气相色谱-质谱法测定乙二醇二缩水甘油醚中环氧氯丙烷的残留量
GC-MS Determination of Residual Amounts of Epichlorohydrin in Glycol Diglycidyl Ether
摘 要
提出了气相色谱-质谱法测定乙二醇二缩水甘油醚中环氧氯丙烷残留量的方法。样品5.000 0 g置于10 mL容量瓶中，用乙醇稀释并定容。所得溶液经超声处理后，采用HP-5MS毛细管柱、载气程序升流和柱程序升温进行气相色谱分离。质谱分析中采用电子轰击离子源和选择离子监测模式。环氧氯丙烷的质量浓度在12.06~602.97 mg·L-1范围内与其峰面积呈线性关系，测定下限（10S/N）为4.21 mg·L-1，测定值的相对标准偏差（n=8）为0.51%。按标准加入法进行回收试验，回收率在94.2%~97.1%之间。
选择离子监测模式
乙二醇二缩水甘油醚
环氧氯丙烷
残留量
gas chromatography-mass spectrometry
selected ion monitor mode
glycol diglycidyl ether
epichlorohydrin
residual amount
Abstract
Gas chromatography-mass spectrometry (GC-MS) was proposed for determination of residual amounts of epichlorohydrin in glycol diglycidyl ether. The sample (5.000 0 g) was placed into 10 mL of volumetric flask, diluted and made its volume up with ethanol. After ultrasonic treatment, the solution obtained was separated through HP-5MS capillary column by GC at carrier gas flow programmed and column temperature programmed. Electron impact ion source (EI) and selected ion monitor (SIM) mode were adopted in MS analysis. Linear relationship between values of peak area and mass concentration of epichlorohydrin was obtained in range of 12.06-602.97 mg·L-1, with lower limits of determination (10S/N) of 4.21 mg·L-1 and value of RSDs (n=8) of 0.51%. Test for recovery was made by standard addition method, giving results in the range of 94.2%-97.1%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201801018
所属栏目 工作简报
基金项目
收稿日期 2017/1/24
修改稿日期
网络出版日期
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备注姚建磊(1986-),男,山东潍坊人,助理工程师,主要从事药物成分的分析研究
引用该论文: YAO Jianlei,DU Yiping,HU Huilian. GC-MS Determination of Residual Amounts of Epichlorohydrin in Glycol Diglycidyl Ether[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(1): 86～89
姚建磊,杜一平,胡慧廉. 气相色谱-质谱法测定乙二醇二缩水甘油醚中环氧氯丙烷的残留量[J]. 理化检验－化学分册, 2018, 54(1): 86～89
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