Polymyxin E component, photochemical product thereof and liquid chromatography-mass spectrometry analysis method

A polymyxin and liquid chromatography technology, which is applied in the fields of polymyxin E components and photochemical products and liquid chromatography-mass spectrometry analysis to achieve the effect of easy popularization

Active Publication Date: 2020-02-28
SHANGHAI INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are still undiscovered PME components

Method used

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  • Polymyxin E component, photochemical product thereof and liquid chromatography-mass spectrometry analysis method
  • Polymyxin E component, photochemical product thereof and liquid chromatography-mass spectrometry analysis method
  • Polymyxin E component, photochemical product thereof and liquid chromatography-mass spectrometry analysis method

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Experimental program
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Embodiment 1

[0069] 1. Instruments and reagents

[0070] Agilent 1260 HPLC, Agilent 1290 HPLC-6550 QTOF-MS (Agilent Technologies, USA), WFH-203B three-purpose UV analyzer (Shanghai Chitang Electronics Co., Ltd.).

[0071] Colistin Sulfate "European Pharmacopoeia" reference substance (batch number: 3.3).

[0072] 2. Experimental conditions

[0073] According to the component analysis method of polymyxin E in "European Pharmacopoeia" version 9.0, a Diamonsil Plus C18 chromatographic column (250mm × 4.6mm, 5 μm) was selected, with sodium sulfate solution: acetonitrile as mobile phase, and the flow rate was 1ml / min; The column temperature is 30° C.; the injection volume is 20 μl; the detection wavelength is 215 nm.

[0074] In this embodiment, the mobile phase A is the mobile phase A containing 0.1% trifluoroacetic acid aqueous solution: acetonitrile=95:5, and the acetonitrile solution containing 0.1% formic acid is the mobile phase B gradient elution, the flow rate is 1ml / min; the column te...

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Abstract

The invention discloses a polymyxin E component, a photochemical product thereof and a liquid chromatography-mass spectrometry analysis method, wherein the polymyxin E component comprises polymyxin Edouble-bonded components, and specifically comprises a polymyxin E1 double-bonded component, and a polymyxin E2 double-bonded component, and double bonds of these components are tested through high-performance liquid chromatography-mass spectrometry (HPLC-MS) and secondary mass spectrometry analysis to be located at the end of N-fatty acyl chain. The double-bonded components are subjected to photochemical reaction, namely a Paterno-Buchi reaction (reaction), under the condition of acetone serving as a reaction reagent to obtain the photochemical product, and the product is verified via HPLC-MSto be a cycloaddition product; the above double-bonded components are designated as 7'-alkenylpolymyxin E1 and 6'-alkenylpolymyxin E2. The polymyxin E double-bonded components may have antibacterialactivity or toxicity different from that of common polymyxin E components and has potential application value, and the structural confirmation for the compounds also provide a research basis for strictly controlling the quality of polymyxin E.

Description

technical field [0001] The invention belongs to the fields of medicinal chemistry and pharmaceutical analytical chemistry, and in particular relates to a polymyxin E (PolymyxinE, PME) component, its photochemical product and a liquid chromatography-mass spectrometry analysis method. Background technique [0002] Polymyxin E (PME) is a multi-component lipopeptide mixture produced by the fermentation of Paenibacillus polymyxa. It is mainly used clinically as PME sulfate (or called colistin, Colistin) or polymyxin E methanesulfonate. Sodium bicarbonate is used as a "last line of defense" to treat infections caused by multidrug-resistant gram-negative bacteria. Since the dosage of PME needs to be increased when using PME alone, but the nephrotoxicity will increase accordingly. Therefore, the use of combined medication or aerosol inhalation becomes a trend to reduce toxicity and improve therapeutic effect. In addition, the development of a single component of PME with low toxicit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/62G01N33/68
CPCC07K7/62G01N33/6848G01N2333/32
Inventor 张含智刘浩秦峰闻宏亮裘亚赵敬丹
Owner SHANGHAI INST FOR FOOD & DRUG CONTROL
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