大鼠尿液与粪便中氟噻草胺的UPLC-MS/MS法测定  

Determination of Flufenacet in Rats' Urine and Feces by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：余洋[1] 林立红[1] 李晓磊[1] 李娜[1] 郑鸿薇 罗雪琪 YU Yang;LIN Li-hong;LI Xiao-lei;LI Na;ZHENG Hong-wei;LUO Xue-qi(Safety Evaluation Center of Shenyang Research Institute of Chemical Industry Co.,Ltd.,Shenyang 110141,China;College of Applied Chemistry,Shenyang University of Chemical Technology,Shenyang 110020,China)

机构地区：[1]沈阳化工研究院有限公司安全评价中心,辽宁沈阳110141 [2]沈阳化工大学应用化学学院,辽宁沈阳110020

出　　处：《分析测试学报》2018年第11期1376-1380,共5页Journal of Instrumental Analysis

基　　金："十三五"国家重点研发计划项目(2016YFD0300708)

摘　　要：建立了一种测定大鼠尿液和粪便中氟噻草胺含量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。粪便与尿液样品采用乙腈提取;液相色谱分离采用Phenomenex反向C18色谱柱(50 mm×4. 6 mm,5μm),以0. 1%甲酸水和乙腈为流动相,流速0. 6 m L/min;质谱检测采用电喷雾离子源,正离子模式和多反应监测(MRM)方式进行扫描。结果表明:氟噻草胺在尿液(0. 10～10. 0 mg/L)和粪便(0. 25～50. 0 mg/L)中线性关系良好,相关系数r> 0. 99,尿液和粪便中氟噻草胺的定量下限分别为0. 10 mg/L和0. 25 mg/L;质控样品的日内与日间相对标准偏差不大于9. 9%。样品稳定性为93. 7%～108%,尿中平均提取回收率为97. 0%～98. 8%,基质效应为98. 8%～107%,均符合生物分析方法验证的要求。考察了大鼠单次灌胃给予氟噻草胺400 mg/kg后的排泄动力学,144 h内尿液与粪便的总累积排泄率为12. 62%,其中尿中的累积排泄率为1. 12%,粪便中的累积排泄率为10. 13%,表明氟噻草胺主要经粪便排泄。该法灵敏、专属、准确,可用于大鼠尿液、粪便中氟噻草胺浓度的测定。An ultrahigh performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was established for the determination of flufenacet in rats urine and feces.The urine and feces samples were extracted with acetonitrile.Chromatographic separation of the target compound was performed on a C 18 column(50 mm×4.6 mm,5μm)using ultrapure water containing 0.1%formic acid and acetonitrile as mobile phases at a flow rate of 0.6 mL·min-1.The detection of flufenacet was carried out by MS with electrospray ionization in positive ionization under multiple reaction monitoring mode.There were good linear relationships for flufenacet in rats’urine and feces over the concentration ranges of 0.10-10.0 mg/L and 0.25-50.0 mg/L,with their correlation coefficients(r)larger than 0.99.The limits of quantitation for flufenacet in urine and feces were 0.10 and 0.25 mg/L,respectively.The intra-RSDs and inter-RSDs for the QC sampes were not more than 9.9%.The stability for flufenacet in urine ranged from 93.7%to 108%,and the recoveries and matrix effects were in the ranges of 97.0%-98.8%and 98.8%-107%,respectively.All the results met the requirements for bioanalytical method validation.The excretion kinetics in rats was also investigated after oral administration of flufenacet at a dosage of 400 mg/kg by body weight.The total accumulated excretion rate for flufenacet in urine and feces was 12.62%in 144 h,in which the excretion percentages for urine and feces were 1.12%and 10.13%,respectively.Results indicated that flufenacet was mainly excreted through feces.This method has the advantages of high sensitivity,selectivity and accuracy,and could be applied in the analysis of flufenacet in rats urine and feces.

关 键 词：氟噻草胺 超高效液相色谱-串联质谱(UPLC-MS/MS) 大鼠 排泄 

分 类 号：O657.63[理学—分析化学] R969.1[理学—化学]