摘要
建立了用于水和鱼体中精草铵膦残留检测的柱前衍生-高效液相色谱法。水样经水合柠檬酸三钠处理后加9-芴甲基氯甲酸酯进行衍生化,鱼样以水为提取剂,提取液经9-芴甲基氯甲酸酯衍生化处理;衍生化反应液经二氯甲烷净化;进一步通过优化色谱分离条件,采用荧光检测器,建立柱前衍生-高效液相色谱检测法,外标法定量。水样中添加浓度为0.01~1.50 mg·L^(-1)时,平均回收率为100.8%~102.3%,相对标准偏差为0.8%~4.1%;鱼体中添加浓度为0.01~1.00 mg·kg^(-1)时,平均回收率为82.5%~101.6%,相对标准偏差为2.3%~6.2%。方法最小定量限为鱼体0.01 mg·kg^(-1)、水0.01 mg·L^(-1)。建立的柱前衍生-高效液相色谱法,可以对水样和鱼体中精草铵膦农药残留的高灵敏准确分析,达到农药残留分析测试要求。
The pre-column derivatization of high performance liquid chromatography(HPLC)method was established for detection of Glufosinate-P-ammonium residues in water and fish.The residues in water and fish samples were detected by HPLC after treated with trisodium citrate and derivatized with 9-fluorene methyl chloroformate.Quantitative analysis was carried out by the standard curve and external standard method.The limit of detection was 0.01 mg·kg^(-1) for fish and 0.01 mg·L^(-1) for water.When the fortified levels were ranged from 0.01 to 1.5 mg·L^(-1),average fortified recoveries in water samples were in the range of 100.8%to 102.3%,and relative standard deviations were 0.8%~4.1%.When the fortified levels were ranged from 0.01 to 1.0 mg·kg^(-1),average fortified recoveries in fish samples were in the range of 82.5%to 101.6%,and relative standard deviations were 2.3%~6.2%.The pre-column derivatization HPLC method can be used to quantitatively and qualitatively detect Glufosinate-P-ammonium residues in water and fish,which can meet the demand of pesticide residue analysis.
作者
徐漫
蔡小宇
田丰
吴文铸
石利利
XU Man;CAI Xiao-yu;TIAN Feng;WU Wen-zhu;SHI Li-li(Nanjing Institute of Environmental Science,Key Laboratory of Pesticide Environmental Assessment and Pollution Control,Ministry of Ecology and Environment of the People s Republic of China,Nanjing 210042,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2022年第5期1223-1228,共6页
Chemical Research and Application
基金
江苏省333工程科研资助计划(BRA2017497)资助
中央级公益性科研院所基本科研业务专项(GYZX180107)资助。
关键词
精草铵膦
高效液相色谱
水
斑马鱼
残留分析
glufosinate-P-ammonium
HPLC
water
Brachydanio rerio
residue analysis
