| 盐析辅助液液萃取交联聚维酮净化-靶向单一离子监测/高分辨质谱法测定蜂蜜中新烟碱类农药残留 |
| 点此下载全文 |
|
| 基金项目:国家食品安全风险评估中心高层次人才队伍建设523项目(“523” Project) |
|
| 中文摘要:基于盐析辅助液液萃取(LLE)交联聚维酮(PVPP)净化技术，建立了蜂蜜中7种新烟碱类农药的靶向单一离子监测(TSIM)/高分辨质谱检测方法。样品用乙腈基于盐析辅助LLE-PVPP提取净化，采用BEH C18色谱柱为分析柱，甲醇-水体系(两相均含0.1%甲酸和5 mmol/L甲酸铵)作为流动相，梯度洗脱，采用高分辨质谱TSIM模式检测目标化合物，内标法定量。结果表明，盐析辅助LLE-PVPP净化技术可实现提取净化一步式样品制备，TSIM扫描模式则显示了更宽的线性动态范围和更高的灵敏度与准确度。7种新烟碱类农药在0.01~100 μg/L或0.02~100 μg/L范围内具有良好的线性关系(r2> 0.999)；方法检出限为0.03~0.07 μg/kg，定量下限为0.1~0.2 μg/kg。在0.2、2、20 μg/kg 3种加标水平下，7种新烟碱类农药在蜂蜜中的平均回收率为84.8%~112.7%，日内精密度(RSDr)为0.9%~5.7%，日间精密度(RSDR)为3.7%~9.7%。该方法前处理简单快速、成本较低，灵敏度高、重现性好，可广泛应用于蜂蜜中新烟碱类农药残留的快速检测。 |
| 中文关键词:新烟碱类农药；交联聚维酮；靶向单一离子监测；高分辨质谱；蜂蜜 盐析辅助液液萃取 |
| |
| Determination of Neonicotinoid Residues in Honey by Target Single Ion Monitoring/High Resolution Mass Spectrometry Combined with Salting-out Assisted Liquid-Liquid Extraction and PVPP Cleanup |
|
|
| Abstract:Based on salting-out assisted liquid-liquid extraction(LLE) and polyvinylpolypyrrolidone(PVPP) cleanup,a method was developed for the determination of seven neonicotinoid pesticides in honey by target single ion monitoring(TSIM)/high-resolution mass spectrometry.The samples were extracted and cleaned up with acetonitrile by salting-out assisted LLE-PVPP method.The chromatographic separation was conducted on a BEH C18 column using methanol-water containing 0.1%formic acid and 5 mmol/L ammonium formate in two phases,as mobile phase by gradient elution.The analysis was performed by high resolution mass spectrometry in TSIM mode,and the quantitation was carried out by the internal standard method.The result showed that salting-out assisted LLE-PPVP cleanup method allowed one-step sample preparation,while TSIM mode showed a wide linear dynamic range with higher sensitivity and accuracy.There existed good linearities(r2>0.999) for seven neonicotinoid pesticides in the concentration ranges of 0.01-100 μg/L or 0.02-100 μg/L.The limits of detection(LODs) and quantitation(LOQs) were in the ranges of 0.03-0.07 μg/kg and 0.1-0.2 μg/kg,respectively.At three spiked levels of 0.2,2,20 μg/kg,the average recoveries for the analytes in honey were between 84.8%and 112.7%,with the intra-day precision(RSDr) and the inter-day precision(RSDR) of 0.9%-5.7%and 3.7%-9.7%,respectively.With the advantages of a rapid and simple pretreatment,low-cost,high sensitivity and good reproducibility,this method was suitable for the determination of neonicotinoid pesticides in honey. |
| Key Words:neonicotinoid pesticides polyvinylpolypyrrolidone(PVPP) target single ion monitoring (TSIM) high resolution mass spectrometry honey salting out assisted liquid liquid extraction |
| 引用本文：吕冰，辛少鲲，陈达炜，赵云峰.盐析辅助液液萃取交联聚维酮净化-靶向单一离子监测/高分辨质谱法测定蜂蜜中新烟碱类农药残留[J].分析测试学报,2018,37(6):639-645. |
| 摘要点击次数: 2065 |
| 全文下载次数: 1106 |
| 查看全文 下载PDF阅读器 |
|
|
