光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
4期
1100-1103
,共4页
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
加速溶劑萃取%液相色譜%原子熒光%動物源性食品%阿散痠%硝苯砷痠%洛剋沙砷%殘留
가속용제췌취%액상색보%원자형광%동물원성식품%아산산%초분신산%락극사신%잔류
Accelerated solvent extraction%Liquid chromatography%Atomic fluorescence spectrometry%Food of animal origin%Arsanilic%Nitarsone%Roxarsone%Residues
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0～2.0mg·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0.5，2，5 mg · kg -13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。
研究建立瞭加速溶劑萃取-液相色譜-原子熒光（ASE-LC-AFS）測定動物源性食品中阿散痠（ASA）、硝苯砷痠（NIT ）與洛剋沙砷（ROX）的殘留量的方法。比較瞭超聲離心提取和加速溶劑萃取技術，併優化瞭加速溶劑萃取技術的提取溶劑比例、提取溫度、提取時間和提取次數。優化瞭液相色譜流動相和原子熒光的工作條件。在0～2.0mg·L -1範圍內內阿散痠、硝苯砷痠和洛剋沙砷的線性關繫良好，線性相關繫數大于0.999，阿散痠、硝苯砷痠、洛剋沙砷檢齣限（S/N＝3）分彆為2.4，7.4，4.1μg · L -1。2種樣品在0.5，2，5 mg · kg -13箇加標水平下的平均迴收率為阿散痠87.1％～93.2％，硝苯砷痠85.2％～93.9％，洛剋沙砷84.2％～93.7％，相對標準偏差（RSD ）分彆為1.3％～4.6％，1.2％～4.2％，1.1％～4.5％。本方法操作簡便，重現性好，適用于動物源性食品中ASA ，NIT和ROX的分析。
연구건립료가속용제췌취-액상색보-원자형광（ASE-LC-AFS）측정동물원성식품중아산산（ASA）、초분신산（NIT ）여락극사신（ROX）적잔류량적방법。비교료초성리심제취화가속용제췌취기술，병우화료가속용제췌취기술적제취용제비례、제취온도、제취시간화제취차수。우화료액상색보류동상화원자형광적공작조건。재0～2.0mg·L -1범위내내아산산、초분신산화락극사신적선성관계량호，선성상관계수대우0.999，아산산、초분신산、락극사신검출한（S/N＝3）분별위2.4，7.4，4.1μg · L -1。2충양품재0.5，2，5 mg · kg -13개가표수평하적평균회수솔위아산산87.1％～93.2％，초분신산85.2％～93.9％，락극사신84.2％～93.7％，상대표준편차（RSD ）분별위1.3％～4.6％，1.2％～4.2％，1.1％～4.5％。본방법조작간편，중현성호，괄용우동물원성식품중ASA ，NIT화ROX적분석。
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 · 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 · L -1 respectively.The average recoveries of ASA ,NIT and ROX from two samples spiked at three levels of 0.5 ,2 ,5 mg · 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 .
