固相萃取原子荧光光谱法检测稻米和虾仁中的无机硒  

Determination of inorganic selenium in rice and shrimp by atomic fluorescence spectrometry with solid phase extraction separation

作　　者：郑宇 王宗义[1] 侯彤瑶 黄漫青[1] 郝宏伟 ZHENG Yu;WANG Zongyi;HOU Tongyao;HUANG Manqing;HAO Hongwei(Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Detection and Control of Spoilage Microorganisms and Pesticide Residues in Agricultural Products,Beijing University of Agriculture,Beijing 102206)

机构地区：[1]北京农学院食品科学与工程学院食品质量安全北京实验室农产品有害微生物及农残安全检测与控制北京市重点实验室,北京102206

出　　处：《分析试验室》2020年第6期695-699,共5页Chinese Journal of Analysis Laboratory

基　　金：北京市教委食品质量安全北京实验室建设专项(5075227125);北京农学院实验技术体系基金项目(1086716287)资助。

摘　　要：建立了氨水提取、三氯乙酸沉淀蛋白、阳离子交换净化分离,原子荧光光谱检测稻米和虾仁中无机硒的新方法。样品经氨水超声提取,三氯乙酸沉淀蛋白,Cleanert PCX小柱分离,HNO3-HClO4消解,HCl还原,原子荧光光谱法进行检测。结果显示,无机硒能被有效提取、分离和检测。方法在(0. 1~4. 0μg/L)浓度范围内,R2> 0. 99,仪器检出限(IDL)为0. 040μg/L,方法检出限(MDL)为1. 60μg/kg。稻米和虾仁样品的加标回收率分别为84. 1%~98. 7%和89. 8%~109. 3%,相对标准差分别为2. 3%~10%和2. 2%~3. 1%。对产地不同的稻米和虾仁样品的实际检测显示,稻米无机硒含量分别为3. 88~45. 90μg/kg,占总硒的百分比最高值为11. 27%,虾仁样品无机硒含量为小于MDL^24. 76μg/kg,占总硒的百分比最高值为3. 83%。A new method for the determination of inorganic selenium in rice and shrimp by atomic fluorescence spectrometry(AFS)with solid phase extraction separation wasdeveloped.The sample was extracted by sonicating with ammonia solution,and the protein in the extract was precipted with trichloroaceticacid.Subsequently,the extract was passed through the Cleanert PCX cartridge for separating inorganic selenium,followed by digesting with HNO3-HClO4and reducing with HCl for AFS testing.The results showed that inorganic selenium could be extracted and seprated from matrixes,and determined effectively.A satisfied linearity was obtained in the rang of 0.1-4.0μg/L withR2>0.99.The detection limit of the instrument(IDL)was 0.040μg/L and the detection limit of method(MDL)was 1.60μg/kg.The recoveries and relative standard deviations were 84.1%~98.7%and 2.3%~10%for rice samples,89.8%~109.3%and 2.2%~3.1%for shrimp samples,respectively.The method was applied to determine the rice and shrimp samples which from differentsources.The results indicated that the inorganic selenium contents were 3.88-45.90μg/kg in the rice samples and lower than MDL-24.76μg/kg in the shrimp samples,which the highest amounts account 11.27%and 3.38%to the total selenium contents,respectively.

关 键 词：原子荧光光谱法 无机硒 固相萃取 稻米 虾仁 

分 类 号：O657.31[理学—分析化学]