LC-MS/MS检测蜂胶中硝基呋喃类代谢物的残留  

Determination of nitrofuran metabolite residues in propolis by LC-MS/MS

作　　者：杨雯筌[1,2] 许蔚[2] 殷耀[2] 张晓燕[2] 陈惠兰[2] 辛志宏[1] 沈崇钰[2] 张睿[2] 

机构地区：[1]南京农业大学食品科技学院,南京210095 [2]江苏出入境检验检疫局食品实验室,南京210001

出　　处：《分析试验室》2013年第3期47-50,共4页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科研基金项目(2012IK167)资助

摘　　要：建立了蜂胶中硝基呋喃类代谢物液相色谱-串联质谱检测方法。样品经固相萃取、衍生、乙酸乙酯提取后进行质谱分析。在1.0、2.0、5.0μg/kg 3个添加水平下,硝基呋喃类代谢物的平均回收率为92.6%～99.3%,日内相对标准偏差小于10%,日间相对标准偏差小于15%。在0.5～20 ng/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。方法适用于蜂胶中硝基呋喃类代谢物的分析确证。A method is established for the determination of nitrofuran metabolite residues in propolis by liquid chromatography-tandem mass spectrometry （LC-MS/MS）. Samples were analyzed by mass spectrometry after solid phase extraction, derivation and extraction by ethyl acetate. The recoveries of nitrofuran metabolite residues ranged from 92. 6% to 99.3% at levels of 1,2,5μg/kg and the relative standard deviation （RSD） was less than 10 % for intra-day and under 15% for inter-day. The method has an excellent linearity from 0. 5 ng/mL 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 determination and confirmation of nitrofuran metabolite residues in propolis due.

关 键 词：蜂胶 硝基呋喃类代谢物 高效液相色谱-串联质谱 固相萃取 

分 类 号：O657.63[理学—分析化学]