Determination of 4 Methyl Cyclosiloxanes in Electronic and Electrical Products by Gas Chromatography-Mass Spectrometry
摘 要
建立了气相色谱-质谱法(GC-MS)测定电子电气产品中4种甲基环硅氧烷含量的方法。称取粉碎后的样品1 g,加入10 mL四氢呋喃,于30℃超声提取30 min,提取液经0.22 μm有机系滤膜过滤,采用GC-MS测定其中4种甲基环硅氧烷的含量。结果显示,4种甲基环硅氧烷的质量浓度在0.1~10.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为1.86×10-3~7.02×10-2mg·kg-1;对阴性样品进行3个浓度水平的加标回收试验,4种甲基环硅氧烷的回收率为85.7%~106%,测定值的相对标准偏差(RSD,n=7)均小于5.0%。
Abstract
A method for determination of the 4 methyl cyclosiloxanes in electronic and electrical products by gas chromatography-mass spectrometry was established. The crushed sample powder of 1 g was extracted by ultrasonic at 30℃ for 30 min with 10 mL of tetrahydrofuran. The extracting solution was filtered by 0.22 μm organic filter membrane, the 4 methyl cyclosiloxanes of which were determined by GC-MS. As shown by the results, linear relationships between mass concentration of 4 methyl cyclosiloxanes and their peak area were kept in the range of 0.1-10.0 mg·L-1, with detection limits (3S/N) in the range of 1.86×10-3-7.02×10-2mg·kg-1. Recovery test was made on negative samples at 3 concentration levels by standard addition method, giving results in the range of 85.7%-106%, and RSDs (n=7) of the determined values were less than 5.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202112010
所属栏目 工作简报
基金项目 2019年国家标准计划项目资助(20191283-T607)
收稿日期 2020/6/17
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备注高欢,高级工程师,硕士,主要从事轻工消费品质量安全的检测与研究,gaohuanshiyong@126.com
引用该论文: GAO Huan,WEI Biwen,MIAO Junwen,HE Weihua. Determination of 4 Methyl Cyclosiloxanes in Electronic and Electrical Products by Gas Chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(12): 1115~1118
高欢,卫碧文,缪俊文,何卫华. 气相色谱-质谱法测定电子电气产品中4种甲基环硅氧烷的含量[J]. 理化检验-化学分册, 2021, 57(12): 1115~1118
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参考文献
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【7】麻景龙,陶强,昗丹琦,等.气相色谱-质谱联用法研究硅橡胶中甲基环硅氧烷向食品模拟液的迁移[J].食品安全质量检测学报, 2016,7(5):2014-2019.
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【9】蒋可志,邬继荣,倪勇,等.气相色谱-质谱法分析甲基苯基硅氧烷混合环体[J].分析化学, 2008,36(8):1129-1132.
【10】颜敏,刘园园,王栖,等.气相色谱-质谱联用法测定避孕套中聚二甲基硅氧烷聚合物的残留物[J].中国计划生育学杂志, 2019,27(6):695-697.
【2】HE B, RHODES-BROWER S, MILLER M R, et al. Octamethylcyclotetrasiloxane exhibits estrogenic activity in mice via ERα[J]. Toxicology and Applied Pharmacology, 2003,192(3):254-261.
【3】周鸿艳,叶朝霞,谭军,等.分散液液微萃取-气相色谱法测定水样中甲基环硅氧烷[J].分析试验室, 2011,30(2):66-69.
【4】贺炳慧,杨睿,田敏,等.食品用硅橡胶材料中低摩尔质量环硅氧烷的测定[J].塑料工业, 2017,45(1):97-100.
【5】高建国,贺炳慧,张辉珍,等.食品接触硅橡胶中十二甲基环六硅氧烷的检测及不确定度分析[J].食品科学, 2017,38(4):265-269.
【6】吴建军,薛民杰,朱力敏.顶空-气相色谱-质谱法测定整形用有机硅制品中两种硅氧烷[J].上海计量测试, 2017,44(3):17-19.
【7】麻景龙,陶强,昗丹琦,等.气相色谱-质谱联用法研究硅橡胶中甲基环硅氧烷向食品模拟液的迁移[J].食品安全质量检测学报, 2016,7(5):2014-2019.
【8】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.
【9】蒋可志,邬继荣,倪勇,等.气相色谱-质谱法分析甲基苯基硅氧烷混合环体[J].分析化学, 2008,36(8):1129-1132.
【10】颜敏,刘园园,王栖,等.气相色谱-质谱联用法测定避孕套中聚二甲基硅氧烷聚合物的残留物[J].中国计划生育学杂志, 2019,27(6):695-697.
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