摘要
采用气相色谱法(GC)和顶空-气相色谱/质谱法(HS-GC/MS)测定环境水样中的二甲胺和二乙胺。优化的实验条件如下:载气为高纯氮气,流速为1mL/min,柱温:35℃,保持15min,以5℃/min速度升至80℃(GC);顶空温度80℃,平衡时间30min,柱温50℃,离子源温度230℃(HS-GC/MS)。将10mL水样移入20mL顶空瓶中,将顶空瓶用铝盖密封。放入自动顶空进样系统中加热进行分析。在上述条件下,二甲胺(1.80～35.9mg/L)和二乙胺(1.42～28.4mg/L)的线性良好。GC和HS-GC/MS测定二甲胺的检出限分别为8.6和10.1mg/L,测定二乙胺的检出限分别为0.09和0.12mg/L;水样平均加标回收率分别为52.6%～56.2%和86.8%～109.6%;相对标准偏差分别为2.0%,5.8%,5.5%,2.0%。结果表明,在分析挥发性的胺类物质时HS-GC/MS比GC具有较强优势。它可省略蒸馏浓缩预处理步骤,直接进样,是一种测定环境水中二甲胺和二乙胺的有效分析方法。
The dimethylamine and diethylamine in ambient water were determined by gas chromatography（GC） and headspace-gas chromatography/mass spectrometry（HS-GC/MS）. The optimized experimental conditions were as follows： high purity nitrogen with a flow rate of 1 mL/min was used; oven temperature was programmed at 35 ℃ for 15 min, then rised to 80 ℃ at the rate of 5 ℃/min （GC）; Headspace temperature of 80 ℃, equilibrium time of 30 min, oven temperature of 50 ℃ and interface temperature of 230 ℃ were chosen（HS-GC/MS）. Ten milliliter water samples were transferred into glass ＂head space＂ vials（20 mL volume）, and then the vials were sealed with a cover. After that, they were heated and analyzed in the auto-headspace sampler. The linearities of dimethylamine and diethylamine were 1.80-35.9 mg/L and 1.42-35.9 mg/L, respectively. The correlation coefficients were 0.9994, 0.9938（GC for dimethylamine and diethylamine） and 0.9993, 0.9968（HS-GC/MS for dimethylamine and diethylamine）, respectively. The lowest determination limits were 8.55, 10.14 mg/L （GC） and 0.09, 0.12 mg/L （HS-GC/MS）, respectively; the recoveries of water samples were 52.6%-56.2%（GC） and 86.8%-109.55%（HS-GC/MS）; the relative standard deviations were 2.0%, 5.8%（GC） and 5.5%, 2.0%（HS-GC/MS）. The results showed that HS-GC/MS was superior to GC for the analysis of volatile amine components. The distillation pretreatment was omitted and the sample can be injected directly.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第5期731-734,共4页
Chinese Journal of Analytical Chemistry
基金
国家高技术研究发展计划(863)(No.SQ2008AA02Z44776722)资助项目
关键词
顶空-气相色谱/质谱
气相色谱
二甲胺
二乙胺
Headspace-gas chromatography-mass spectrometry
Gas chromatography
Dimethylamine
Diethylamine
