气相色谱-质谱法测定硅凝胶中两种硅氧烷  

Determination of Two Siloxanes in Silicone Gel by GC-MS

作　　者：郝玉红[1] 吴建军[1] 

机构地区：[1]上海市计量测试技术研究院,上海201203

出　　处：《理化检验（化学分册）》2015年第6期818-820,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：采用索氏提取-气相色谱-质谱法测定硅凝胶中八甲基环四硅氧烷(D4)及十甲基环五硅氧烷(D5)。以二氯甲烷为溶剂采用索氏提取处理样品,提取液在HP-5毛细管色谱柱上分离,质谱中选择电喷雾离子源-选择离子检测模式。D4和D5的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)分别为0.011,0.013 mg·L-1。平均加标回收率分别为90.3%,85.1%,测定值的相对标准偏差(n=6)分别为1.5%,1.6%。A method of GC-MS combined with soxhlet extraction was used for the analysis of Octamethyl cyclotetrasiloxane（ D4） and Decamethyl cyclopenta siloxane（ D5） in silicone gel samples. The sample was extracted with dichloromethane by soxhlet extraction,and the extracted solution was separated on a HP-5 capillary column. EI-SIM was adopted in MS. The linear relationship were found between the peak area and the mass concentration of D4 and D5 was in a certain range, with detection limits of 0. 0 1 1 and 0. 0 1 3 mg · L- 1,respectively. The average recoveries measured by standard addition method were 9 0. 3 % and 8 5. 1 %,and RSD were 1. 5 % and 1. 6 %,respectively.

关 键 词：气相色谱-质谱法 索氏提取 硅凝胶 八甲基环四硅氧烷 十甲基环五硅氧烷 

分 类 号：O657.63[理学—分析化学]