气相色谱-质谱联用法定量分析硅油中二甲基硅氧烷环体的研究

Study on Quantitative Analysis of Dimethylcyclosiloxane in Silicone Oil by Gas Chromatography-Mass Spectrometry

以正己烷为萃取溶剂,通过超声萃取硅油中二甲基硅氧烷环体,然后采用气相色谱-质谱联用仪定量分析其中的八甲基环四硅氧烷(D_(4))、十甲基环五硅氧烷(D_(5))和十二甲基环六硅氧烷(D_(6))的质量分数。探讨了标准曲线的线性和测试方法的正确度、精密度。结果表明,0~80μg/mL质量浓度范围内,D_(4)、D_(5)和D_(6)标准曲线的相关系数均大于0.997,定量分析方法正确度、精密度满足要求,D_(4)、D_(5)和D_(6)质量分数的检出限分别为8、7和10 mg/kg,测定下限分别为32、28和40 mg/kg。

The dimethylcyclosiloxane in silicone oil are extracted by ultrasonic extraction with n-hexane as the solvent,the quantitative analysis of octamethylcyclotetrasiloxane(D_(4)),decamethylcyclopentasiloxane(D_(5))and dodecamethylcyclohexasiloxane(D_(6))were investigated by gas chromatography-mass spectrometry.The linearity of the standard curves,the accuracy and precision of the analysis method was investigated.The results show that the correlation coefficients of D_(4),D_(5)and D_(6)standard curves are greater than 0.997 in the concentration range of 0-80μg/mL,and the accuracy and precision meet the requirements.The detection limits of D_(4),D_(5)and D_(6)are 8,7 and 10 mg/kg,respectively,whose lower limits are 32,28 and 40 mg/kg,respectively.