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A method for detecting related substances in piperacillin sodium and sulbactam sodium for injection

A technology of cillin sodium sulbactam sodium and related substances, applied in the field of pharmaceutical preparations, can solve the problems of high polarity, inability to separate sulbactam impurities from sulbactam, unsuitability for detection, etc., and achieve simple operation and good economy Benefits and promotion prospects, the effect of low cost

Active Publication Date: 2016-01-20
XIANGBEI WELMAN PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

BP2009, USP32 and CP2010 all use the HPLC method to detect piperacillin sodium, wherein the proportion of the organic phase in the mobile phase is at least 25%, but (2S)-2-amino-3-methyl-3-sulfinic acid butyric acid The polarity of sulbactam sodium is very large, and the sulbactam impurity cannot be separated from sulbactam; in addition, the current method for detecting related substances of sulbactam sodium adopts gradient elution, and the elution time is only 13min, and the elution time of the organic phase is high. Only about 1min, it is found through experiments that such chromatographic detection conditions are not suitable for the detection of related substances of piperacillin sodium
However, if the method for detecting related substances in the two single prescriptions of piperacillin sodium and sulbactam sodium is simply adopted, it is not suitable for the detection of related substances in the compound piperacillin sodium and sulbactam sodium.

Method used

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  • A method for detecting related substances in piperacillin sodium and sulbactam sodium for injection
  • A method for detecting related substances in piperacillin sodium and sulbactam sodium for injection
  • A method for detecting related substances in piperacillin sodium and sulbactam sodium for injection

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: Detection of related substances of piperacillin sodium and sulbactam sodium for injection

[0042] 1. Instruments and conditions

[0043] High performance liquid chromatography: Agilent1200

[0044] Chromatographic column: AgilentXDB-C18 (250mm*4.6mm, 5um)

[0045] Mobile phase: Phase A is methanol: water: 0.2mol / l sodium dihydrogen phosphate solution: 10% tetrabutylammonium hydroxide solution=550:366:82:2V / V

[0046] Phase B is water: 0.2mol / l sodium dihydrogen phosphate solution: 10% tetrabutylammonium hydroxide solution=447:100:3V / V

[0047] pH of mobile phase: 5.5

[0048] Flow rate: 1.0ml / min

[0049] Detection wavelength: 220nm

[0050] Column temperature: 30°C

[0051] Injection volume: 10ul

[0052] Gradient elution conditions are as follows:

[0053]

[0054]

[0055] 2. Solution Preparation

[0056] Mixed solvent: mobile phase A and mobile phase B are mixed at a ratio of 5:95V / V;

[0057] Test solution: Take 30 mg of piperacillin ...

Embodiment 2

[0062] Embodiment 2: Detection of related substances of piperacillin sodium and sulbactam sodium for injection

[0063] 1. Instruments and conditions

[0064] High performance liquid chromatography: Agilent1200

[0065] Chromatographic column: AgilentXDB-C18 (250mm*4.6mm, 5um)

[0066] Mobile phase: phase A is methanol: water: 0.2mol / l sodium dihydrogen phosphate solution: 10% tetrabutylammonium hydroxide solution = 550:366:82:2, V / V

[0067] Phase B is water: 0.2mol / l sodium dihydrogen phosphate solution: 10% tetrabutylammonium hydroxide solution=447:100:3V / V

[0068] pH of the mobile phase: 4.5

[0069] Flow rate: 1.5ml / min

[0070] Detection wavelength: 225nm

[0071] Column temperature: 20°C

[0072] Injection volume: 10ul

[0073] Gradient elution conditions are as follows:

[0074]

[0075] 2. Solution Preparation

[0076] Mixed solvent: mobile phase A and mobile phase B are mixed at a ratio of 5:95V / V;

[0077] Test solution: Take 30 mg of piperacillin sodi...

Embodiment 3

[0082] Embodiment 3: the determination method of related substances of piperacillin sodium sulbactam sodium for injection

[0083] Detection of Related Substances of Piperacillin Sodium and Sulbactam Sodium for Injection

[0084] 1. Instruments and conditions

[0085] High performance liquid chromatography: Agilent1200

[0086] Chromatographic column: WaterssymmetryC18 (250mm*4.6mm, 5um)

[0087] Mobile phase: phase A is methanol: water: 0.2mol / l sodium dihydrogen phosphate solution: 10% tetrabutylammonium hydroxide solution = 550:366:82:2,

[0088] Phase B is water: 0.2mol / l sodium dihydrogen phosphate solution: 10% tetrabutylammonium hydroxide solution=447:100:3

[0089] pH of the mobile phase: 6.5

[0090] Flow rate: 0.5ml / min

[0091] Detection wavelength: 254nm

[0092] Column temperature: 35°C

[0093] Injection volume: 20ul

[0094] Gradient elution conditions are as follows:

[0095]

[0096]

[0097] 2. Solution Preparation

[0098] Mixed solvent: mobi...

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Abstract

The invention provides a method for detecting related substances in piperacillin sodium and sulbactum sodium for injection. The method adopts an octadecyl silane bonded silica-gel chromatographic column to carry out gradient elution so as to rapidly and precisely complete the detection on related substances in piperacillin sodium and sulbactum sodium. In the obtained chromatogram, the main related substance (2S)-2-amino-3-methyl-3-sulfinobutyric acid and piperacillin penicilloic acid are well separated, piperacillin and sulbactum are also well separated from other related substances, and the separation degree is more than 1.5. The degradation researches and methodology on piperacillin sodium and sulbactum sodium show that the provided method has a stability indicating function, and thus the detection method can be used to control the limits of impurities in piperacillin sodium and sulbactum sodium, and can also be used to control the quality of piperacillin sodium and sulbactum sodium for injection. The method has the advantages of convenient operation and low cost, and has a good economic profit and promotion prospect.

Description

technical field [0001] The invention relates to a pharmaceutical preparation, in particular to a detection method of the pharmaceutical preparation, in particular to a method for detection of related substances in piperacillin sodium sulbactam sodium for injection. Background technique [0002] Piperacillin sodium is a penicillin antibiotic, which plays a bactericidal effect by interfering with the synthesis of bacterial cell walls, and is widely used in the prevention and treatment of various infectious diseases caused by Gram-negative bacteria. Because it contains a β-lactam ring, it is easily hydrolyzed by the β-lactamase produced by bacteria to produce drug resistance. Sulbactam sodium is a β-lactamase inhibitor, which has irreversible competitive inhibition for β-lactamase produced by Staphylococcus aureus and most Gram-negative bacteria, so sulbactam sodium is often combined with penicillins or cephalosporins Combined use of mycocin drugs has a good antibacterial syne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王霆高靓邓桂兴孙明杰
Owner XIANGBEI WELMAN PHARMA CO LTD
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