摘要
研究建立了加速溶剂萃取-液相色谱-原子荧光(ASE-LC-AFS)测定动物源性食品中阿散酸(ASA)、硝苯砷酸(NIT)与洛克沙砷(ROX)的残留量的方法。比较了超声离心提取和加速溶剂萃取技术,并优化了加速溶剂萃取技术的提取溶剂比例、提取温度、提取时间和提取次数。优化了液相色谱流动相和原子荧光的工作条件。在0~2.0 mg·L^(-1)范围内内阿散酸、硝苯砷酸和洛克沙砷的线性关系良好,线性相关系数大于0.999,阿散酸、硝苯砷酸、洛克沙砷检出限(S/N=3)分别为2.4,7.4,4.1μg·L^(-1)。2种样品在0.5,2,5mg·kg^(-1)3个加标水平下的平均回收率为阿散酸87.1%~93.2%,硝苯砷酸85.2%~93.9%,洛克沙砷84.2%~93.7%,相对标准偏差(RSD)分别为1.3%~4.6%,1.2%~4.2%,1.1%~4.5%。本方法操作简便,重现性好,适用于动物源性食品中ASA,NIT和ROX的分析。
A method for simultaneous determination of arsanilic ,nitarsone and roxarsone（ROX） residues in foods of animal ori-gin was developed by accelerated solvent extraction-liquid chromatography-atomic fluorescence spectrometry （ASE-LC-AFS） . The ultrasound centrifugation extraction and accelerated solvent extraction were compared ,and the accelerated solvent extraction conditions ,namely the proportion of the extraction solvent ,the extraction temperature ,extraction time and extraction times , were optimized .The operating conditions of LC-AFS and the mobile phase were optimized .Under the optimal conditions ,the calibration curves for ASA ,NIT and ROX were linear over the concentration range of 0~2.0 mg ＆#183; L -1 and their correlation co-efficients were 0.999 2~0.999 8. The detection limits of ASA ,NIT and ROX were 2.4 ,7.4 and 4.1 μg ＆#183; L -1 respectively.The average recoveries of ASA ,NIT and ROX from two samples spiked at three levels of 0.5 ,2 ,5 mg ＆#183; kg -1 were in the ranges of 87.1% ~93.2% ,85.2% ~93.9% ,and 84.2% ~93.7% w ith RSDs of 1.4% ~4.6% ,1.2% ~4.2% ,and 1.1% ~4.5% , respectively. This method possesses the merits of convenience and good repeatability ,and is a feasible method for analysis of ASA ,NIT and ROX in foods of animal origin .
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
2014年第4期1100-1103,共4页
Spectroscopy and Spectral Analysis
基金
天津出入境检验检疫局项目(TK032-2011)资助
关键词
加速溶剂萃取
液相色谱
原子荧光
动物源性食品
阿散酸
硝苯砷酸
洛克沙砷
残留
Accelerated solvent extraction
Liquid chromatography
Atomic fluorescence spectrometry
Food of animal origin
Arsanilic
Nitarsone
Roxarsone
Residues
