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A kind of preparation method of bacitracin impurity 1 based on photocatalysis

A bacitracin and photocatalytic technology, which is applied in the field of biochemistry, can solve the problems of low bacitracin impurity L content, unsuitable preparation method, and low preparation efficiency, and achieve the effects of simple post-processing, low cost, and simple steps

Active Publication Date: 2020-12-01
长沙晨辰医药科技有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0005] Introduced in the existing literature, Jon D.Epperson and Li-June Ming adopted the traditional reversed-phase HPLC method to directly separate the bacitracin impurity L from bacitracin (name in the literature: bacitracin A 2 ), the method adopts the fermentation sample to directly separate and prepare, the content of bacitracin impurity L in the sample is low, the overall preparation efficiency is very low, and the cost is very high, so it is not suitable as the preparation method of the impurity reference substance

Method used

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  • A kind of preparation method of bacitracin impurity 1 based on photocatalysis
  • A kind of preparation method of bacitracin impurity 1 based on photocatalysis
  • A kind of preparation method of bacitracin impurity 1 based on photocatalysis

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Effect test

Embodiment 1

[0027] Instruments: Preparative Liquid Phase (Waters 2525); Rotary Rotary Evaporator (Shanghai Yarong); Photochemical Reactor (Shanghai Julai Experimental Instrument Co., Ltd.).

[0028] Preparation of crude bacitracin impurity L: Dissolve 3 g of bacitracin raw material in 50 ml of ethanol, add 1 ml of trifluoroacetic acid to aid dissolution, and react for 2 hours at 50° C. with a light intensity of 5000 Lux in a photochemical reactor to obtain a content of impurity L of 30%. crude products. The above content is the content characterized by the HPLC area normalization method.

[0029] Preparative column: the filler is Kromasil EternityXT-10-C18, and the column tube is HB-DAC50.

[0030] Preparative liquid phase separation chromatographic conditions: carry out isocratic elution with 0.1% volume concentration trifluoroacetic acid aqueous solution-acetonitrile (70:30, V / V) as mobile phase; Flow rate is 100mL / min; Detection wavelength 254nm; Column temperature is Room temperatur...

Embodiment 2

[0046] Instruments: Preparative Liquid Phase (Waters 2525); Rotary Rotary Evaporator (Shanghai Yarong); Photochemical Reactor (Shanghai Julai Experimental Instrument Co., Ltd.).

[0047] Preparation of crude bacitracin impurity L: Dissolve 3 g of bacitracin raw material in 30 ml of methanol, add 1 ml of trifluoroacetic acid, and react at 50° C. for 3 hours in a photochemical reactor with light intensity of 4500 Lux to obtain a crude product with an impurity L content of 35%. . The above content is the content characterized by the HPLC area normalization method.

[0048] Preparative column: the filler is Kromasil EternityXT-10-C18, and the column tube is HB-DAC50.

[0049] Preparative liquid phase separation chromatographic conditions: carry out isocratic elution with 0.1% volume concentration trifluoroacetic acid aqueous solution-acetonitrile (70:30, V / V) as mobile phase; Flow rate is 100mL / min; Detection wavelength 254nm; Column temperature is Room temperature; manual injec...

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Abstract

The invention provides a preparation method of a bacitracin impurity L based on photocatalysis. The preparation method comprises the following steps: S1, dissolving a bacitracin raw material medicament in a solvent, and performing illuminating at 50-60 DEG C for 1-3h to obtain a crude product containing the bacitracin impurity L; and S2, separating the bacitracin impurity L from other components by adopting a preparation liquid phase, collecting a peak fraction of the bacitracin impurity L, and evaporating the collected peak fraction of the bacitracin impurity L to dryness to obtain a reference product of the bacitracin impurity L. According to the technical scheme of the invention, a photocatalytic chemical conversion method is adopted to convert bacitracin A into an epimer of the bacitracin A, namely an impurity L, under action of illumination, so that the steps are simple and convenient, efficiency is high, low-cost enrichment of an impurity crude product is realized, post-treatmentis simple, cost is low, and pollution is small.

Description

technical field [0001] The invention belongs to the technical field of biochemistry, and in particular relates to a method for preparing bacitracin impurity L based on photocatalysis. Background technique [0002] Bacitracin is fermented by Bacillus licheni formus. It has a strong antibacterial effect on most Gram-positive bacteria. Its antibacterial effect is similar to that of penicillin. It is also effective against penicillin-resistant Staphylococcus aureus. It is mainly used for the treatment of Various infections caused by drug-resistant Staphylococcus aureus, such as sepsis, pneumonia, endocarditis, etc. European Pharmacopoeia EP9.6 includes 17 related substances of A, B, C, D, E, F, G, H, I, J, K, L, M, N, O, P, Q, among which the impurity L The limit is 2.0%, and the impurity L is the D-alloisoleucine epimer of bacitracin A, its chemical structure is shown below, which has an important impact on the safety and effectiveness of the drug. [0003] [0004] In rec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/58C07K1/14
CPCC07K7/58
Inventor 张根
Owner 长沙晨辰医药科技有限公司
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