A sample pretreatment method and detection method suitable for the detection of cyclomethicone in cosmetics

By optimizing the sample pretreatment method for cosmetics, and utilizing a liquid-liquid extraction system with an equal volume mixture of cyclohexane and methylcyclohexane as solvents, along with gas chromatography-tandem mass spectrometry, the matrix effect problem in the detection of cyclodimethylsiloxane in cosmetics was solved, achieving high accuracy and high precision in detection.

CN122409924APending Publication Date: 2026-07-17GUANGZHOU DRUG CONTROL INST
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Patent Information

Application Number
CN202610596303.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-04-30
Publication Date
2026-07-17

AI Technical Summary

Technical Problem

Existing technologies for detecting cyclodimethylsiloxanes in cosmetics suffer from matrix effects, leading to decreased accuracy and precision of detection results and making it difficult to simultaneously and effectively remove interfering components from the cosmetic matrix and extract the target analyte.

Method used

A liquid-liquid extraction system was developed using an equal volume mixture of cyclohexane and methylcyclohexane as solvent. By combining gas chromatography-tandem mass spectrometry with the control of the water content and solvent ratio of the polar solvent, the separation and purification of cyclopolydimethylsiloxane and interfering substances were achieved, thus optimizing the sample pretreatment method.

Benefits of technology

It effectively removes interfering substances from oil-based and wax-based cosmetics, improving the accuracy and precision of detection results. It enables the simultaneous detection of three cyclic polydimethylsiloxanes with a recovery rate of 90-110%, a matrix effect of 90-110%, a correlation coefficient greater than 0.998, a detection limit of 30 ng/mL, and a quantitation limit of 100 ng/mL.

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Abstract

本发明公开了一种适用于化妆品中环聚二甲基硅氧烷检验的样品前处理方法及其检测方法,该样品前处理方法包括以下步骤:称取化妆品样品,加入极性溶剂超声提取,离心,分离上清液;依次向上清液中加入水和烷烃,振荡混匀后,离心,转移上层烷烃层;下层溶液再加入烷烃,振荡混匀后,离心,取上层烷烃层,针对下层溶液的该操作可以重复若干次;合并所得上层烷烃层;所述的烷烃为环己烷与甲基环己烷等体积混合溶剂。本发明的样品前处理方法通过少量极性有机溶剂提取环聚二甲基硅氧烷的同时,避免提取过多的非极性干扰物质;通过调控极性溶剂的含水率,将环聚二甲基硅氧烷提取至非极性溶剂,同时极性干扰物质保留在极性溶剂中,达到净化效果。
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