摘要
建立了水一沉积物系统中四氟醚唑的液相色谱-质谱联用（LC-MS／MS）测定方法。沉积物样品依次经y（丙酮）：V（水）=9：1混合提取和二氯甲烷萃取后，中性氧化铝与弗罗里硅土层析柱净化，用LC-MS／MS测定；水样经二氯甲烷萃取后直接用LC-MS／MS测定。结果表明：在0．5～5μg/L或0．5～5μg／kg添加水平下，四氟醚唑在水中的平均回收率为89％～98％，相对标准偏差（RSD）为1．8％～13％，在沉积物中的平均回收率为97％～103％，RSD为6．3％～11％。该方法中四氟醚唑的最小检出量为2．OPg，四氟醚唑在水中最低检测浓度（LOQ）为0．5μg/L，在沉积物中的LOQ为0．5μg/kg。该方法选择性好、灵敏度高、重现性好、基质干扰小，适用于水一沉积物系统中四氟醚唑残留的检测。
A liquid chromatography-tandem mass spectroscopy （LC-MS/MS） method was developed for determining tetraconeazole residue in water and sediment system. The sediment samples were extracted with V （ acetone ） ： V （water） = 9 ： 1, and partitioned by dichloromethane liquid-liquid extraction, then cleaned up on neutral alumina and Florisil layer column. The water samples were prepared by dichloromethane liquid-liquid extraction and determined by LC-MS/MS. The results showed that when spiked from 0. 5 to 5.0 μg/L, the average recoveries of tetraconazole in water were89% to 98%, with relative standard deviations （RSDs） between 1.8% to 13% ; when spiked from 0. 5 to 5 μg/kg, the average recoveries in sediment were 97% to 103%, with RSDs between 6. 3% to 11% ; The limit of detection （LOD） was 2.0 pg, the limit of quantification （LOQ） in water and sediment were 0. 5 μg/L and 0.5 μg/kg, respectively. The selectivity, reproducibility, accuracy and matrix effects were validated. The method was proved to be appropriate for determination of tetraconeazole residue in water and sediment system.
出处
《农药学学报》
CAS
CSCD
北大核心
2014年第2期179-185,共7页
Chinese Journal of Pesticide Science
基金
化学品生态毒理测试与风险评估技术合作研究(2011DFB41640)
关键词
液相色谱-质谱联用
四氟醚唑
水-沉积物系统
残留量
liquid chromatography-tandem mass spectrum
tetraconazole
water-sediment system
residues
