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
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%.
索氏提取
硅凝胶
八甲基环四硅氧烷
十甲基环五硅氧烷
GC-MS
Soxhlet extraction
Silicone gel
Octamethyl cyclotetrasiloxane (D4)
Decamethyl cyclopenta siloxane (D5)
Abstract
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 0.011 and 0.013 mg·L-1,respectively. The average recoveries measured by standard addition method were 90.3% and 85.1% ,and RSD were 1.5% and 1.6%,respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201506021
所属栏目 工作简报
基金项目
收稿日期 2015/1/30
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备注郝玉红(1980-),女,山西阳泉人,工程师,硕士,主要从事材料分析检测工作.
引用该论文: HAO Yu-hong,WU Jian-jun. Determination of Two Siloxanes in Silicone Gel by GC-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(6): 818～820
郝玉红,吴建军. 气相色谱-质谱法测定硅凝胶中两种硅氧烷[J]. 理化检验－化学分册, 2015, 51(6): 818～820
被引情况:
【1】时磊,陈海英,蔡小虎,胡璟珂,吕爱娟,沈小明,孙艳艳, "超声提取-气相色谱法同时测定稻谷中18种有机氯农药和7种多氯联苯",理化检验－化学分册 52, 1090-1094(2016)
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参考文献
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【2】王元贵,李昕,张进江.硅凝胶人工角膜临床应用研究[J].武警医学院学报,2000,9(4):290-291．
【3】LIEBIERMAN M W,LYKISSA E D,BARRIOS R,et al. Cyclosiloxanes produce fatal liver and lung damage in mice[J]. Environ Health Perspect,1999,107(2):161-165．
【4】HE B,RHODES B S,MILLER M R. Octamethylcyclotetrasiloxane exhibits estrogenic activity in mice via ERalpha[J]. Toxicol Appl Pharmcol,2003,192(3):254-261．
【5】李莉,王春仁,付步芳.GC-MS法测定硅凝胶乳房假体中低分子量物质[J].药物分析杂志,2010,30(7):1361-1363．
【6】付步芳,冯晓明,奚廷斐.人工乳房硅凝胶填充物中小分子物质的检测[J].生物医学工程与临床,2010,14(5):387-389．
【7】赖莹,林睿,黄丽,等.气相色谱-质谱法测定有机建筑粘合剂中3种苯胺类化合物含量[J].理化检验-化学分册,2014,50(6):734-736．
【8】闻亚,徐心怡,聂晶,等.超声辅助-表面活性剂增强乳化微萃取-气相色谱-质谱法测定薄荷芳香水中的挥发性成分[J].理化检验-化学分册,2014,50(9):1065-1069．
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