers after subcutaneous injection, so as to exert a 24h ultra-long-acting effect. The CAS number of insulin degludec is 844439-96-9, the molecular weight is 6103.97204, and the molecular formula of insulin degludec is C 274 h 411 N 65 o 81 S 6 . [0003] Insulin degludec side chain, chemical name is (S)-16-((1-carboxy-4-((2,5-diketopyrrol-1-yl)oxy)-4-ketobutyl)amino )-16-carbo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 范晓梅叶艳影黄文清郭林峰李晓平杨福斌郑宝液栾保磊饶万兵李艳华
Owner DONGGUAN HEC BIOPHARMACEUTICAL R&D CO LTD
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