(2s,5r)-phenoxyaminopiperidine-2-carboxamide detection method
A phenoxyaminopiperidine, detection method technology, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve problems such as undiscovered, and achieve the effects of simple operation and high sensitivity
Active Publication Date: 2021-03-02
ENANTIOTECH CORP
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Problems solved by technology
[0004] At present, there are no relevant literatures and reports on the chiral purity detection method of (2S, 5R)-phenoxyaminopiperidine-2-carboxamide. -Formamide quality control requires the development of a detection method for (2S,5R)-phenoxyaminopiperidine-2-carboxamide, especially the detection method for its chiral purity
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Embodiment 1
[0045] A detection method for (2S,5R)-phenoxyaminopiperidine-2-carboxamide
[0046] 1. Instruments and testing conditions
[0047] Shimadzu LC-15C high-performance liquid chromatograph uses chiralcel AD-H as the chromatographic column, and the specification of the chromatographic column is 4.6*250mm, 5μm. That is, the filler particle size of the chromatographic column is 5 μm, the pore diameter is 4.6 mm, and the column length of the chromatographic column is 250 mm. Flow rate: 1.0ml / min; Column temperature: 25°C; Detection wavelength: 210nm; Detector: UV detector, injection volume: 20μl.
[0048] Mobile phase: n-hexane: absolute ethanol: isopropanol: diethylamine, the volume ratio is 850:150:50:0.5;
[0050] 2. Experimental steps
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Abstract
The invention discloses a method for detecting (2S, 5R)-phenoxyamidopiperidine-2-methanamide. According to the detection method, a high performance liquid chromatograph (HPLC) is adopted, and an areanormalization method is adopted for quantitative analysis. The chromatographic condition includes: the chromatographic column is chiralcel AD-H; the sample size is 15-25 [mu]l; the flow velocity is 0.8-1.2 ml / min; the temperature of the column is 10-40 DEG C; the detection wavelength is 208-212 nm; the mobile phase comprises hexane, absolute ethanol, isopropanol and diethylamine at a volume ratioof (820-880):150:50:0.5; and the detector is an ultraviolet detector. Through the detection method, (2S, 5R)-phenoxyamidopiperidine-2-methanamide can be fast accurately measured. The method is high insensitivity and simple to operate, and allows total separation to be achieved. The method provides basis for research, development and quality detection of the kind of (2S, 5R)-phenoxyamidopiperidine-2-methanamide.
Description
technical field [0001] The invention relates to a detection method of an avibactam sodium intermediate, belongs to the technical field of drug analysis, and specifically relates to a detection method of (2S, 5R)-phenoxyaminopiperidine-2-carboxamide. Background technique [0002] (2S,5R)-phenoxyaminopiperidine-2-carboxamide, its CAS number is 1416134-49-0, is an important intermediate for the production of Avibactam sodium, its chiral purity, isomerism Isomeric impurities directly affect the chiral purity of avibactam sodium, the amount of isomer impurities, thereby directly affecting the curative effect of avibactam sodium medicine. [0003] Chemical name of avibactam sodium: [(1R,2S,5R)-2-(aminocarbonyl)-7-oxo-1,6-diazabicyclo[3.2.1]oct-6-yl]sulfuric acid Monoester, which belongs to diazabicyclooctone compound, is currently the most promising new type of β-lactamase inhibitor. Compared with the three marketed β-lactamase inhibitors, it has a long-acting and reversible cov...
Claims
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IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 蒙发明曹欢燕徐亮邓超芹俞伟文樊志麒
Owner ENANTIOTECH CORP