分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2009年
12期
1401-1404
,共4页
汤凯洁%顾小红%陶冠军%秦芳%汤坚%夏咏梅
湯凱潔%顧小紅%陶冠軍%秦芳%湯堅%夏詠梅
탕개길%고소홍%도관군%진방%탕견%하영매
磺酰脲除草剂%液相色谱-质谱联用%分子印迹固相萃取%大米
磺酰脲除草劑%液相色譜-質譜聯用%分子印跡固相萃取%大米
광선뇨제초제%액상색보-질보련용%분자인적고상췌취%대미
sulfonylurea herbicide%high performance liquid chromatography-mass spectrometry%molecular imprinting solid phase extraction%rice sample
采用苄嘧磺隆分子印迹固相萃取柱(MISPE)对加标大米中的苄嘧磺隆、甲磺隆、苯磺隆和烟嘧磺隆4种磺酰脲类除草剂进行净化和富集预处理,并采用LC-MS方法进行定量分析.质谱条件为:正离子检测模式(M+H),检测质量范围为m/z 200 ~800 ,毛细管电压3.93 kV,锥孔电压20 V,脱溶剂温度250 ℃,辅助气流速4 L/min.4种磺酰脲类除草剂在0.01 ~0.70 mg·L~(-1)范围内线性良好.回收率为68% ~100%,表明样品液中的烟嘧磺隆、甲磺隆、苯磺隆和苄嘧磺隆能直接被分子印迹固相萃取柱中的印迹位点保留,而杂质几乎不被保留.分子印迹固相萃取柱对磺酰脲类除草剂表现出良好的识别性能.
採用芐嘧磺隆分子印跡固相萃取柱(MISPE)對加標大米中的芐嘧磺隆、甲磺隆、苯磺隆和煙嘧磺隆4種磺酰脲類除草劑進行淨化和富集預處理,併採用LC-MS方法進行定量分析.質譜條件為:正離子檢測模式(M+H),檢測質量範圍為m/z 200 ~800 ,毛細管電壓3.93 kV,錐孔電壓20 V,脫溶劑溫度250 ℃,輔助氣流速4 L/min.4種磺酰脲類除草劑在0.01 ~0.70 mg·L~(-1)範圍內線性良好.迴收率為68% ~100%,錶明樣品液中的煙嘧磺隆、甲磺隆、苯磺隆和芐嘧磺隆能直接被分子印跡固相萃取柱中的印跡位點保留,而雜質幾乎不被保留.分子印跡固相萃取柱對磺酰脲類除草劑錶現齣良好的識彆性能.
채용변밀광륭분자인적고상췌취주(MISPE)대가표대미중적변밀광륭、갑광륭、분광륭화연밀광륭4충광선뇨류제초제진행정화화부집예처리,병채용LC-MS방법진행정량분석.질보조건위:정리자검측모식(M+H),검측질량범위위m/z 200 ~800 ,모세관전압3.93 kV,추공전압20 V,탈용제온도250 ℃,보조기류속4 L/min.4충광선뇨류제초제재0.01 ~0.70 mg·L~(-1)범위내선성량호.회수솔위68% ~100%,표명양품액중적연밀광륭、갑광륭、분광륭화변밀광륭능직접피분자인적고상췌취주중적인적위점보류,이잡질궤호불피보류.분자인적고상췌취주대광선뇨류제초제표현출량호적식별성능.
The pre-treatment methodology of purification and preconcentration of four sulfonylurea herbicides,including bensulfuron-methyl(BSM),metsulfuron-methyl(MSM),nicosulfuron(NS)and tribenuron-methyl(TBM) in spiked rice samples were developed using BSM molecular imprinting polymers solid phase extraction(MISPE)cartridges prepared by using the molecular imprinted polymer(MIP)as the sorbent.The MIP was prepared using the BSM as template molecule,trimethylolpropane trimethacrylate(TRIM) ∶ divinyl benzene(DVB)(1 ∶ 1) as the cross-linker,dichloromethane as porogen.The MISPE extraction procedure has been optimized.The quantitative analysis of four herbicides was performed by liquid chromatography-mass spectrometry under positive ion mode.The calibration curves were linear for four sulfonylurea herbicides in the concentration range of 0.01-0.70 mg·L~(-1) and the recoveries from spiked rice samples were between 68% and 100%.The result indicated that except the interferents,the sulfonylurea herbicides of BSM,MSM,NS and TBM were strongly retained by the imprinting sites in BSM molecular imprinting polymers SPE cartridges.The MIP showed high selective recognition and affinity to four sulfonylurea herbicides.