摘要
建立了固相萃取-高效液相色谱-电喷雾质谱(HPLC-MS)测定白酒中乐果、敌敌畏、甲基对硫磷、马拉硫磷、对硫磷农药残留的检测方法。白酒样品用C18固相萃取柱富集净化、二氯甲烷洗脱、氮吹浓缩;采用C18反相色谱柱,以含有0.1%乙酸的水/甲醇(35∶65,v/v)为流动相;电喷雾正离子模式,选择有机磷农药的准分子离子为定性离子进行MS测定。结果表明,5种有机磷农药的平均加标回收率为71.0%～87.8%,相对标准偏差为2.7%～8.5%;方法的最小检出限为0.05～0.16μg/L。该法有很高的选择性、灵敏度和准确度,满足白酒中痕量有机磷农药的高灵敏分析。
A high performance liquid chromatography-electrospray ionization tandem mass spectrometry method was developed for simultaneous determination of dimethoate, dichlorvos, parathion-methyl, malathion and parathion in liquor samples. Liquor sample was purified by solid phase extraction and eluted with methylene dichloride,the eluate was evaporated to dryness with nitrogen and was deproteinizated with methanol. Chromatogrphic separation was performed on a C18 column with water （containing 0.1% acetic acid）/methanol （65：35） elution. The protonated moleacular of pesticides was selected as quantitative ion scanning in positive electrospray ioization mode.The results showed that the average recovery of standard addition was 71.0 %～87.8 % with the relative standard deviation was fi＇om 2.7 %～8.5 %. The detection limit of the method was 0.05 μg/L～0.16 μg/L.The method has high selectivity, high sensitivity and high accuracy, which could realize high sensitive analysis of trace organophosphorus pesticides in liquor.
出处
《酿酒科技》
北大核心
2008年第6期103-105,共3页
Liquor-Making Science & Technology
关键词
白酒
有机磷农药
高效液相色谱-质谱联用
固相萃取
liquor
organophosphorous pesticide
high performance liquid chromatography-electrospray ionization tandem mass spectrometry（HPLC-MS）
solid phase extraction
