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A kind of polymyxin e component and its photochemical product and liquid chromatography-mass spectrometry analysis method

A polymyxin, photochemical technology, applied in the field of medicinal chemistry and pharmaceutical analytical chemistry, to achieve the effect of easy promotion

Active Publication Date: 2022-04-19
SHANGHAI INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still undiscovered PME components

Method used

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  • A kind of polymyxin e component and its photochemical product and liquid chromatography-mass spectrometry analysis method
  • A kind of polymyxin e component and its photochemical product and liquid chromatography-mass spectrometry analysis method
  • A kind of polymyxin e component and its photochemical product and liquid chromatography-mass spectrometry analysis method

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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 (Polymyxin E, PME) component and its photochemical product and liquid chromatography-mass spectrometry analysis method; wherein, the polymyxin E component includes a polymyxin E double bond Chemical components, specifically including polymyxin E1 double bond components and polymyxin E2 double bond components, these components are analyzed by high performance liquid chromatography-mass spectrometry (HPLC-MS) and secondary mass spectrometry Verify that the double bond is at the end of the N‑fatty acyl chain. The double-bonded component obtains a photochemical product through a photochemical reaction, that is, a Paternobig reaction (reaction), under the condition that acetone is used as a reaction reagent, and this type of product is verified as a [2+2] cycloaddition product by HPLC-MS ; The above-mentioned double bond components are named 7'-alkenyl polymyxin E1 and 6'-alkenyl polymyxin E2. The double-bonded components of polymyxin E may have antibacterial activity or toxicity different from that of common polymyxin E components, which has potential application value, and the structural confirmation of such compounds is also a basis for strict control of polymyxin E. The quality provides the basis for research.

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 Patents(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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