摘要
目的建立全血中除草剂百草枯的高效液相色谱-四级杆串联飞行时间质谱（LC-Q/TOF）的检验方法。方法用乙腈提取样品中的百草枯,以乙腈（0.1%甲酸）-50mmol·L-1醋酸铵水溶液（甲酸调p H 3.5）为流动相,梯度洗脱,经RX-SIL色谱柱（2.1×100mm,1.8μm）分离,以电喷雾离子源正离子模式采集全扫描及MS/MS数据进行分析。结果该方法灵敏度达5.0μg·L-1,在10.0-1000.0μg·L-1范围内线性关系良好;低、中、高3种浓度的加样回收率分别为90.5%、91.5%、87.4%,相对标准偏差（RSD）均小于10%。结论该法操作简单、灵敏度高,结果可靠,完全满足公安机关在办理百草枯中毒案件中的需要。
OBJECTIVE To develop a method for determination of paraquat in whole blood by high performance liquid chromatography Q-TOF tadem mass spectrometry. METHODS Paraquat in samples was extracted with acetonitrile for analysis using HPLC-Q / TOF. The paraquat was separated by the RX-SIL column（ 2. 1 × 100 mm,1. 8μm）and with acetonitrile（ add 0. 1% fomic acid）-50mmol·L- 1ammonium acetate solution（ adjusted to p H 3. 5 by formic acid） as the mobile phase. The data was collected under the electrospray ionization in the positive ion mode. Paraquat was determined by both full scan and target MS / MS mode. RESULTS The detection limit of this method was 5. 0μg·L- 1. It had a good linear relationship of paraquat in the range of 10. 0 ~ 1000. 0μg·L- 1. The mean recoveries of low,middle and high concentrations were 90. 5%,91. 5%,87. 4%,and all of the relative standard deviation（ RSD） were less than 10%. CONCLUSION The method is easy to operate,sensitive and reliable which could be applied to forensic identification.
出处
《海峡药学》
2015年第12期255-257,共3页
Strait Pharmaceutical Journal
基金
湖南省公安厅科研计划项目〔2011HN029〕
