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7-ADCA composition and method for detecting impurities in 7-ADCA composition

A 7-ADCA and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult chromatographic separation and detection obstacles, and achieve the effects of high sensitivity, high accuracy, and strong specificity

Pending Publication Date: 2022-02-25
YILI CHUANNING BIOTECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] However, for the 7-ADCA products obtained in further production, the structures of 7-ADCA, DAOC, DCPC and D-7-ACA are relatively similar, and it is difficult to achieve chromatographic separation
This creates a big obstacle for the detection of DAOC, DCPC and D-7-ACA impurities in 7-ADCA products

Method used

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  • 7-ADCA composition and method for detecting impurities in 7-ADCA composition
  • 7-ADCA composition and method for detecting impurities in 7-ADCA composition
  • 7-ADCA composition and method for detecting impurities in 7-ADCA composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This embodiment includes the following steps:

[0042] 1. Preparation of the test solution:

[0043] Preparation of mobile phase A: Mobile phase A is 10 mmol / L potassium dihydrogen phosphate solution (adjust pH to 4.0 with phosphoric acid).

[0044] Preparation of the test solution: Weigh 50mg of 7-ADCA sample (the test), put it in a 100ml volumetric flask, add 10ml of co-solvent, dissolve it, then dissolve it with mobile phase A and dilute to the scale, shake well to get the test solution. Wherein, the co-solvent is a mixture of 0.2% by weight ammonia water and acetonitrile in a volume ratio of 50:50.

[0045]Preparation of standard addition solution: use mobile phase A as solvent, prepare D-7-ACA, DCPC, 7-ADCA and DAOC at concentrations of 10μg / ml, 10μg / ml, 1mg / ml, 0.5mg / ml Spiked solution.

[0046] 2. Perform HPLC chromatographic detection:

[0047] Instrument: Agilent 1260 high performance liquid chromatography;

[0048] The chromatographic conditions are:

...

Embodiment 2

[0064] This embodiment includes the following steps:

[0065] 1. Preparation of the test solution:

[0066] Prepare mobile phase A, mobile phase A is 10mmol / L potassium dihydrogen phosphate solution (adjust pH to 4.5 with phosphoric acid).

[0067] Weigh 50 mg of 7-ADCA sample (test product), put it in a 100 ml volumetric flask, add 10 ml of co-solvent, dissolve, then dissolve with mobile phase A and dilute to the mark, shake well to get the test product solution.

[0068] Wherein, the co-solvent is a mixture of 0.25% by weight ammonia water and acetonitrile in a volume ratio of 60:40.

[0069] 2. Perform HPLC chromatographic detection:

[0070] Instrument: Agilent 1260 high performance liquid chromatography;

[0071] The chromatographic conditions are:

[0072] Chromatographic column: Osaka Soda CAPCELL PAK C18-MGII (4.6*250mm, 5um);

[0073] Mobile phase: Mobile phase A is a 10 mmol / L potassium dihydrogen phosphate solution (adjust the pH to 4.5 with phosphoric acid); m...

Embodiment 3

[0086] This embodiment includes the following steps:

[0087] 1. Preparation of the test solution:

[0088] Prepare mobile phase A, mobile phase A is 20mmol / L potassium dihydrogen phosphate solution (adjust pH to 5.0 with phosphoric acid).

[0089] Weigh 50 mg of 7-ADCA sample (test product), put it in a 100 ml volumetric flask, add 10 ml of co-solvent, dissolve, then dissolve with mobile phase A and dilute to the mark, shake well to get the test product solution.

[0090] Wherein, the co-solvent is a mixture of 0.5% by weight ammonia water and acetonitrile in a volume ratio of 60:40.

[0091] 2. Perform HPLC chromatographic detection:

[0092] Instrument: Agilent 1260 high performance liquid chromatography;

[0093] The chromatographic conditions are:

[0094] Chromatographic column: Philomon Luna C18(2) (4.6*250mm, 5um);

[0095] Mobile phase: mobile phase A is 20mmol / L potassium dihydrogen phosphate solution (adjust the pH to 5.0 with phosphoric acid); mobile phase B i...

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Abstract

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a 7-ADCA composition and a method for detecting impurities in the 7-ADCA composition. The 7-ADCA composition provided by the invention comprises the following components in percentage by weight: 90.0-99.9% of 7-aminodeacetoxycephalosporanic acid, 0 to 5.0 percent of deacetoxycephalosporin C, 0 to 5.0 percent of deacetyl cephalosporin C, and 0 to 5.0 percent of deacetyl-7-aminocephalosporanic acid. Impurities acetoxycephalosporin C, deacetyl cephalosporin C and deacetyl-7-aminocephalosporanic acid in the 7-ADCA composition are detected through high performance liquid chromatography, and chromatographic conditions are as follows: octadecylsilane chemically bonded silica with the carbon content greater than 12% is taken as a filler of a chromatographic column; a phosphate solution is used as a mobile phase A, and a phosphate solution-acetonitrile mixed solution is used as a mobile phase B; the detection method disclosed by the invention is good in accuracy, high in sensitivity and strong in specificity, and has very high application potential in quality control of 7-ADCA products.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a 7-ADCA composition and a detection method for impurities therein. Background technique [0002] The structural formula of 7-aminodesacetoxycephalosporanic acid (7-ADCA) is as follows: [0003] [0004] It is an important semi-synthetic intermediate of cephalosporin antibiotics, and is used in the pharmaceutical industry to synthesize cephalexin, cephradine and cefadroxil, which are widely used in the market. [0005] At present, most manufacturers use penicillin G potassium salt to undergo chemical synthesis to expand the ring, and then enzymatically remove the side chain to obtain it. Chinese invention patent application "CN112831421A-a cephalosporin compound production strain and its application" proposes a new process, which directly obtains desacetoxy cephalosporin C through fermentation, and then removes the side chain through enzymatic hydrolysis Ge...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/065Y02P20/55
Inventor 董进臣陈倩张宝新牛李杰周路张霞飞高占虎
Owner YILI CHUANNING BIOTECH CO
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