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Method for measuring content of tetrabutylammonium bromide in organic drug

A technology of tetrabutylammonium bromide and organic drugs, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of low penetration rate of instruments, unfriendly environment, poor specificity, etc., achieves strong specificity, avoids Long analysis time, good reproducibility

Active Publication Date: 2015-06-03
CHONGQING PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Poor specificity: ion chromatography, bromide ion selective electrode method, etc. may be interfered by other bromine-containing compounds remaining in the drug;
[0009] Not friendly enough to the environment: due to the use of methanesulfonic acid in ion chromatography and the use of N,N-dimethylformamide in bromide ion selective electrode method, these reagents are highly toxic
[0010] At the same time, UPLC-MS / MS and ion chromatography still have the disadvantages of low instrument penetration rate and high cost of use.
[0011] But the method that adopts high performance liquid chromatography to measure tetrabutylammonium bromide content in relevant organic medicine has no report

Method used

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  • Method for measuring content of tetrabutylammonium bromide in organic drug
  • Method for measuring content of tetrabutylammonium bromide in organic drug
  • Method for measuring content of tetrabutylammonium bromide in organic drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Instruments and Conditions

[0051] High performance liquid chromatography: Agilent 1260;

[0052] Chromatographic column: Octadecylsilane bonded silica gel as filler (AichromBond-AQ C18 4.6 mm×250mm, 5μm);

[0053] The mobile phase A is the aqueous phase: 0.005mol / L tetramethylammonium hydroxide solution, the pH value is adjusted to 3.0 with phosphoric acid, and the mobile phase B is the organic phase: acetonitrile.

[0054] Elute according to the gradient elution table (see Table 1) (after 5 minutes, it is the equilibrium system stage).

[0055]

[0056] Injection volume: 20μl;

[0057] Column temperature: 30°C;

[0058] Detection wavelength: 210nm.

[0059] Experimental procedure

[0060] Take about 400 mg of the crude drug canagliflozin, accurately weigh it, put it in a 10ml volumetric flask, add acetonitrile aqueous solution (acetonitrile:water=90:10v / v, the same below) to dissolve and dilute to the mark, shake well, and serve as Test solution. Take about...

Embodiment 2

[0063] Instruments and Conditions

[0064] High performance liquid chromatography: Agilent 1260;

[0065] Chromatographic column: Octadecylsilane bonded silica gel as filler (AichromBond-AQ C18 4.6 mm×250mm, 5μm);

[0066] Mobile phase A: aqueous phase 0.005mol / L tetramethylammonium hydroxide solution, adjust the pH value to 3.0 with phosphoric acid, mobile phase B: acetonitrile;

[0067] Elute according to the gradient elution table (see Table 2) (after 5 min, it is the equilibrium system stage).

[0068]

[0069] Injection volume: 20μl;

[0070] Column temperature: 30°C

[0071] Detection wavelength: 210nm.

[0072] Experimental procedure

[0073] Take about 400mg of the crude drug of canagliflozin, weigh it accurately, put it in a 10ml volumetric flask, add an appropriate amount of tetrabutylammonium bromide solution accurately, add acetonitrile aqueous solution to dissolve and dilute to make tetrabutylammonium bromide in every 1ml 4 μg of the mixed solution, shake...

Embodiment 3

[0075] Instruments and Conditions

[0076] High performance liquid chromatography: Agilent 1260;

[0077] Chromatographic column: Octadecylsilane bonded silica gel as filler (AichromBond-AQ C18 4.6 mm×250mm, 5μm);

[0078] Mobile phase A: aqueous phase 0.005mol / L tetramethylammonium hydroxide solution, adjust the pH value to 2.0 with phosphoric acid, mobile phase B: acetonitrile;

[0079] Elute according to the gradient elution table (see Table 3) (after 5 min, it is the equilibrium system stage).

[0080]

[0081] Injection volume: 20μl;

[0082] Column temperature: 30°C.

[0083] Experimental procedure

[0084] Take about 10 mg of tetrabutylammonium bromide reference substance, accurately weigh it, put it in a 25ml volumetric flask, add acetonitrile aqueous solution to dissolve and dilute to the mark, shake well, and use it as a stock solution. Take 500mg of Empagliflozin crude drug, accurately weighed, put in a 10ml volumetric flask, accurately add 0.1ml of stock so...

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Abstract

The invention discloses a method for measuring residual amount of tetrabutylammonium bromide in an organic drug. The method is characterized in that the liquid chromatography is adopted, a reversed phase column is selected, and a mobile phase is formed by acetonitrile and a tetramethylammonium hydroxide and phosphoric acid solution for gradient elution. Compared with the prior art, the method provided by the invention achieves better separation of the tetrabutylammonium bromide from the organic drug, high test reproducibility, sensitivity and specificity, as well as simplicity and convenience in operation, and is conductive to the control of quality and usage safety for the organic drug.

Description

technical field [0001] The invention belongs to the field of pharmaceutical analysis methods, and in particular relates to a method for determining the content of tetrabutylammonium bromide in organic medicines by using high performance liquid chromatography. Background technique [0002] Tetrabutylammonium bromide is an organic chemical phase transfer catalyst, which is used in the synthesis of pharmaceutical intermediates such as benzyltriethylammonium chloride, ethyl cinnamate, and pseudoionone, and is also used in anti-infective drugs. In the synthesis of organic drugs such as ampicillin and sultacillin, tetrabutylammonium bromide is also used as a catalyst in the synthesis of antidiabetic drugs such as dapagliflozin with a new mechanism of action. Since tetrabutylammonium bromide is irritating to human skin, eyes and respiratory system, it may be poisoned when the human body inhales, ingests or contacts a certain amount of tetrabutylammonium bromide. When tetrabutylamm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 陈皓刘泽荣张道林唐远富
Owner CHONGQING PHARMA RES INST
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