Determination of synthetic muscone content by gas chromatography

Artificially synthesized muskactive ingredientcorrectβ-Methyl cyclopentadecanone, commonly known as muscone. due toβ-The synthesis conditions of methyl cyclopentadecanone are harsh, the operating units are cumbersome, and the products containIsomerismDue to the phenomenon, the detection procedures are relatively complex. Tengzhou Zhongke Spectral Analysis Instrument uses gas chromatography to analyzetraditionStarting with the external standard method and improving it, we attempted to use the internal standard method and achieved successidealThe detection effect.

[Keywords] external standard method;internal standard method;muskone;HPLC
　
1. Instruments and reagents

Gas chromatograph configuration and reagents:

　　


2 Methods and Results

detected condition:Column temperature 200℃Hydrogen flameionChemical detector（FID）The carrier gas isN 2, flow rate500ml/minPrecision weighing of internal standards andmuskKetone reference standard, calculate correction factor;Accurately weigh the internal standard and the tested sample again to determine the content of the tested sample. result The internal standard method is fast and agile, overcoming the long detection time and consumables 、programDisadvantages such as complexity. conclusion The internal standard method is used to determine the content of muscone, which is simple to operate, accurate in detection results, and has good repeatability.

Determination of Musk Ketone Content by Internal Standard Method
The internal standard method can be used to determine a certain substance in the test sample Impurities or main component content. Firstly, calculate the correction factor, and then measure the internal standard (n-nonadecane) with the tested samplecompare， Calculate the content of the tested substance after Zui.

　　2.1 Internal standard method operating procedure
（1）Accurately weigh the internal standard and reference substance, process them in the same volumetric flask, and prepare them8μg/μlMusk ketonesolution, sample injection5μl. UtilizeSQ-204Self made gas chromatographOV-17Stainless steel column, column temperature is200℃Hydrogen flame ionization detector（FID）The carrier gas isN 2, flow rate500ml/minCalculate the correction factor.
（2）Accurately weigh the internal standard and the tested sample, utilizingGC-2010 modelGas chromatography was used to detect the content of the tested sample, and parallel operations were performed using the external standard method. The results are shown in the table1.

Analysis spectrum:

Musk ketone hasevaporateSex,Gas phase is often used for content determinationchromatographyLow dosage, simple operation, and flexible method.

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