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Detection method for brivaracetam and related substances thereof

A detection method and related substance technology, applied in the field of analysis and detection, can solve the problems of clinical drug safety risks, inaccurate results, difficult to separate, etc., and achieve the effects of reducing the risk of clinical drug use, high analytical sensitivity, and accurate and reliable results

Active Publication Date: 2020-02-21
北京海晶生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventors found that the polarity of individual impurities related to briracetam was very different, and it was easy to miss detection; the polarity difference between individual impurities and briracetam was very small, so it was difficult to separate, resulting in inaccurate results and potential safety for clinical medication. sexual risk

Method used

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  • Detection method for brivaracetam and related substances thereof
  • Detection method for brivaracetam and related substances thereof
  • Detection method for brivaracetam and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1 mobile phase and chromatographic column screening

[0047] Take blank solvent, mixed reference substance solution, and 10 μl of sensitivity solution, inject them into the liquid chromatograph, record the chromatogram, and complete the determination.

[0048] The chromatographic detection conditions and detection results are shown in Table 1 and attached Figure 1-4 wherein the buffer solution contains phosphate and cation-pairing reagent, the concentration of phosphate is 0.01mol / L, and the concentration of cation-pairing reagent is shown in Table 1; Alkylsilane bonded silica gel, phenyl chromatographic column is phenylsilane bonded silica gel chromatographic column, amino chromatographic column is aminosilane bonded silica gel chromatographic column, gradient elution program is shown in Table 2.

[0049] Among them, the test result marks are as follows:

[0050] Ⅰ All impurities cannot be completely separated from the main peak of Brivaracetam or the sol...

Embodiment 2

[0060] Example 2 pH value screening

[0061] Take blank solvent, mixed reference substance solution, and 10 μl of sensitivity solution, inject them into the liquid chromatograph, record the chromatogram, and complete the determination.

[0062] Chromatographic conditions: Shimadzu LC-20AT high-performance liquid chromatograph is used, the chromatographic column is Waters Xbridge shield RP18 (4.6×150mm, 3.5μm), the column temperature is 40°C, the ultraviolet detector is used, and the detection wavelength is 200nm; - buffer salt (2:98) is mobile phase A, with acetonitrile-buffer salt (98:2) as mobile phase B, flow rate is 1.5ml / min, buffer solution is sodium heptanesulfonate containing 0.005mol / L and The aqueous solution of 0.001 mol / L acetate was subjected to gradient elution according to the procedure in Table 2, and the selection and detection results of the pH value are shown in Table 3-7.

[0063] Among them, the test result marks are as follows:

[0064] Ⅰ All impurities...

Embodiment 3

[0082] Take blank solvent, mixed reference substance solution, and 10 μl of sensitivity solution, inject them into the liquid chromatograph, record the chromatogram, and complete the determination.

[0083] Chromatographic conditions: Shimadzu LC-20AT high performance liquid chromatograph is used, the column temperature is 40°C, the ultraviolet detector is used, and the detection wavelength is 200nm; acetonitrile-buffer salt (3:97) is used as mobile phase A, and acetonitrile -buffer salt (98:2) is mobile phase B, and flow rate is 1.5ml / min, and buffer solution is the citrate aqueous solution that comprises the sodium heptanesulfonate of 0.003mol / L and 0.1mol / L, and pH value is 3, The gradient elution conditions are shown in Table 8, and the results of the mixed control sample solution are shown in Table 9.

[0084] Table 8: Gradient elution conditions of embodiment 3

[0085]

[0086]

[0087] Table 9: Example 3 Mixed Reference Substance Solution Detection Result Table ...

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Abstract

The invention relates to a detection method for brivaracetam and related substances thereof. The detection method comprises a step of adopting high performance liquid chromatography to perform detection. The following liquid chromatography conditions are adopted: a reverse chromatographic column is adopted; a mobile phase A is a mixed solution of acetonitrile and a buffer solution in a volume ratio of (0-5):(95-100); a mobile phase B is a mixed solution of acetonitrile and a buffer solution in a volume ratio of (95-100):(0-5), and gradient elution is performed; the buffer solution contains 0.001 mol / L-0.1mol / L of a cationic ion pair reagent and 0.001 mol / L-0.1mol / L of buffer salt; and the pH value of the buffer solution is lower than 6. The detection method provided by the invention can realize full separation of brivaracetam and related substances thereof, is high in analysis sensitivity and accurate and reliable in result, can effectively improve the drug quality control level and safety of brivaracetam and reduces the risk of drug use.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a detection method of briracetam and related substances thereof. Background technique [0002] The molecular formula of "Brivaracetam" is C 11 h 20 N 2 o 2 , the English name is Brivaracetam, the CAS number is 357336-20-0, and the structural formula is shown in formula 1. It is a third-generation antiepileptic drug developed by UCB Company in Belgium. The trade name is For the treatment of partial-onset epilepsy patients 16 years of age and older, adjuvant therapy with or without secondary generalized seizures. [0003] [0004] In the process of synthesizing the compound, the by-products that are brought into the subsequent reaction due to the incomplete reaction of the key intermediates and the starting materials, the reaction by-products caused by the low purity of the starting materials, and the degradation of the drug itself The degradatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89G01N30/74G01N30/54
CPCG01N30/89G01N30/74G01N30/54Y02P20/55
Inventor 曹相林夏瑞曹丽娜孟杰商丹丹
Owner 北京海晶生物医药科技有限公司
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