摘要
建立蜂花粉中硝基呋喃类代谢物液相色谱-串联质谱检测方法。样品经高氯酸酸化后,固相萃取净化、衍生、乙酸乙酯提取,串联质谱进样分析。在1.0、2.0、5.0μg/kg这3个添加水平下,硝基呋喃类代谢物的平均回收率范围为89.5%～100.9%,日内相对标准偏差小于10%,日间相对标准偏差小于15%。在0.5～20ng/mL范围内呈良好的线性(r>0.99),检测限为0.25μg/kg,定量限为1.0μg/kg。该检测方法简单,选择性好,抗干扰能力强,适用于蜂花粉中硝基呋喃类代谢物的分析确证。
A method was established for the determination of nitrofuran metabolite residues in bee pollen by liquid chromatography-tandem mass spectrometry（LC-MS-MS）.After acidified,samples were purified through HLB solid phase extraction columns,derivatized,and then extracted with ethyl acetate.The extracted residues were analyzed by mass spectrometry.The recoveries of nitrofuran metabolites ranged from 89.5% to 100.9% at spiked concentrations of 1,2 μg/kg.and 5 μg/kg.The method showed good precisions for intra-day（RSD 10%） and inter-day assays（RSD 15%）,and had an excellent linearity in the range from 0.5 to 20 ng/mL（r 0.99）.The detection limit and quantitation limit were 0.25 μg/kg.and 1.0 μg/kg,respectively.This validated method is suitable for the determination and confirmation of nitrofuran metabolite residues in bee pollen thanks to its excellent selectivity and strong anti-interference capability.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2013年第16期183-190,共8页
Food Science
基金
国家质检总局科研基金项目(2012IK167)
关键词
蜂花粉
硝基呋喃类代谢物
高效液相色谱-串联质谱
固相萃取
bee pollen
nitrofuran metabolites
liquid chromatography-tandem mass spectrometry（LC-MS-MS）
solid phase extraction（SPE）
