论文部分内容阅读
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 method for the determination of paraquat residues in bamboo shoots by ultra-high performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with methanol-0.1 mol / L hydrochloric acid (1: 1, V / V) and purified by Oasis WCX SPE column (60 mg / mm, 1.7μm) separation, positive ion multi-reaction monitoring mode monitoring, external standard quantitative. Results Paraquat had a good linearity in the range of 10 ~ 500 μg / L with a correlation coefficient of 0.998 2, a limit of detection of 2 μg / kg and a limit of quantification of 5 μg / kg. The spiked samples were tested at concentrations of 5, 50 and 200 μg / kg. The recoveries were 82.2% -104.8% with relative standard deviations of 8.3% -10.9%. Conclusion The method is simple, sensitive and accurate and suitable for the detection of paraquat in bamboo shoots.