茶叶科学
茶葉科學
다협과학
2010年
1期
52-56
,共5页
基质固相分散%反相高效液相色谱%苯脲类除草剂%茶叶
基質固相分散%反相高效液相色譜%苯脲類除草劑%茶葉
기질고상분산%반상고효액상색보%분뇨류제초제%다협
MSPD%RP-HPLC%phenylurea herbicides%tea
建立了基质固相分散萃取(matrix solid phase dispersion, MSPD)-反相高效液相色谱(reversed phase high performance liquid chromatography, RP-HPLC)检测利谷隆、灭草隆、敌草隆和绿麦隆4种苯脲类除草剂的新方法.茶叶样品与C18填料混合碾磨后与中性氧化铝一起装柱,二氯甲烷为淋洗剂,使样品的萃取与净化一步完成.讨论了MSPD法和色谱分析的各种影响因素,最佳实验条件下灭草隆在0.01~10.00 mg/L范围内线性关系良好,检测限为5 μg/L;绿麦隆、敌草隆和利谷隆在0.025~10.00 mg/L范围内线性关系良好,检测限为10 μg/L.4种除草剂在茶叶样品中的回收率在83.5%~100.4%之间,相对标准偏差小于7.1%.该方法简单、快速、干扰少、回收率高,符合茶叶中除草剂残留分析要求.
建立瞭基質固相分散萃取(matrix solid phase dispersion, MSPD)-反相高效液相色譜(reversed phase high performance liquid chromatography, RP-HPLC)檢測利穀隆、滅草隆、敵草隆和綠麥隆4種苯脲類除草劑的新方法.茶葉樣品與C18填料混閤碾磨後與中性氧化鋁一起裝柱,二氯甲烷為淋洗劑,使樣品的萃取與淨化一步完成.討論瞭MSPD法和色譜分析的各種影響因素,最佳實驗條件下滅草隆在0.01~10.00 mg/L範圍內線性關繫良好,檢測限為5 μg/L;綠麥隆、敵草隆和利穀隆在0.025~10.00 mg/L範圍內線性關繫良好,檢測限為10 μg/L.4種除草劑在茶葉樣品中的迴收率在83.5%~100.4%之間,相對標準偏差小于7.1%.該方法簡單、快速、榦擾少、迴收率高,符閤茶葉中除草劑殘留分析要求.
건립료기질고상분산췌취(matrix solid phase dispersion, MSPD)-반상고효액상색보(reversed phase high performance liquid chromatography, RP-HPLC)검측리곡륭、멸초륭、활초륭화록맥륭4충분뇨류제초제적신방법.다협양품여C18전료혼합년마후여중성양화려일기장주,이록갑완위림세제,사양품적췌취여정화일보완성.토론료MSPD법화색보분석적각충영향인소,최가실험조건하멸초륭재0.01~10.00 mg/L범위내선성관계량호,검측한위5 μg/L;록맥륭、활초륭화리곡륭재0.025~10.00 mg/L범위내선성관계량호,검측한위10 μg/L.4충제초제재다협양품중적회수솔재83.5%~100.4%지간,상대표준편차소우7.1%.해방법간단、쾌속、간우소、회수솔고,부합다협중제초제잔류분석요구.
A new method for the simultaneous determination of 4 herbicides (Monuron, Chlortoluron, Diuron and Linuron) was established with MSPD-RP-HPLC. The mixture of tea samples and C18 stuffing were pulverized, then mixed with alumina packed to a syringe column, the extraction and purification of the samples were carried out with one-step using dichloromethane as eluting reagent. The effecting factors of MSPD and conditions of the chromatography were discussed. Under optimum conditions, the linear ranges of Monuron was 0.01~10.0 mg/L with 5 μg/L of the detection limits, and the linear ranges of Chlortoluron, Diuron and Linuron were 0.025~10.0 mg/L with 10 μg/L of the detection limits. The average recoveries of 4 herbicides ranged from 83.5% to100.4% with less than 7.1% of the relative standard deviations in tea samples. The method suggested was simple, rapid, and less interference with high recovery rate, and meet the analytical requirements of herbicide residues in tea.