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Methods for detecting impurities in tigecycline

A technology of tigecycline and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the detection of undiscovered N-tert-butylglycine hydrochloride and N-tert-butylglycyl chloride hydrochloride Methods and other issues to achieve the effect of ensuring drug safety, short detection time, accurate and reliable measurement results

Active Publication Date: 2013-05-08
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The inspection method for related substances reported in the quality standard for import registration of tigecycline for injection can only determine minocycline hydrochloride, 9-aminominocycline hydrochloride and tigecycline differential among the above-mentioned known impurities. isomers and 9-nitrominocycline hydrochloride, while N-tert-butylglycine hydrochloride and N-tert-butylglycyl chloride hydrochloride cannot be detected under the determination conditions of this related substance
There is no report on the detection method of N-tert-butylglycine hydrochloride and N-tert-butylglycyl chloride hydrochloride

Method used

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  • Methods for detecting impurities in tigecycline
  • Methods for detecting impurities in tigecycline
  • Methods for detecting impurities in tigecycline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The detection of N-tert-butylglycyl chloride hydrochloride in the tigecycline of embodiment 1

[0054] (1) Take tigecycline, extract it with acetonitrile, filter, and settle to volume to obtain the test solution;

[0055] (2) Take N-tert-butylglycyl chloride hydrochloride, dissolve and dilute it with acetonitrile to obtain the reference solution;

[0056] (3) Inject the test solution and the reference solution into the high-performance liquid chromatograph respectively, and detect according to the following chromatographic conditions:

[0057] Chromatographic column: Amino column UltimateXB-NH2 (250mm×4.6mm, 5μm);

[0058] Mobile phase: methanol-isopropanol volume ratio: 90:10;

[0059] Flow rate: 1.0ml / min;

[0060] Detection wavelength: 215nm.

[0061] The test results are shown in Table 1.

Embodiment 2

[0062] The detection of N-tert-butylglycine hydrochloride in embodiment 2 tigecycline

[0063] (1) Take tigecycline, extract it with methanol-isopropanol (90︰10v / v), filter, and constant volume to obtain the test solution;

[0064] (2) Take N-tert-butylglycine hydrochloride, dissolve and dilute it with methanol-isopropanol (90:10v / v) to obtain the reference substance solution;

[0065] (3) Inject the test solution and the reference solution into the high-performance liquid chromatograph respectively, and detect according to the following chromatographic conditions:

[0066] Chromatographic column: Amino column UltimateXB-NH2 (250mm×4.6mm, 5μm);

[0067] Mobile phase: methanol-isopropanol volume ratio: 90:10;

[0068] Flow rate: 1.0ml / min;

[0069] Detection wavelength: 215nm.

[0070] The test results are shown in Table 1.

[0071] Table 1

[0072] batch number

[0073]The results showed that, in the above-mentioned batches of products, the contents of N-tert-b...

Embodiment 3

[0074] Embodiment 3 detection condition investigation

[0075] 1. Selection of chromatographic conditions

[0076] (1) Verification of existing chromatographic conditions

[0077] Detect N-tert-butylglycine hydrochloride and N-tert-butylglycine chloride hydrochloride in tigecycline with reference to the determination method of related substances in "Quality Standards for Import Registration of Tigecycline for Injection":

[0078] Avoid light operation. Take an appropriate amount of this product, weigh it accurately, add solvent (take 4.35g of dipotassium hydrogen phosphate and 0.5g of sodium bisulfite, put it in a 1000ml measuring bottle, add water to dissolve and dilute to the mark, adjust the pH with 1mol / L potassium hydroxide solution value to 8.0) and diluted to make a solution containing 0.5 mg of tigecycline per 1 ml as the test solution; respectively accurately weigh N-tert-butylglycine hydrochloride and N-tert-butylglycine chloride An appropriate amount of hydrochlo...

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Abstract

The invention discloses a method for detecting N-tertbutyl glycyl acyl hydrochloride in tigecycline. The invention further discloses a method for detecting N-tertbutyl glycine hydrochloride in tigecycline. The methods are used for detecting the N-tertbutyl glycyl acyl hydrochloride and the N-tertbutyl glycine hydrochloride in tigecycline, are accurate and reliable in detection result, strong in specificity and short in detection time; and moreover a good separation degree of the N-tertbutyl glycyl acyl hydrochloride and the N-tertbutyl glycine hydrochloride is achieved, so that the possibility in comprehensively detecting the impurities in a tigecycline product, controlling the product quality and ensuring the medicine security is provided.

Description

technical field [0001] The invention relates to a detection method for impurities in tigecycline, in particular to a detection method for N-tert-butylglycyl chloride hydrochloride or N-tert-butylglycine hydrochloride. Background technique [0002] Tigecycline (Tigecycline), chemical name: (4S,4aS,5aR,12aS)-4,7-bis(dimethylamino)-9-[(tert-butylamino)acetamido]-3,10, 12,12a-tetrahydroxy-1,11-dioxo-1,4,4a,5,5a,6,11,12a-octahydrotetracene-2-carboxamide, also known as 9-tert-butylglycerol Aminoaminocycline or Dingglyminocycline, the first glycylcycline antibiotic approved for marketing, has the molecular formula: C 29 h 39 N 5 o 8 ; Molecular structural formula is as follows: [0003] [0004] Tigecycline is a new broad-spectrum antibiotic that can be selected at the beginning of treatment when the cause is not clear, and does not need to adjust the dose according to the impairment of renal function. Studies have shown that tigecycline can overcome two major resistance m...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 孙毅田阿娟夏玉立
Owner CHENGDU BAIYU PHARMA CO LTD
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