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Method for quantitative determination of PSMA key intermediate chiral isomer

A technology for quantitative determination of chiral isomers, which is applied in the field of chemical medicine and can solve the problems of low column efficiency, difficult to effectively separate chiral isomers, and effective separation of chiral isomers of difficult compounds.

Pending Publication Date: 2021-09-14
SUZHOU IBIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] It is difficult to effectively separate the chiral isomers of the compound (Formula 2) by using conventional chiral columns and high-performance liquid chromatography with conventional mobile phases. The peak shape is poor and the column efficiency is very low.
Chiral isomers are difficult to be effectively separated by general high-performance liquid chromatography, and appropriate detection methods must be used to achieve the purpose of analysis and separation

Method used

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  • Method for quantitative determination of PSMA key intermediate chiral isomer
  • Method for quantitative determination of PSMA key intermediate chiral isomer
  • Method for quantitative determination of PSMA key intermediate chiral isomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: water: acetonitrile: the HPLC detection of trifluoroacetic acid=50:50:0.1 blank solvent

[0034] 1. Instruments and conditions

[0035] Instrument: Thermo U3000 High Performance Liquid Chromatograph

[0036] Chromatographic column: CHIRALCEL OD-R (specification 4.6×250mm, 5um)

[0037] Mobile phase: A phase: 0.1% trifluoroacetic acid aqueous solution B phase: 0.1% trifluoroacetic acid acetonitrile solution

[0038] Detection wavelength: 220nm

[0039] Flow rate: 1.0mL / min

[0040] Column temperature: 30°C

[0041] Injection volume: 10uL

[0042] Elution gradient: 40% B ~ 80% B, elution time: 0 ~ 20min

[0043] 2. Experimental steps

[0044] The injection volume is 10uL of water: acetonitrile: trifluoroacetic acid = 50:50:0.1 blank solvent, carry out liquid chromatography analysis according to the above chromatographic conditions, record the chromatogram, the results are shown in figure 1 .

[0045] The results of this test method figure 1 It is o...

Embodiment 2

[0046] Embodiment 2: the HPLC detection of compound (formula 2) isomer (A+B) solution

[0047] 1. Instruments and conditions

[0048] Instrument: Thermo U3000 High Performance Liquid Chromatograph

[0049] Chromatographic column: CHIRALCEL OD-R (specification 4.6×250mm, 5μm)

[0050] Mobile phase: A phase: 0.1% trifluoroacetic acid aqueous solution B phase: 0.1% trifluoroacetic acid acetonitrile solution

[0051] Detection wavelength: 220nm

[0052] Flow rate: 1.0mL / min

[0053] Column temperature: 30°C

[0054] Injection volume: 10uL

[0055] Elution gradient: 40% B ~ 80% B, elution time: 0 ~ 20min

[0056] Wherein, the structural formulas of A and B are as follows:

[0057]

[0058]

[0059] 2. Experimental steps

[0060]Take compound (formula 2) isomer A reference substance 10mg, accurately weighed, place in a 10mL volumetric flask, add an appropriate amount of diluent to dissolve and dilute to the mark, and make a solution containing 1mg of reference substanc...

Embodiment 3

[0063] Embodiment 3: the HPLC detection of compound (formula 2) isomer B solution

[0064] 1. Instruments and conditions

[0065] Instrument: Thermo U3000 High Performance Liquid Chromatograph

[0066] Chromatographic column: CHIRALCEL OD-R (specification 4.6×250mm, 5μm)

[0067] Mobile phase: A phase: 0.1% trifluoroacetic acid aqueous solution, B phase: 0.1% trifluoroacetic acid acetonitrile solution

[0068] Detection wavelength: 220nm

[0069] Flow rate: 1.0mL / min

[0070] Column temperature: 30°C

[0071] Injection volume: 10uL

[0072] Elution gradient: 40% B-80% B, elution time: 0-20min

[0073] 2. Experimental steps

[0074] Take 10 mg of compound (formula 2) isomer B reference substance, accurately weigh it, place it in a 10 mL volumetric flask, add an appropriate amount of diluent to dissolve and dilute to the mark, and make a compound (formula 2) containing 0.5 mg per 1 mL of solution The solution of the isomer B reference substance is used as the compound (f...

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Abstract

The invention provides a method for quantitative determination of a PSMA key intermediate chiral isomer. The method is a reversed-phase high performance liquid chromatography, and the chromatographic conditions are that a polysaccharide coated reversed-phase chiral column is adopted, the chiral column is CHIRALCEL OD-R, water, acetonitrile and trifluoroacetic acid in a ratio of 50: 50: 0.1 are used as a diluent, the column temperature of the chiral column is 30 DEG C, a phase A, namely a 0.1% trifluoroacetic acid aqueous solution, and a phase B, namely a 0.1% trifluoroacetic acid acetonitrile solution are used as mobile phases, the flow velocity of the mobile phases is 1.0 mL / min, and the detection wavelength of liquid chromatography is 220nm. The method has the beneficial effects that the method can efficiently and accurately realize separation and determination of the chiral isomer of the PSMA key intermediate, the chiral isomer of the PSMA key intermediate can be rapidly and accurately analyzed, the peak shape is relatively good, and the separation degree conforms to the specification so that the quality of the PSMA key intermediate is effectively controlled. The method is high in separation degree, good in specificity, high in sensitivity and easy and convenient to operate.

Description

technical field [0001] The invention belongs to the technical field of chemistry and medicine, and in particular relates to a method for quantitatively determining the chiral isomer of a key intermediate of PSMA. Background technique [0002] Prostate-specific membrane antigen (PSMA) is a type II cell surface membrane-bound glycoprotein with a molecular weight of about 110kD, including an intracellular fragment (amino acid sequence 1-18), a transmembrane domain (amino acid sequence 19-43), and an extracellular domain (amino acid sequence 44-750). The intracellular fragment and the transmembrane domain are now considered to have no significant role, while the extracellular domain is involved in a variety of specific activities. PSMA plays a very important role in the nervous system, it promotes the metabolism of N-acetylaspartamine (NAAG) and generates glutamic acid and N-acetylaspartic acid. Correspondingly, it is also sometimes related to N-acetyl α-linked acid dipeptidas...

Claims

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Application Information

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IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 黄保华胡新礼刘晓栋戴建
Owner SUZHOU IBIO TECH CO LTD
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