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作 者:倪张林[1] 喻晴[1] 屈明华[1] 汤富彬[1] NI Zhang-Lin;YU Qing;QU Ming-Hua;TANG Fu-Bin(Research Institute of Subtropical Forestry,Chinese Academy of Forestry,Quality Testing Center for Non-wood Forest Products of National Foresty and Grassland Administration(Hangzhou),Hangzhou 311400,China)
机构地区:[1]中国林业科学研究院亚热带林业研究所,国家林业和草原局经济林产品质量检验检测中心(杭州),杭州311400
出 处:《分析化学》2020年第4期530-535,共6页Chinese Journal of Analytical Chemistry
基 金:中央级公益性科研院所基本科研业务费专项资金(No.CAFYBB2017QC002)资助。
摘 要:建立了旋涡提取-电感耦合等离子体光谱法(ICP-OES)准确测定橄榄油中9种金属元素的方法。采用5%(V/V)HNO 3作为提取液,通过5 min旋涡提取即可完全提取橄榄油中的待测金属元素,提取过程中加入适量二氯甲烷,将提取液置于上层,可使料液比加大至1∶1(m/V)。方法的定量限在0.01~0.05 mg/kg之间,可完全满足橄榄油中9种金属元素的测定要求。方法的加标回收率在90.2%~103.6%之间,相对标准偏差(RSD,n=6)小于5.0%,方法简单快捷、灵敏度高、稳定性好。本方法与GB 5009.268-2016的微波消解法测定结果无显著性差异(p>0.05),结果准确可靠。A vortex-assisted liquid-liquid extraction protocol followed by inductively coupled plasma optical emission spectrometer(ICP-OES)was developed for determination of nine elements(Cr,Mn,Fe,Ni,Cu,As,Zn,Cd,and Pb)in olive oil samples.The experiment was performed under optimum conditions including 5%HNO 3(V/V)and vortex-assisted extraction for 5 min.Dichloromethane was used to make the extraction solvent to the upper layer,which increased the ratio of oil-extraction solvent to 1∶1(m/V).Quantification limits were 0.01-0.05 mg/kg,which was satisfied with the request of determination of legislated metals in olive oil samples.The accuracy of the method was assessed by spiking experiments and comparison of the results from the extraction procedure with those obtained by national standard method of China.The recoveries were 90.2%-103.6%with RSD less than 5%.No statistical differences,based on t-test at a confidence level of 95%,were detected between two methods.The proposed method was simple,fast and accurate in determination of olive oil samples.
关 键 词:橄榄油 金属元素 旋涡提取 电感耦合等离子体光谱仪
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