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Gas chromatography detection method for 4-methyl-cyclopentadecanone

A kind of methyl cyclopentadecanone, gas chromatography technology, applied in the field of gas chromatography detection method of 4-methyl cyclopentadecanone, can solve the problems such as the results are too different, can not be used for identification, no statistical significance and the like , to achieve the effect of small sample size, wide application range, simple equipment and operation

Active Publication Date: 2014-07-23
山东宏济堂制药集团股份有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] When detecting the content of 4-methylcyclopentadecanone, first use high-performance liquid chromatography to detect it, first derivate it into a hydrazone, and then carry out chromatographic analysis. Since the substance is a racemate, two chromatographic peaks with the same area The peaks can not be separated by changing various conditions, so this method cannot be used for identification; then directly carry out liquid chromatography detection, because 4-methylcyclopentadecanone belongs to terminal absorption, and the detection peak area of ​​ultraviolet detector is too small, It is not easy to identify the substance; later, it was detected by an evaporative light detector, and the results of many tests were too different and had no statistical significance, so it could not be used
When gas chromatography is used for detection, the separation effect is poor when using a packed column filled with methylpolysiloxane

Method used

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  • Gas chromatography detection method for 4-methyl-cyclopentadecanone
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  • Gas chromatography detection method for 4-methyl-cyclopentadecanone

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Embodiment Construction

[0023] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments, so that those skilled in the art can better understand the present invention, but the present invention is not limited thereto.

[0024] Choice of Experimental Conditions

[0025] Column Selection

[0026] Packed columns packed with methyl polysiloxane provide poor separation. A capillary column with a relatively polar polyethylene glycol 20M as the stationary liquid was selected as the chromatographic column, and the separation effect was good, and the resolution and tailing factor all met the requirements.

[0027] Selection of column temperature

[0028] Using column temperatures of 160°C, 180°C, and 200°C, the chromatograms were not ideal. After many attempts, the temperature program was finally set: the initial temperature was 140°C, maintained for 8 minutes, and increased at a rate of 5°C per minute. To 160°C, maintain for 5 minutes, the...

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Abstract

The invention belongs to the field of drug detection, and in particular relates to a gas chromatography detection method for 4-methylcyclopentadecanone. The method comprises the following steps: selection of chromatographic column, selection of column temperature, selection of solvent, chromatographic condition and system adaptability test and determination. Using the above method to detect 4-methylcyclopentadecanone, this method can detect substances below 1 mg; it can effectively separate isomers and isotopes with very similar properties; it can separate complex components The sample is separated into single components; it only takes more than ten minutes to complete the analysis, which is beneficial to guide and control production; it can analyze low content or high content during analysis, and is not limited by component content; general sample consumption It is a few milliliters; it has the advantages of high sensitivity, high selectivity, high efficiency, fast detection speed, wide application range, small sample amount required, relatively simple equipment and operation, and cheap instrument price.

Description

technical field [0001] The invention belongs to the field of drug detection, and in particular relates to a gas chromatography detection method for 4-methylcyclopentadecanone. Background technique [0002] The purpose of 4-methylcyclopentadecone is to mix it with macrocyclic musk complex hexadecanolide and pentadecanolide to form a mixture, which is used as a fragrance for body wash, In shampoos, laundry detergents, rinse conditioners, fabric softeners, etc., 4-methylcyclopentadione is used only as a substitute for polycyclic musk fragrances. [0003] When detecting the content of 4-methylcyclopentadecanone, first use high-performance liquid chromatography to detect it, first derivate it into a hydrazone, and then carry out chromatographic analysis. Since the substance is a racemate, two chromatographic peaks with the same area The peaks can not be separated by changing various conditions, so this method cannot be used for identification; then directly carry out liquid chro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 李樱文哲亮毕丽娟高钧李秀凤李海燕
Owner 山东宏济堂制药集团股份有限公司
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