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Method for determining anisidine value of lipid emulsion

A technology of methoxyaniline value and fat emulsion, which is applied in the preparation of test samples and the measurement of color/spectral properties, etc., can solve the problems of inaccurate measurement results and inability to measure methoxyaniline.

Active Publication Date: 2012-12-05
JIANGSU JIUXU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. This method uses vacuum rotary evaporation in a water bath at 60°C to remove water. If the temperature is too high and the rotary evaporation time is too long, the peroxide may continue to be degraded into aldehydes, ketones and small molecule aldehydes, which may be removed by high temperature vacuum rotary evaporation, resulting in the determination of Inaccurate results
[0004] 2. When the main drug has ultraviolet absorption at 350nm wavelength, the value of methoxyaniline cannot be determined after the water is removed by rotary evaporation

Method used

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  • Method for determining anisidine value of lipid emulsion
  • Method for determining anisidine value of lipid emulsion
  • Method for determining anisidine value of lipid emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Precisely measure 10ml of propofol injection and place it in a separatory funnel.

[0048] Add 1ml of 2mol / L hydrochloric acid, add 1ml of ethanol, 10ml of dichloromethane or chloroform along the bottle wall, and shake vigorously.

[0049] Static samples cannot be separated, so dichloromethane and chloroform are not suitable as extraction agents.

Embodiment 2

[0051] Precisely measure 10ml of propofol injection and place it in a separatory funnel.

[0052] Add 1ml of 2mol / L hydrochloric acid, add 1ml of ethanol and 10ml of ethyl acetate along the bottle wall, and shake vigorously.

[0053] The layers were left to stand, and the upper oil phase was transferred to a 250ml flask. The lower aqueous phase was extracted twice with ethyl acetate, each time with 10 ml of ethyl acetate, and the oil phases were combined, namely ethyl acetate liquid.

[0054] Concentrate below 40°C with a rotary evaporator.

[0055] The residue was dissolved in isooctane and transferred to a 25ml measuring bottle and diluted to the mark with isooctane as the test solution.

[0056] Take the test solution, take isooctane as a blank, and measure the absorbance value at 350nm according to UV-Vis spectrophotometry, and the absorbance value is A0.

[0057]Accurately measure 10ml of the test solution, put it into a brown stoppered test tube, accurately add 2ml of...

Embodiment 3

[0065] Precisely measure 10ml of propofol injection and place it in a separatory funnel.

[0066] Add 1ml of 2mol / L hydrochloric acid, add 1ml of ethanol and 10ml of ethyl acetate along the bottle wall, and shake vigorously.

[0067] The layers were left to stand, and the upper oil phase was transferred to a 250ml flask. The lower aqueous phase was extracted twice with ethyl acetate, each time with 10 ml of ethyl acetate, and the oil phases were combined, namely ethyl acetate liquid.

[0068] Concentrate below 60°C with a rotary evaporator.

[0069] The residue was dissolved in isooctane and transferred to a 25ml measuring bottle and diluted to the mark with isooctane as the test solution.

[0070] Take the test solution, take isooctane as a blank, and measure the absorbance value at 350nm according to UV-Vis spectrophotometry, and the absorbance value is A0.

[0071] Accurately measure 10ml of the test solution, put it into a brown stoppered test tube, accurately add 2ml o...

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Abstract

The invention relates to a method for determining an anisidine value of lipid emulsion. The method comprises the following steps: extracting the lipid emulsion with ethyl acetate and drying the ethyl acetate phase by low-temperature vacuum rotation distillation to obtain a residue 1 as a sample; or adding hexyl hydride to dissolve the residue 1, carrying out extraction with acetonitrile, enabling the hexyl hydride phase for standby use, and drying the acetonitrile phase by low-temperature vacuum rotation distillation to obtain a residue 2; dissolving the residue 2 with alcohol, sequentially adding a sodium hydrogen sulfite solution and ethyl acetate, carrying out extraction with water, carrying out extraction with ethyl acetate after adding hydrochloric acid in the water phase, combining the ethyl acetate phase with the hexyl hydride phase, and carrying out low-temperature vacuum rotation distillation for drying to obtain a residue 3 as a sample. According to the method for determining the anisidine value of the lipid emulsion, the interference to the detection result resulting from high-temperature operation and ultraviolet absorption of a main drug is effectively avoided; and the method is especially applicable to determination of the anisidine value of the lipid emulsion with the main drug having ultraviolet absorption at the wavelength of 350nm.

Description

technical field [0001] The invention relates to a method for measuring the methoxyaniline value of a fat emulsion. Background technique [0002] The existing method for determining the methoxyaniline value of fat emulsion refers to the "Quality Standards for Fat Emulsion Injection (C14-C24)" (draft for comments) issued by the Chinese Pharmacopoeia Commission. This method has the following disadvantages and deficiencies. [0003] 1. This method uses 60°C water bath vacuum rotary evaporation to remove water. If the temperature is too high and the rotary evaporation time is too long, the peroxide may continue to degrade into aldehydes, ketones and small molecule aldehydes, which may be removed by high temperature vacuum rotary evaporation, resulting in the determination of The result is inaccurate. [0004] 2. When the main drug has ultraviolet absorption at 350nm wavelength, the value of methoxyaniline cannot be determined after the water is removed by rotary evaporation. ...

Claims

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Application Information

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IPC IPC(8): G01N1/40G01N21/33
Inventor 陈沛单李宏岳昌林
Owner JIANGSU JIUXU PHARMA
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