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食品研究与开发:2017,38(22):167-171
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SPE-HPLC-MS/MS检测动物源性食品中金刚烷胺残留
云雅光1,2,池永红2,王硕1,*
(1.天津科技大学,天津300457;2.包头轻工职业技术学院,内蒙古包头014035)
Determination of Amantadine in Animal-derived Food by Combining SPE with HPLC-MS/MS
YUN Ya-guang1,2,CHI Yong-hong2,WANG Shuo1,*
(1.Tianjin University of Science and Technology,Tianjin 300457,China;2.Baotou Light Industry Vocational Technical College,Baotou 014035,Inner Mongolia,China)
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投稿时间:2017-03-14    
中文摘要: 建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5 μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 mL/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1 μg/L~100.0 μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为 1.0 μg/kg,定量限(Limit of quantitation,LOQ)为 3.0 μg/kg,对 3 个添加浓度(30.0、60.0、90.0 μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。
Abstract:An accurate and sensitive method for the detection of amantadine(AM)residues in animal-derived food products was developed by combining solid-phase extraction with high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS/MS).The Oasis MCX solid-phase extraction column was used for complex matrix purification and Agilent SB-C18 column(2.1 mm ×150 mm,3.5 μm)was employed for separation in liquid chromatography using a mobile phase consisting of 0.1%formic acid and acetonitrile(80∶20,volume ratio)with the flow rate 0.2 mL/min.The electrospray ionization (ESI)source in the positive mode and the multiple-reaction monitoring(MRM)mode were used for the quantitative analysis with external standard method.The results showed that the calibration curves were in good linearity for the AM ranged from 0.1 μg/L to 100 μg/L with the correlation coefficients(R2)> 0.999.The limits of detection(LODs)and the limits of quantification (LOQs)of this method were 1.0 μg/kg and 3.0 μg/kg respectively.The average recovery rates were from 83.6%to 94.2%with the good relative standard deviations (RSDs,RSD<4.0%,n=3)in chosen chicken mus cle,chicken liver,egg,beef and mutton samplesat three standard addition levelsof 30.0,60.0,and 90.0 μg/kg.
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