华中农业大学学报
華中農業大學學報
화중농업대학학보
JOURNAL OF HUAZHONG AGRICULTURAL UNIVERSITY
2013年
4期
73-76
,共4页
杨愿愿%杨晓云%黄其亮%洪海%苗雪雪%徐汉虹
楊願願%楊曉雲%黃其亮%洪海%苗雪雪%徐漢虹
양원원%양효운%황기량%홍해%묘설설%서한홍
分散固相萃取%高效液相色谱%四螨嗪%柑橘%残留检测
分散固相萃取%高效液相色譜%四螨嗪%柑橘%殘留檢測
분산고상췌취%고효액상색보%사만진%감귤%잔류검측
dispersive solid phase extraction%high performance liquid chromatographic%clofentezine%or-anges%residue detection
建立了高效液相色谱法快速检测柑橘中四螨嗪残留量的方法。试样经乙腈提取,使用N-丙基乙二胺键合固相吸附材料(PSA)和C18吸附剂净化,在C18柱上以乙腈-水(V ∶ V=70∶30)为流动相进行分离,在268 nm波长下检测。四螨嗪在0.05~5.00 mg/L时线性关系良好(R2=0.9993);柑橘果肉和果皮中四螨嗪的最低检测限( LOD)均为0.05 mg/kg;在0.05~1.00 mg/kg添加水平时,果肉和果皮中四螨嗪的回收率分别为77.6%~91.6%、79.3%~105.6%,相对标准偏差(RSD)均低于8.1%。
建立瞭高效液相色譜法快速檢測柑橘中四螨嗪殘留量的方法。試樣經乙腈提取,使用N-丙基乙二胺鍵閤固相吸附材料(PSA)和C18吸附劑淨化,在C18柱上以乙腈-水(V ∶ V=70∶30)為流動相進行分離,在268 nm波長下檢測。四螨嗪在0.05~5.00 mg/L時線性關繫良好(R2=0.9993);柑橘果肉和果皮中四螨嗪的最低檢測限( LOD)均為0.05 mg/kg;在0.05~1.00 mg/kg添加水平時,果肉和果皮中四螨嗪的迴收率分彆為77.6%~91.6%、79.3%~105.6%,相對標準偏差(RSD)均低于8.1%。
건립료고효액상색보법쾌속검측감귤중사만진잔류량적방법。시양경을정제취,사용N-병기을이알건합고상흡부재료(PSA)화C18흡부제정화,재C18주상이을정-수(V ∶ V=70∶30)위류동상진행분리,재268 nm파장하검측。사만진재0.05~5.00 mg/L시선성관계량호(R2=0.9993);감귤과육화과피중사만진적최저검측한( LOD)균위0.05 mg/kg;재0.05~1.00 mg/kg첨가수평시,과육화과피중사만진적회수솔분별위77.6%~91.6%、79.3%~105.6%,상대표준편차(RSD)균저우8.1%。
A quick method was developed for determining clofentezine residues in oranges by HPLC with dispersive solid phase extraction. The residues of clofentezine in samples was extracted by acetronitrile,cleaned up by PSA and C18 adsorbent. HPLC was performed on a C18 column with UV detection at 268 nm using aceto-nitrile-water(70 ∶ 30,V/V) as mobile phase. The newly developed method showed a good linear relationship at the range of 0. 05-5. 00 mg/L with good precision and accuracy for clofentezine(R2=0. 999 3). The limit of quantification (LOD) of clofentezine in orange pulp and peel was all 0. 05 mg/kg. With RSD lower than 8. 1%for pulp and peel,the average recoveries were 77. 6%-91. 6% and 79. 3%-105. 6% for pulp and peel samples spiked with 0. 05-1. 00 mg/kg of clofentezine,respectively.