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Determination method of edetate disodium in clevidipine butyrate injection emulsion

A technology of clevidipine butyrate and edetate disodium, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., and can solve problems such as the inability to achieve quality control of EDTA-2Na

Active Publication Date: 2018-12-04
TIANJIN INSTITUTE OF PHARMA RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When this method measures EDTA-2Na, the concentration of EDTA-2Na in the solution should reach 10mg·mL -1 , unable to achieve quality control of trace amounts of EDTA-2Na

Method used

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  • Determination method of edetate disodium in clevidipine butyrate injection emulsion
  • Determination method of edetate disodium in clevidipine butyrate injection emulsion
  • Determination method of edetate disodium in clevidipine butyrate injection emulsion

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Experimental program
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Effect test

Embodiment 1

[0050] 1. Instruments and reagents

[0051] 1.1 Instrument: High performance liquid chromatography is AgiLent 1200Series; chromatographic column is InertsiL ODS-3, purchased from GL Science Inc.; electronic analytical balance is METTLER TOLEDO XS205;

[0052] 1.2 Reagents: Acetonitrile is chromatographically pure, water is ultrapure water, and other reagents are analytically pure.

[0053] 1.3 Drugs: Blank clevidipine butyrate injection emulsion is from Tianjin Kanghong Pharmaceutical Technology Development Co., Ltd.;

[0054] Clevidipine butyrate injection emulsion was purchased from Medicines Co., batch number: 16GF0226;

[0055] Edetate disodium was purchased from USP standard, batch number: JOJ421.

[0056] 2. Chromatographic conditions and system adaptability: octadecylsilane bonded silica gel is used as filler;

[0057] Mobile phase: A phase and B phase composed of organic phase and aqueous phase respectively;

[0058] Wherein: A phase is the tetrabutylammonium hydro...

Embodiment 2

[0098] The control experiment of embodiment 2 sample processing

[0099]Three batches of clevidipine butyrate injection emulsion (batch numbers: 1312102131-1, 1312112131, 1312122131) were taken, and the content of edetate disodium was determined according to the following conditions.

[0100] The chromatographic column adopting octadecylsilane bonded silica gel as filler; mobile phase A phase is 25mmoL / L tetrabutylammonium hydroxide solution (adjust pH6.4 with phosphoric acid)-acetonitrile volume ratio is 4:1, mobile phase Phase B is a methanol-water volume ratio of 9:1, and the gradient elution program is shown in Table 1. The detection wavelength is 254nm, the flow rate is 1.0mL / min, the column temperature is 35°C, and the injection volume is 50μL.

[0101] Sample processing method:

[0102] 1) Precisely measure 1 mL of 500 μg / mL edetate disodium solution, put it in a 50 mL centrifuge tube, add 9 mL of blank clevidipine butyrate injection emulsion, and precisely add isop...

Embodiment 3

[0109] Embodiment 3 chromatographic conditions optimization

[0110] Three batches of clevidipine butyrate injection emulsion (batch numbers: 1312102131-1, 1312112131, 1312122131) were taken, and the content of edetate disodium was determined according to the following conditions.

[0111] Chromatographic conditions: a chromatographic column using octadecylsilane bonded silica gel as a filler; the detection wavelength is 254nm, the flow rate is 1.0mL / min, the column temperature is 35°C, and the injection volume is 50μL.

[0112] (1) Gradient elution: mobile phase A is 25mmoL / L tetrabutylammonium hydroxide solution (adjust pH 6.4 with phosphoric acid)-acetonitrile volume ratio is 4:1, mobile phase B is methanol-water volume ratio is 9:1, the gradient elution program is shown in Table 1.

[0113] (2) Isocratic elution: mobile phase is 25mmoL / L tetrabutylammonium hydroxide solution (adjust pH 6.4 with phosphoric acid)-acetonitrile-isopropanol volume ratio is 6:3:1, isocratic e...

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Abstract

The invention provides a preparation method of a sample used for HPLC detection of disodium edetate in a clevidipine butyrate injection emulsion. The preparation method comprises the following steps: adding an isopropanol and n-hexane mixed liquid into the clevidipine butyrate injection emulsion, shaking the mixed liquid and the emulsion, centrifuging the obtained solution, taking obtained water phase, and adding a metal ion salt solution able to complex edetic acid to form a complex in order to form a sample solution. The invention also provides a method for detecting disodium edetate in the clevidipine butyrate injection emulsion. The detection method is an HPLC method. An oil phase and a water phase in the clevidipine butyrate injection emulsion are effectively separated to make disodium edetate dissolved in the water phase be accurately detected. The detection method has the advantages of high detection sensitivity, good precision and high specificity, and is an effective method for strictly controlling the content of disodium edetate in the clevidipine butyrate injection emulsion.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a detection method for edetate disodium in clevidipine butyrate injection emulsion Background technique [0002] Clevidipine Butyrate Injectable Emulsion is the third generation of new short-acting dihydropyridine calcium channel blocker developed by AstraZeneca in the United Kingdom. An appropriate amount of edetate disodium (EDTA-2Na) is added into the preparation as a complexing agent and an antioxidant. Clinical studies have confirmed that edetate disodium can interact with Ca 2+ It forms a metal chelate with good water solubility. Large doses or too fast intravenous injection can easily lead to loss of bone calcium or hypocalcemia. Therefore, it is very important to monitor the content of edetate disodium in clevirdine butyrate injection emulsion . It is generally believed that the safe and effective concentration of EDTA-2Na in injection emulsion is 0.005-0.1mg·mL -1 . [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 王彦竹刘钫王杏林孙歆慧宋丽明邹美香
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
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