色谱

色谱

• 研究报告 • 上一篇    下一篇

气相色谱/质谱-选择离子检测法同时测定大米中的25种持久性有机污染物

侯圣军1,2,陈丹丹1,2,李翔1,李刚1,杨强1,闵顺耕2,仲维科1,储晓刚1,王大宁1   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2. College of Science, China Agricultural University, Beijing 100094, China
  • 收稿日期:2004-12-15 修回日期:1900-01-01 出版日期:2005-05-30 发布日期:1988-09-25
  • 通讯作者: 仲维科
  • 基金资助:

Simultaneous Determination of 25 Persistent Organic Pollutants in Rice by Gas Chromatography-Mass Spectrometry with Selected Ion Monitoring Mode

HOU Shengjun1,2, CHEN Dandan1,2, LI Xiang1, LI Gang1, YANG Qiang1, MIN Shungeng2, ZHONG Weike1, CHU Xiaogang1, WANG Daning1   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2. College of Science, China Agricultural University, Beijing 100094, China
  • Received:2004-12-15 Revised:1900-01-01 Online:2005-05-30 Published:1988-09-25

PDF

680

被引次数

31

摘要： 利用超声波提取、固相萃取净化对样品进行前处理,然后采用气相色谱/质谱-选择离子检测模式对大米中的25种持久性有机污染物进行了分析。色谱条件:DB-35MS毛细管色谱柱(30 m×0.25 mm i.d.×0.25 μm)；载气为氦气,流速1 mL/min;进样口温度300 ℃；不分流进样，进样量1 μL;柱温为程序升温模式。质谱条件:电子轰击电离源,70 eV;采集方式为选择离子方式,扫描质量范围50~450 u。实验采用保留时间以及定性、定量特征离子的丰度比定性，采用峰面积外标法定量，制作了25种持久性有机污染物的标准工作曲线。不同浓度水平的添加回收率试验表明,25种持久性有机污染物的添加回收率为81.99%～100.60%,相对标准偏差为2.37%～18.48%,除异狄氏剂、反式氯丹和顺式氯丹的检测限分别为20,30和20 ng/g外,其他有机污染物的检测限为0.1～5 ng/g。该方法的灵敏度、准确度和精密度均符合农药多残留测定技术的要求。

关键词: 超声波, 持久性有机污染物, 大米 , 气相色谱-质谱-选择离子模式

Abstract: A multi-residue analytical method for the simultaneous determination of persistent organic pollutants (POPs) in rice samples was developed. POPs were extracted from rice with ethyl acetate/n-hexane(80∶20,v/v) by sonication, and determined by gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode. A fused silica capillary column DB-35MS (30 m× 0.25 mm i.d. ×0.25 μm) was employed. Operating conditions were as follows: injector port temperature, 300 °C; column temperature, programming; carrier gas, helium; flow rate, 1.0 mL/min; sample size, 1 μL with splitless injection. The mass spectrometric detector (MSD) was operated in electron impact ionization mode with an ionizing energy of 70 eV. Analysis was performed with selected ion monitoring (SIM) using one target and one or two qualifier ion.POPs were confirmed by their retention times, their qualifier and target ions, and their qualifier/target abundance ratios. Recovery studies were performed at 0.05, 0.1, and 0.5 mg/L spiked levels of each POPs, and the recoveries obtained ranged from 81.99% to 100.60% with relative standard deviations between 2.37% and 18.48%. The detection limits of the method ranged from 0.1 to 5 ng/g for the different POPs except endrin, trans-chlordane and cis-chlordane. The results show that the method developed is sensitive and reliable.

Key words: persistent organic pollutants, rice , gas chromatography/mass spectrometry