摘要
建立了高效液相色谱-电喷雾电离源串联质谱同时测定大豆中167种农药残留的高灵敏度、高检测通量的方法.样品加水混合后用乙腈匀浆提取,再加入无水硫酸镁、氯化钠、柠檬酸三钠二水合物、柠檬酸氢二钠倍半水合物盐析分层后,提取液经C18、PSA固相萃取柱净化,甲酸-甲醇（2∶98）洗脱,洗脱液浓缩定容后经Atlantis C18色谱柱（100 mm ±2.1 mm,3μm）分离,采用电喷雾电离串联质谱法在正负离子切换多反应检测模式（MRM）下进行测定,质曲线外标法定量.167种农药在大豆中0.01、0.02、0.
A high sensitivity and throughput method was developed for the simultaneous determinationof 167 pesticide residues in soybean by liquid chromatography - electrospray tandem mass spectrome-try（LC -MS/MS）. Sample was soaked with water and extracted with acetonitrile, followed by sal-ting out with anhydrous MgSO4, NaC1, Na3Citrate dihydrate and Na2HCitrat sesquihydrate mixture.The extract was added to Cls and PSA solid phase extraction columns, and eluted with 2% formicacid methanol solution. The eluent was concentrated to a constant volume and separated on an Atlan-tis Cls column（ 100 mm x 2. 1 mm,μ m） . The analyte was analyzed by HPLC -MS/MS with apositive and negative ions switching mechanism under multiple reaction monitoring mode. The resultswere quantified with matrix-matched standard solutions as the external standard. The average recover-ies of the pesticides at three spiked concentration levels of 0. 01, 0. 02, 0. 05 mg/kg were in therange of 67.3% - 123.5% , with RSDs of 4.7% - 13.9%. All the pesticides in matrix-matchedstandard solutions were linear in the range of 0 - 50. 0 μg/L with correlation coefficients more than0. 99. The limits of quantitation（S/N 〉 10） for all pesticides were 0. 01 mg/kg. The proposed meth-od was suitable for the screening of multi-pesticide residues in soybean for its high sample throughput,low LOQ, good accuracy and precision.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第5期499-505,共7页
Journal of Instrumental Analysis
基金
浙江省公益性技术应用研究计划项目(2012C37074
2012C37072)
关键词
高效液相色谱-串联质谱
大豆
农药多残留
高通量
liquid chromatography - electrospray tandem mass spectrometry （ LC - MS/MS）
soy-bean
multi-pesticide residues
high - throughput
