摘要
目的运用超高效液相色谱-串联质谱联用技术,建立竹笋中百草枯残留的检测方法。方法样品用甲醇-0.1 mol/L盐酸溶液(1∶1,V/V)提取后,经Oasis WCX固相萃取柱(60 mg/3 ml)净化,采用UPLC BEH HILIC色谱柱(100 mm×2.1 mm,1.7μm)分离,正离子多反应监测模式监测,外标法定量。结果百草枯在10~500μg/L范围内具有良好线性关系,相关系数为0.998 2,检出限为2μg/kg,定量限为5μg/kg。进行5、50和200μg/kg三个浓度的样品加标试验,回收率为82.2%~104.8%,相对标准偏差为8.3%~10.9%。结论该方法简便、灵敏、准确,适合于竹笋中百草枯的检测。
Objective To establish a detection method for paraquat residues in bamboo shoots by ultra performance liquid chromatography-tandem mass spectrometry. Methods Samples were extracted with methanol-0. 1 mol/L hydrochloric acid solution（ 1∶ 1,V/V）. After cleaned up with Oasis WCX solid phase extraction columns（ 60 mg/3 ml）,samples were separated in UPLC BEH HILIC column（ 100 mm × 2. 1 mm,1. 7 μm）. The analytes were detected with mass spectrometer in multiple reaction monitoring mode with external standard. Results It showed good linearity with the correlation coefficients of 0. 998 2 in the range of 10-500 μg/L. The limit of detection was 2 μg/kg and the limit of quantitation was 5 μg/kg. Under 5,50 and 200 μg/kg spiked levels,the recoveries ranged from 82. 2% to 104. 8% with the relative standard deviation（ RSD） of 8. 3%-10. 9%. Conclusion The results indicated that this method was simple,rapid,sensitive and suitable for the determination of paraquat residues in bamboo shoots.
出处
《中国食品卫生杂志》
2017年第3期312-315,共4页
Chinese Journal of Food Hygiene
基金
浙江省医药卫生一般研究计划项目(2016KYB339)
关键词
超高效液相色谱-串联质谱
百草枯
竹笋
食品污染物
农药
Ultra performance liquid chromatography-tandem mass spectrometry
paraquat
bamboo shoots
food contaminants
pesticide
