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高效液相色谱-串联质谱法测定猪肝中硝基呋喃类代谢物残留
引用本文:刘正华,杨娟,李拥军,李谦,郑飞腾,李盛安,冯敏铃. 高效液相色谱-串联质谱法测定猪肝中硝基呋喃类代谢物残留[J]. 广东农业科学, 2012, 39(4): 87-89
作者姓名:刘正华  杨娟  李拥军  李谦  郑飞腾  李盛安  冯敏铃
作者单位:1. 中山市小榄镇农业服务中心,广东中山,528415
2. 佛山市三水区农产品质量安全检测中心,广东佛山,528100
3. 中山市农产品质量监督检验所,广东中山,528403
基金项目:中山市科技计划项目(20114A195)
摘    要:建立了呋喃唑酮代谢物AOZ、呋喃西林代谢物SEM、呋喃妥因代谢物AHD、呋喃它酮代谢物AMOZ的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品经乙酸乙酯提取后,用Oasis HLB固相萃取柱净化,以乙腈和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用电喷雾正离子(ESI+)电离,多反应监测(MRM)模式检测,外标法定量。4种硝基呋喃类代谢物在0.5~20.0 ng/mL范围内均具有良好的线性关系,相关系数不低于0.9906,平均加标回收率为91.0%~101.5%,相对标准偏差均小于8%。该方法具有准确、灵敏、高效、环保,适用于猪肝中多种硝基呋喃类代谢物的同时测定。

关 键 词:高效液相色谱-串联质谱  猪肝  硝基呋喃类代谢物  残留

Determination of nitrofuran metabolite residues in liver by liquid chromatography tandem mass spectrometry
LIU Zheng-hua , YANG Juan , LI Yong-jun , LI Qian , ZHENG Fei-teng , LI Sheng-an , FENG Min-ling. Determination of nitrofuran metabolite residues in liver by liquid chromatography tandem mass spectrometry[J]. Guangdong Agricultural Sciences, 2012, 39(4): 87-89
Authors:LIU Zheng-hua    YANG Juan    LI Yong-jun    LI Qian    ZHENG Fei-teng    LI Sheng-an    FENG Min-ling
Affiliation:1.Agricultural Service Center of Xiaolan Town,Zhongshan 528415,China; 2.The Quality and Safety Testing Center of Agricultural Products of Sanshui District,Foshan 528100,China; 3.Zhongshan Quality Supervision & Inspection Institute of Agricultural Products,Zhongshan 528403,China)
Abstract:A HPLC-MS/MS method was developed for determination of 4 nitrofuran metabolite residues in liver.The sample was extracted with ethyl acetate and purified by Oasis HLB solid-phase extraction column,then detected by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).Acetonitrile and formic acid-ammonium acetate buffer were used as mobile phase by gradient elution.The analysis of target compounds was carried out by HPLC-MS/MS under positive electrospray ionization(ESI+) and multiple reaction monitoring(MRM) mode.The calibration curves for 4 nitrofuran metabolite residues all had good linear relationships with correlation coefficients not less than 0.9906.The spiked recoveries were ranged from 91.0% to 101.5% with relative standard deviations less than 8%.It was an effective method which fit for the nitrofuran metabolite residues analysis and has high accuracy,precision and sensitivity.
Keywords:HPLC-MS/MS  liver  nitrofuran metabolite  residue
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