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Analytical method for determining cycloheptatriene peptide anthelmintic intermediates

An intermediate, volume ratio technology, applied in the field of pharmaceutical analysis, can solve the problem of ineffective separation of p-m

Pending Publication Date: 2021-11-23
CHONGQING QIANTAI BIOLOGICAL MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The process of obtaining Amodex intermediate 1 from PF1022A through nitration is the key process to increase the yield of the finished product. As the target product, p-p cannot be effectively separated from p-m under the existing method

Method used

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  • Analytical method for determining cycloheptatriene peptide anthelmintic intermediates
  • Analytical method for determining cycloheptatriene peptide anthelmintic intermediates
  • Analytical method for determining cycloheptatriene peptide anthelmintic intermediates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] High performance liquid chromatography: LC-2030C

[0040] Chromatographic column: phenylsilane bonded silica gel column (Agilent ZORBAX SB-Phenyl 4.6×75mm 3.5um)

[0041] Mobile phase: 0.1% phosphoric acid aqueous solution is mobile phase A; acetonitrile is mobile phase B

[0042] The elution procedure of mobile phase A and B is:

[0043]

[0044] Flow rate: 1.0ml / min

[0045] Wavelength: 210nm

[0046] Injection volume: 10ul

[0047] Column temperature: 40°C

[0048] Implementation steps:

[0049] Test solution: Take Emeralds intermediate 1 and make a solution with a concentration of about 1.0mg / ml

[0050] Take 10 μl of the test solution and inject it into the liquid chromatograph, and record the chromatogram. see attached results figure 1 .

Embodiment 2

[0052] High performance liquid chromatography: LC-2030C

[0053] Chromatographic column: Octylsilane bonded silica gel column (Agilent ZORBAX SB-C8 4.6×150mm 3.5um)

[0054] The flow is the same as Example 1;

[0055] The elution procedure of mobile phase A and B is:

[0056]

[0057]

[0058] Flow velocity, wavelength, injection volume and column temperature are the same as in Example 1

[0059] Implementation steps:

[0060] Get the need testing solution 10 μ l of Example 1 and inject into the liquid chromatograph, record the chromatogram. see attached results figure 2 .

Embodiment 3

[0062] High performance liquid chromatography: LC-2030C

[0063]Chromatographic column: octadecylsilane bonded silica gel column ( C18, 4.6mm×250mm, 5μm)

[0064] The flow is the same as Example 1;

[0065] The elution procedure of mobile phase A and B is:

[0066]

[0067] Flow velocity, wavelength, injection volume and column temperature are the same as in Example 1

[0068] Implementation steps:

[0069] Get the need testing solution 10 μ l of Example 1 and inject into the liquid chromatograph, record the chromatogram. see attached results image 3 .

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Abstract

The invention relates to a method for determining purity and impurities of an emodepside intermediate 1 through high performance liquid chromatography, and relates to the technical field of medicines. According to the technical scheme, a sample is prepared into a test solution by a proper method, methanol-tetrahydrofuran-water is taken as a mobile phase, a main component, namely, an emodepside intermediate 1 and related impurities are separated on a pentafluorophenyl bonded silica gel column, and an ultraviolet detector is used for detection. The method can be used for effectively separating the isomer of the emodepside intermediate 1, and the efficiency of optimizing the emodepside process is improved.

Description

technical field [0001] The invention belongs to the technical field of medical analysis, and in particular relates to an analysis method for determining the intermediate 1 of Amedes. Background technique [0002] Amedex (PF 1022-221) is a cycloheptatriene peptide with broad-spectrum anthelmintic activity. Its structural formula is as follows: [0003] [0004] Amodex intermediate 1 is an intermediate produced in the first step of the synthesis of Amodex, which is obtained by nitration of PF1022A. Its structure is as follows: [0005] [0006] The reaction system of the nitration process is very complex, and the products include regioselective products in addition to incompletely converted intermediates in the nitro reduction process. Patent WO2019040585A1 defines the regioselective products of nitration reaction, mainly: p-p, p-m, m-m, o-m products of the two benzene rings of PF1022A. Its structure is as follows: [0007] p-p [0008] [0009] p-m [0010] ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/30G01N30/32G01N30/34G01N30/74G01N30/86
Inventor 周莹易中宏吴禄春张有理
Owner CHONGQING QIANTAI BIOLOGICAL MEDICINE
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