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Tigecycline intermediate analysis detection method

A detection method and tigecycline technology, which are applied in the field of high performance liquid chromatography analysis, can solve the problems of expensive chromatographic column, cumbersome method, low practicability, etc., and achieve stable and reliable results, simple operation and high practicability. Effect

Active Publication Date: 2015-04-15
SHANDONG NEWTIME PHARMA
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  • Description
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Problems solved by technology

Patents US2007 / 0049561A1 and US2009 / 0099376A1 disclose high-performance liquid chromatography detection methods for this intermediate, but the chromatographic columns used in these methods are relatively expensive, and the methods are relatively cumbersome, and the practicability of general application in R&D and production is low

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  • Tigecycline intermediate analysis detection method
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  • Tigecycline intermediate analysis detection method

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Effect test

Embodiment 1

[0019] Instruments and conditions: Agilent1100 liquid chromatography system, chromatographic column: ZORBAX SB-C18 (4.6×250mm, 5μm), detection wavelength 245nm, column temperature 30°C, flow rate 1.0mL / min, mobile phase: 0.05mol / L ammonium acetate solution : N,N-dimethylformamide: trifluoroacetic acid = 60:39.8:0.2, each liter of the mixed solution of the first three contains 0.01mol of ethylenediaminetetraacetic acid, adjust the pH value to 7.02 with 10% ammonia water.

[0020] Experimental procedure: dissolve the tigecycline intermediate with mobile phase and quantitatively dilute to make a solution containing about 0.3 mg of tigecycline intermediate per 1 mL, as the test solution, accurately measure 20 μL of the test solution and inject Liquid chromatograph, carry out high performance liquid chromatographic analysis according to above-mentioned conditions, record chromatogram, the result sees attached figure 1 .

[0021] attached figure 1 It shows that under the chromatog...

Embodiment 2

[0023] Instrument and conditions: Agilent1100 liquid chromatography system, chromatographic column: ZORBAX SB-C18 (4.6×250mm, 5μm), detection wavelength 245nm, column temperature 30°C, flow rate 0.6mL / min, mobile phase: 0.05mol / L ammonium acetate solution : N,N-dimethylformamide: trifluoroacetic acid=50:49.8:0.2, each liter of the mixed solution of the first three contains 0.01mol of ethylenediaminetetraacetic acid, adjust the pH value to 7.02 with 10% ammonia water.

[0024] Experimental procedure: dissolve the tigecycline intermediate with mobile phase and quantitatively dilute to make a solution containing about 0.3 mg of tigecycline intermediate per 1 mL, as the test solution, accurately measure 20 μL of the test solution and inject Liquid chromatograph, carry out high performance liquid chromatographic analysis according to above-mentioned conditions, record chromatogram, the result sees attached figure 2 .

[0025] attached figure 2 It shows that under the chromatogr...

Embodiment 3

[0027] Instrument and conditions: Agilent1100 liquid chromatography system, chromatographic column: ZORBAX SB-C18 (4.6×250mm, 5μm), detection wavelength 245nm, column temperature 30°C, flow rate 1.2mL / min, mobile phase: 0.05mol / L ammonium acetate solution : N,N-dimethylformamide: trifluoroacetic acid = 70:29.8:0.2, each liter of the mixed solution of the first three contains 0.01mol of ethylenediaminetetraacetic acid, adjust the pH value to 7.02 with 10% ammonia water.

[0028] Experimental procedure: dissolve the tigecycline intermediate with mobile phase and quantitatively dilute to make a solution containing about 0.3 mg of tigecycline intermediate per 1 mL, as the test solution, accurately measure 20 μL of the test solution and inject Liquid chromatograph, carry out high performance liquid chromatographic analysis according to above-mentioned conditions, record chromatogram, the result sees attached image 3 .

[0029] attached image 3 It shows that under the chromatogr...

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Abstract

The invention discloses a tigecycline intermediate analysis detection method used for tigecycline intermediate quality control, a chromatographic column with octadecylsilane chemically bonded silica as a packing is used for high performance liquid chromatography analysis detection at the column temperature of 25-35 DEG C in the flow rate of 0.6-1.2mL / min with the detection wavelength of 245nm, wherein the pH value of the mobile phase is adjusted to 6.80-7.20 with 10% ammonia. The tigecycline intermediate analysis detection method selects an ordinary chromatographic column and a liquid chromatographic system, has the advantages of low price, high practicability and simple operation, can effectively separate a tigecycline intermediate from impurities.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to an analysis and detection method for a tigecycline intermediate. Background technique [0002] Tigecycline was researched and developed by Wyeth Corporation of the United States. It is the first glycylcycline antibiotic approved for clinical intravenous administration. Its mechanism of action is similar to that of tetracycline antibiotics, both through binding to bacterial ribosomes , to prevent the entry of transfer RNA, so that amino acids cannot be combined with peptide chains, and finally play a role in blocking bacterial protein synthesis and limiting bacterial growth, but the binding ability of tigecycline to ribosomes is 5 times that of other tetracyclines. [0003] 9-aminominocycline hydrochloride is an important intermediate for the synthesis of tigecycline, and its chemical formula is C 23 h 28 N 4 o 7 HCl, the structural formula is: [00...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 赵志全
Owner SHANDONG NEWTIME PHARMA
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