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Ion chromatography separation integral pulse amperometric detection and analysis method for diphosphonate medicine

A technology of bisphosphonate and ion chromatography, which is applied in the field of ion chromatography separation and integral pulse amperometric detection and analysis of bisphosphonate drugs, can solve the problems of complex steps, unstable derivatives, time-consuming and other problems, and achieve simplification of the process flow Effect

Inactive Publication Date: 2014-06-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disadvantages of derivatization reactions include its complex steps, time-consuming, and the possibility that its derivatives are unstable

Method used

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  • Ion chromatography separation integral pulse amperometric detection and analysis method for diphosphonate medicine
  • Ion chromatography separation integral pulse amperometric detection and analysis method for diphosphonate medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0033] This example is to analyze and detect the content of bisphosphonate drugs in human plasma

[0034] Instruments used: DX-600 ion chromatograph (Dionex, USA), GP50 gradient pump, LC25 chromatographic column thermostat and ED50A electrochemical detector; DionexAG18 (50mm×2mm) and AS18 (250mm×2mm) anion exchange columns, 10μL Quantitative loop; flow rate: 0.25mL / min; column temperature: 30°C; injection volume: 10μL;

[0035] Detection method: integral pulse ampere detection, waveform setting: T1: 0.00-0.04s, E1 = -0.3V; T1: 0.05-0.21s, E2 = -0.15V; T3: 0.22-0.46s, E3 = 0.22V; T4 : 0.47-0.56s, E4=-0.15V; T5: 0.57-0.58s, E5=-2.00V; T6: 0.59, E6=0.6V, integral interval: 0.21-0.56s.

[0036] Data processing: Chameleon software of Chrome 6.8;

[0037] Eluent: 24mM NaOH solution;

[0038] Analysis steps:

[0039] (1) Actual sample processing: Dilute plasma with deionized water, add acetonitrile to precipitate protein, mix and vortex for 1 min, centrifuge at 1000 rpm for 10 mi...

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Abstract

The invention relates to an ion chromatography separation and analysis method for diphosphonate medicine, particularly to an ion chromatography separation pulse amperometric detection and analysis method for isocratic separation integral pulse amperometric detection and analysis method, which includes the following steps as actual sample treating, baseline surveying, sample injecting and ion exchange, elution and electrochemistry detection and analysis. The method can excellently separates and analyzes the diphosphonate medicine, saves time, enables the relative standard deviation of the peak height and peak area to be less than 2.0%, greatly simplifies the process flow, and can also be used for the detection of the diphosphonate medicine in the blood sample.

Description

technical field [0001] The present invention relates to the ion chromatographic separation and analysis method of bisphosphonate drugs (including alendronic acid, pamidronic acid, ibandronic acid and risedronic acid), in particular to the dual An analysis method for ion chromatographic separation and integral pulsed amperometric detection of phosphonate drugs. Background technique [0002] Bisphosphonates are a class of compounds that are widely used to treat skeletal disorders, including hypercalcemia malignant, osteoporosis, and Paget's disease. This type of compound has a P-C-P structure, and a carbon atom is connected between two phosphoric acid groups. Bisphosphonates such as alendronate, pamidronic acid, ibandronate, and risedronate are polar compounds. This makes it difficult to retain on non-polar stationary phases such as C18 or C8 columns. Due to the lack of chromophores, there is no UV absorption and fluorescence is not easy to detect. Because of its low volati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/12
Inventor 刘玉秀陈梅兰陈智栋朱岩
Owner ZHEJIANG UNIV