摘要
建立顶空气相色谱–质谱法测定土壤中5种乙酸酯类化合物的方法。对仪器工作条件进行优化,平衡温度为70℃,平衡时间为20min,氯化钠用量为2.0g。选用DB–624毛细管柱(30m×0.32mm,1.8μm),在柱流量1.5mL/min条件下采用电子轰击电离源,全扫描定性,选择离子外标法定量。当土壤取样量为2.0g时,5种乙酸酯类化合物的含量在1.0~20.0mg/kg范围内与其色谱峰面积呈良好的线性,线性相关系数大于0.999,方法检出限为0.22~0.32mg/kg。在3个不同加标水平下,土壤样品加标回收率为88.5%~107.0%,测定结果的相对标准偏差为3.0%~11.0%(n=6)。该方法检测快速,灵敏度高,满足土壤样品中5种乙酸酯类化合物快速测定要求。
A method was established to determine five kinds of acetate esters compounds in soils by headspace–gas chromatography–mass spectrometry. The analytical conditions were optimied. The equilibrium temperature and time were 70℃,20 min respectively,sodium chloride dosage was 2.0 g. Capillary column DB–624 (30 m×0.32 mm,1.8 μm) was used. Qualitative analysis was performed by full scan,and quantitation was performed by the external standard method under electron ionization conditions at flow rate of 1.5 mL/min. The content of five kinds of acetate esters compounds was linear with its chromatographic peak area in the range of 1.0–20.0 mg/kg,the correlation coefficients were more than 0.999. The detection limits were 0.22–0.32 mg/kg. At three different concentration levels,the average recoveries of spiked soil samples were in the range of 88.5%–107.0%. The relative standard deviations of detection results was 3.0%–11.0%(n=6). The method is rapid in detection,has high sensitivety,it can meet the requirements of rapid detection of acetate esters compounds in soil samples.
作者
郭佳惠
汪凌佳
曾珍
唐占谱
陈峰
GUO Jiahui;WANG Lingjia;ZENG Zhen;TANG Zhanpu;CHEN Feng(Hangzhou Environmental Monitoring Center Station,Hangzhou 310007,China)
出处
《化学分析计量》
CAS
2019年第4期26-29,共4页
Chemical Analysis And Meterage
基金
杭州市农业和社会发展科研项目(20191203B66)
杭州市农业和社会发展科研项目(20191203B65)
关键词
乙酸酯类化合物
气相色谱-质谱法
顶空
土壤
acetate ester compound
gas chromatography-mass spectrometry
headspace
soil
