| 超高效液相色谱-串联质谱法测定动物性食品中10种拟除虫菊酯类农药残留 |
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| 基金项目:国家星火计划项目（2015GA721001） |
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| 中文摘要:建立了动物性食品中10种拟除虫菊酯类农药残留的超高效液相色谱-串联质谱(UPLC-MS／MS)检测方法。样品经冰乙酸-乙腈（1∶99，体积比）超声提取，低温冷冻除去大部分的油脂杂质后，再用Z-Sep+和C18净化。以01%甲酸水溶液（含5 mmol/L乙酸铵）和甲醇为流动相，经ACQUITY HSS T3色谱柱分离，采用电喷雾电离，多反应监测模式进行测定。结果表明，10种拟除虫菊酯在25~100 μg/L范围内线性关系良好，相关系数均大于0997，检出限为09 ~24 μg/kg，定量下限为30~80 μg/kg；在10、50、100 μg/kg 3个加标水平下，空白样品的加标回收率为703% ~120%，相对标准偏差（RSD）为12% ~112%。该方法前处理简单、灵敏度高、准确性好，且在10 min内可完成检测，满足动物性食品中10种拟除虫菊酯农药残留的快速检测要求。 |
| 中文关键词:拟除虫菊酯 动物性食品 氧化锆 超高效液相色谱-串联质谱(UPLC-MS／MS) 基质效应 |
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| Determination of 10 Pyrethroid Pesticide Residues in Animal Foods by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS／MS) method was developed for the determination of 10 pyrethroid pesticide residues in animal foods.The samples were extracted with glacial acetic acid-acetonitrile（1∶99，by volume），and most of the oil impurities were removed by cryogenic freezing，and then further purified with Z-Sep+ and C18.The separation of target compounds was performed with ACQUITY HSS T3 column using 01% formic acid aqueous solution containing 5 mmol/L ammonium acetate and methanol as mobile phases，and the detection of pesticides was carried out in electrospray ionization under multiple reaction monitoring mode.Results showed that the calibration curves for 10 pyrethroids were linear in the range of 25-100 μg/L with their correlation coefficients all larger than 0997.The limits of detection were in the range of 09-24 μg/kg and the limits of quantitation were 30-80 μg/kg.The spiked recoveries for 10 pyrethroid pesticides at three levels of 10，50 and 100 μg/kg were in the range of 703%- 120% with relative standard deviations（RSDs）of 12%-112%.With simple pretreatment，high sensitivity and good accuracy，the method completed detection on the targets within 10 min，and could meet the requirements for rapid detection of 10 pyrethroid pesticide residues in animal foods. |
| Key Words:pyrethroid animal food zirconium dioxide ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS／MS) matrix effect |
| 引用本文：张聪，周常义，江锋，曾磊，杨名平，苏国成.超高效液相色谱-串联质谱法测定动物性食品中10种拟除虫菊酯类农药残留[J].分析测试学报,2018,37(8):887-893. |
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