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Pretreatment method for unstable compound

A compound and stable technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the instability of peptide compounds and other problems, achieve the effect of convenient and safe operation, improve extraction recovery rate, and reduce signal suppression

Pending Publication Date: 2022-04-12
南京药明康德新药开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problem of instability of peptide compounds in solution or matrix, and also improves the extraction recovery of compounds

Method used

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  • Pretreatment method for unstable compound
  • Pretreatment method for unstable compound
  • Pretreatment method for unstable compound

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Working solution concentration: 150ng / mL (peptide A low concentration LQC) and 4000ng / mL (polypeptide A, high concentration HQC);

[0041] 2. Matrix: rat plasma (containing 0.85% H 3 PO 4 , added before use);

[0042] 3. Compound concentration in matrix (50-fold dilution): 3.00ng / mL (A, LQC) and 800ng / mL (A, HQC);

[0043] 4. Internal standard: 100ng / mL (Verapamil);

[0044] 5. Place in a polypropylene tube at room temperature for 24 hours and at -80°C for 14 days;

[0045] 6. Prepare t0 samples;

[0046] 7. Refer to the above operation for extraction, see Table 1 and Table 2 for the results. The results in Table 1 and Table 2 show that polypeptide A is stable in SD rat plasma samples at room temperature for at least 24 hours. Stable for at least 14 days in an ultra-low temperature freezer (temperature set to -80°C). The chromatogram of polypeptide A in double blank SD rat plasma is shown in figure 1 ; The chromatogram of polypeptide A in single blank SD rat ...

Embodiment 2

[0053] 1. Working solution concentration: 150ng / mL (peptide A low concentration LQC) and 4000ng / mL (polypeptide A, high concentration HQC);

[0054] 2. Matrix: cynomolgus monkey plasma (containing 0.85% H 3 PO 4 , added before use);

[0055] 3. Compound concentration in matrix (50-fold dilution): 3.00ng / mL (A, LQC) and 800ng / mL (A, HQC);

[0056] 4. Internal standard: 100ng / mL (Verapamil);

[0057] 5. Place in a polypropylene tube at room temperature for 24 hours and at -80°C for 14 days;

[0058] 6. Prepare t0 samples;

[0059]7. Refer to the above operation for extraction, see Table 3 and Table 4 for the results. The results in Table 3 and Table 4 show that the polypeptide A is stable in the cynomolgus monkey plasma sample at room temperature for at least 24 hours. Stable for at least 14 days in an ultra-low temperature freezer (temperature set to -80°C).

[0060] table 3

[0061]

[0062] Table 4

[0063]

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Abstract

The invention discloses a pretreatment method for an unstable compound, which comprises the following steps: 1) after sampling, immediately adding a phosphoric acid solution according to a volume ratio of a sample to the phosphoric acid solution of 19: 1, the phosphoric acid solution being phosphoric acid to water according to a volume ratio of 17: 83; (2) a small amount of formic acid solution A is added in the pretreatment process to improve mass spectrum signals, the volume ratio of formic acid to water in the formic acid solution A is 3: 1000, and methanol is adopted as a precipitating agent for precipitation; the method provided by the invention solves the problem of operation inconvenience caused by the need of acid reinforcement in the operation process, and reduces the risk of operation. The phosphoric acid solution can solve the problem of low recovery rate of peptide extraction, and can stabilize peptide compounds. However, a phosphoric acid solution with a certain concentration usually affects mass spectrum response when entering mass spectrum. By using the phosphoric acid solution with the proportion, the signal response of a mass spectrometer is not influenced while the stability is solved and the extraction recovery rate is improved.

Description

technical field [0001] The invention relates to a pretreatment method for compounds, in particular to a pretreatment method for unstable compounds. Background technique [0002] In drug research, it is usually necessary to determine the drug concentration in various biological matrices such as plasma, urine, bile, cerebrospinal fluid, and tissue. Some samples are unstable due to the presence of compounds in the matrix that are degraded, oxidized, or react with components in the matrix. Factors lead to non-linear quantitative standard curves, which cannot be accurately quantified and affect the determination of real results. [0003] From the perspective of LC-MS bioanalysis, the main challenge of prodrugs is how to solve the instability of prodrugs, and these instabilities are in the sample before the collection, processing, storage and quantitative analysis of biological samples by LC-MS. can occur during preparation. Common measures to solve this problem at this stage ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
Inventor 赵欢张玲玲卢金莲高峥贞
Owner 南京药明康德新药开发有限公司