摘要
建立了一种超声波辅助提取-气相色谱法测定茶叶中9种有机磷农药残留的检测方法。茶叶磨碎,丙酮-正己烷(体积比为1∶1)超声波提取,活性炭小柱净化,丙酮定容,气相色谱-火焰光度法(GC-FPD)进行检测,外标法定量。以9种有机磷农药(敌敌畏、甲胺磷、乙酰甲胺磷、乐果、毒死蜱、杀螟硫磷、喹硫磷、三唑磷、水胺硫磷)为分析物,考察并优化了色谱条件、提取溶剂、净化条件和基质效应,确定了最佳试验条件。在最优试验条件下,回归方程线性范围为0.020-0.120μg/m L,R2〉0.99,方法检出限为0.004 0-0.010 0 mg/kg;9种有机磷农药残留混标于0.025、0.040和0.080μg/m L 3个加标水平的回收率范围为80.88%-125.46%,相对标准偏差(RSD,n=6)为1.36%-10.75%。该方法准确、稳定,可满足茶叶中9种有机磷农药残留的检测要求。
A gas chromatographic method for the simultaneous determination of 9 organophosphorus pesticides residues in tea was established. Samples were ground,extracted with acetone-hexane(1∶1,V/V),then was cleaned-up with a activated carbon cartridge,dissolved in acetone,analyzed by GC-FPD and quantified by external standard method. With 9 organophosphorus pesticides including dichlorovos,methamidophos,acephate,dimethoate,chlorpyrifos,fenitrothion,quinalphos,triazophos and isocarbophos as analytes,the chromatographic conditions,extraction solvents,purification conditions and matrix effect were investigated and optimized to determine the optimal experimental conditions. Under the optimal experimental conditions,the method showed a good linearity(R2〉0.99) in the range of 0.020-0.120 μg / m L,the limit of detections were 0.004 0-0.01 mg / kg. At the spiked levels of 0.025,0.040 and 0.080 μg / m L,the recoveries of 9 analytes were in the range of 80.88%-125.46%,and the relative standard deviations(RSDs,n =6) were 1.36% -10.75%. The method was accurate,stable,and could meet requirements for the detection of 9 organophosphorus pesticides from tea.
出处
《湖北农业科学》
2016年第21期5623-5627,共5页
Hubei Agricultural Sciences
基金
云南省企业技术中心创新能力建设项目(2009D1037)
关键词
超声波辅助提取
气相色谱法
茶叶
有机磷农药残留
ultrasonic-assisted extraction
gas chromatography(GC)
tea
organophosphorus pesticide residues