食品科学

• 分析检测 • 上一篇    下一篇

LC-MS-MS检测蜂花粉中硝基呋喃类代谢物

杨雯筌,辛志宏,殷 耀,张晓燕,许 蔚,吴 斌,丁 涛,张 睿   

  1. 1.南京农业大学食品科技学院,江苏 南京 210095;
    2.江苏出入境检验检疫局食品实验室,江苏 南京 210001
  • 出版日期:2013-08-25 发布日期:2013-09-03

Determination of Nitrofuran Metabolite Residues in Bee Pollen by LC-MS-MS

YANG Wen-quan,XIN Zhi-hong,YIN Yao,ZHANG Xiao-yan,XU Wei,WU Bin,DING Tao,ZHANG Rui   

  1. 1. College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China;
    2. Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Online:2013-08-25 Published:2013-09-03

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。

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

Abstract:

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.

Key words: bee pollen, nitrofuran metabolites, liquid chromatography-tandem mass spectrometry (LC-MS-MS), solid phase extraction (SPE)