食品科学 ›› 2011, Vol. 32 ›› Issue (6 ): 179-182.doi: 10.7506/spkx1002-6630-201106041

• 分析检测 • 上一篇    下一篇

原子荧光光谱法测定富硒螺旋藻片中不同形态、价态的硒

王 梅1,张红香2,邹志辉1,杨冰仪1,陈 健1   

  1. 1.广东药学院公共卫生学院 2.山东绿叶制药有限公司
  • 收稿日期:2010-04-16 修回日期:2011-01-13 出版日期:2011-03-25 发布日期:2011-03-03
  • 通讯作者: 王梅 E-mail:wmei02@163.com

Determination of Chemical State and Valence for Selenium in Se-enriched S.pirulina Tablets by Atomic Fluorescence Spectrometry

WANG Mei1,ZHANG Hong-xiang2,ZOU Zhi-hui1,YANG Bing-yi1,CHEN Jian1   

  1. 1. School of Public Health, Guangdong Pharmaceutical University, Guangzhou 510310, China;
    2. Shandong Luye Pharma Group Co. Ltd., Yantai 264003, China
  • Received:2010-04-16 Revised:2011-01-13 Online:2011-03-25 Published:2011-03-03
  • Contact: WANG Mei E-mail:wmei02@163.com

摘要: 采用氢化物发生原子荧光法测定两种富硒螺旋藻片中不同形态和价态的硒含量。研究仪器原子化器高度、盐酸、硼氢化钾浓度对硒荧光信号值的影响,比较微波和湿法消化两种消化方法,以及反复冻融和超声波细胞粉碎法对蛋白溶出率的影响。结果显示,两种消化方法无显著性差异(P=0.6900),反复冻融法所得硒含量仅为超声波细胞粉碎法的25%~30%,超声波细胞粉碎法优于反复冻融法。在最佳实验条件下,测得两种富硒螺旋藻片硒含量有显著性差异(P<0.0001),但都存在无机态和有机态的硒,并以有机硒为主,占60%左右,且主要是以蛋白质结合的形式存在,无机态的四价硒和六价硒含量,样品1有显著性差异(P=0.0094),但样品2的四价硒和六价硒含量无统计学差异(P=0.2269)。方法的检出限为0.64ng/g,加标回收率为93.0%~98.8%,该方法操作简便,灵敏度高,检出限低,线性范围宽,可作为不同形态和价态的硒含量的测定方法。

关键词: 原子荧光, 富硒螺旋藻片, 硒, 形态, 价态

Abstract: Selenium contents with different chemical states and valences in two kinds of Se-enriched s.pirulina tablets were determined by atomic fluorescence spectrometry generated from hydride. The effects of atomizer height, HCl concentration and KBH4 concentration on Se fluorescence signal were investigated. The microwave digestion and wet digestion were also compared. In addition, the effects of ultrasonic cell-break method and repeated freezing-thaw method on the extraction rate of protein were explored. Results indicated that two digestion methods had no significant difference (P = 0.6900), and selenium content in samples treated by repeated freezing-thaw method was only 25%-30% of that treated by ultrasonic cell-break method, which suggested that ultrasonic cell-break method was better than repeated freezing-thaw method. Under the optimal conditions, selenium contents in Se-enriched s.pirulina tablets were significant difference (P < 0.0001). Although both inorganic Se and organic Se co-existed, the organic Se in the states of Se (IV) and Se (VI) was still prominent, which was up to 60%. The contents of Se in both states in sample 1 revealed a significant difference (P = 0.0094), but the contents of Se in both states in sample 2 had no significant difference (P = 0.2269). The detection limit of this method was 0.64 ng/g, and the recovery rate of spiked samples was in the range of 93.0%-98.8%. Therefore, this method is characteristics of simple operation, high sensitivity and low detection limit, and provides a theoretical reference for determining the content of Se in different states and valences from Se-enriched s.pirulina tablets.

Key words: atomic fluorescence spectrometry, Se-enriched s.pirulina tablets, Se, chemical state, valence

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