色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 309-313.DOI: 10.3724/SP.J.1123.2011.11027

• 技术与应用 • 上一篇    下一篇

高效液相色谱-线性离子阱三级质谱法检测花生中涕灭威及其代谢物涕灭威砜、涕灭威亚砜

杨欣1*, 李鹏2, 赵云峰1, 吴永宁1   

  1. 1. 中国疾病预防控制中心营养与食品安全所, 北京 100021; 2. 中国农业大学动物医学院, 北京 100193
  • 收稿日期:2011-11-14 修回日期:2012-01-05 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 杨欣,硕士,副研究员,主要从事食品安全检测技术及标准化相关工作.
  • 基金资助:

    卫生部公益性科研专项项目(No. 200902009).

Determination of aldicarb and its metabolites in peanuts by high performance liquid chromatography-linear ion trap triple stage mass spectrometry

YANG Xin1*, LI Peng2, ZHAO Yunfeng1, WU Yongning1   

  1. 1. National Institute of Nutrition and Food Safety, Chinese Centre for Disease Control and Prevention, Beijing 100021, China; 2. College of Veterinary Medicine, China Agricultural University, Beijing 100193, China
  • Received:2011-11-14 Revised:2012-01-05 Online:2012-03-28 Published:2012-05-02

PDF

393

被引次数

5

摘要：

建立了花生中涕灭威及其代谢物涕灭威砜、涕灭威亚砜的高效液相色谱-线性离子阱三级质谱分析方法。样品经环己烷饱和的乙腈提取,凝胶渗透色谱净化后,用高效液相色谱-线性离子阱三级质谱法对样品中的目标物进行定性确证和定量分析。在Capcell PAK CR色谱柱上以含5 mmol/L NH4Ac-HAc的乙腈为流动相进行梯度洗脱分离。采用电喷雾离子源正离子模式进行三级选择离子监测,以涕灭威-d3作为3个目标物的内标物。通过比较基质匹配曲线和纯溶剂标准曲线计算回收率评估基质效应。方法的线性范围为10～500 μg/L,检出限为4～5 μg/kg。涕灭威、涕灭威砜、涕灭威亚砜在3个加标水平(10、20、40 μg/kg)的回收率为81.5%～115%,相对标准偏差为6.35%～15.1%。应用该方法对花生样品进行了测定,结果令人满意。

关键词: 高效液相色谱-线性离子阱三级质谱法, 花生, 凝胶渗透色谱净化, 涕灭威, 涕灭威砜, 涕灭威亚砜

Abstract:

A high performance liquid chromatography-linear ion trap triple stage mass spectrometry (HPLC-IT/MS3) method was established to detect aldicarb, aldicarb sulfoxide, and aldicarb sulfone in peanuts. The samples were extracted by acetonitrile saturated with cyclohexane, followed by clean-up with gel permeation chromatography (GPC). The determination was performed using HPLC-IT/MS3 for the identification and quantification of the compounds. The separation was carried on a Capcell PAK CR column with gradient elution using 5 mmol/L acetic acid/ammonium acetate/acetonitrile as mobile phase. The ionization of molecules was performed by electrospray mode. Selective reaction monitoring (SRM) was the acquisition mode used for the monitoring of MS3 transitions for each compound using aldicarb-d3 as internal standard for three analytes. Matrix effects were evaluated by comparing the recovery of matrix-matched and solvent-based calibration curves. The calibration graphs were linear in the ranges of 10~500 μg/L and the detection limits ranged from 4 to 5 μg/kg. The average recoveries ranged between 81.5% and 115% at three different spiked levels (10, 20 and 40 μg/kg). Satisfactory results were obtained in the determination of real peanut samples by this method.

Key words: aldicarb, aldicarb sulfone, aldicarb sulfoxide, gel permeation chromatography (GPC) clean-up, peanuts, high performance liquid chromatography-linear ion trap triple stage mass spectrometry (HPLC-IT/MS3)