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High-efficiency liquid phase analysis method of diethylphosphonoacetic acid

A technology for diethylphosphoric acetic acid and high-performance liquid phase analysis, which is applied in the directions of analyzing materials, material separation, and measuring devices to achieve the effects of stable retention time, good accuracy and stability, and low equipment requirements

Active Publication Date: 2017-06-30
JIANGSU WANBANG BIOPHARMLS
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Problems solved by technology

At present, there is no literature report on the relevant analysis method for diethylphosphonoacetic acid. In order to ensure the quality of production and research and development, it is necessary to control its quality. more urgent and important

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  • High-efficiency liquid phase analysis method of diethylphosphonoacetic acid

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Embodiment 1

[0022] Embodiment 1: Chromatographic purity determination

[0023] According to high performance liquid chromatography (Chinese Pharmacopoeia 2010 edition two appendix V D) determination.

[0024] Chromatographic conditions and system suitability test use octadecyl bonded silica gel as filler; use 0.02 mol / L potassium dihydrogen phosphate (adjust the pH value to 3.0 with phosphoric acid)-acetonitrile (90:10) as mobile phase A, 0.02 mol / L potassium dihydrogen phosphate (adjust the pH value to 3.0 with phosphoric acid)-acetonitrile (20:80) as the mobile phase B, the elution procedure is shown in Table 1, the detection wavelength is 210nm, the flow rate is 0.8 ml / min, the column temperature is 30°C. Take an appropriate amount of diethylphosphonoacetic acid reference substance, dissolve and dilute it with 10% acetonitrile to make a solution containing about 5mg per 1ml, as the reference substance solution. Precisely measure 20 μl each of the blank solution and the reference solu...

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Abstract

The invention discloses a high-efficiency liquid phase analysis method of diethylphosphonoacetic acid. The high-efficiency liquid phase analysis method is characterized by specifically comprising the following steps of using 10% acetonitrile to dissolve and dilute the diethylphosphonoacetic acid into a solution which contains 0.5mg to 50mg of diethylphosphonoacetic acid per ml, wherein the solution is used as a test sample solution, filling a high performance liquid chromatograph with the solution, and setting the sampling volume to 1 to 100mu l; by utilizing an ultraviolet detector with detection wavelength of 200 to 230nm, using an acetonitrile-phosphate solution as a flowing phase with the flow rate of 0.5 to 3.0ml / min and using a fixed-phase octadecyl silane chromatographic column with column temperature of 30 DEG C, measuring the chromatographic purity of the diethylphosphonoacetic acid; according to a peak area, calculating the purity and content of a sample. The high-efficiency liquid phase analysis method for measuring has the advantages that the method is simple, the precision is high, the stability is good, and the reoccurrence is good.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and relates to a high-efficiency liquid phase analysis method of diethylphosphonoacetic acid. Background technique [0002] Diethylphosphonoacetic acid CAS number is 3095-95-2, molecular formula: C 6 h 13 o 5 P, molecular weight: 196.14, structural formula as follows: [0003] . [0004] Clear or yellow viscous liquid used to provide phosphonate intermediates for intramolecular HEW reactions. At present, there is no literature report on the relevant analytical methods for diethylphosphonoacetic acid. In order to ensure the quality of production and research and development, it is necessary to control its quality. It is particularly urgent and important. Contents of the invention [0005] The purpose of the present invention is to provide a kind of good stability, good reproducibility, simple operation, can carry out the assay method to diethylphosphonoacetic acid chromatographic p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 苗瑞娜刘跃跃林彬乔德水高雪芹
Owner JIANGSU WANBANG BIOPHARMLS
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