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Comparison of graphite furnace and hydride generation atomic absorption spectrometry for the determination of selenium status in chicken meat

机译:石墨炉和氢化物发生原子吸收光谱法测定鸡肉中硒含量的比较

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Four different procedures for the determination of selenium in chicken meat by atomic absorption spectrometry were investigated. They consisted on conventional ambient pressure acid digestion carried out before and after sample drying, associated or not with fat extraction. For all procedures muscle and skin were analyzed separately. Drying was carried out in a conventional oven at 65 ℃ for 24 h. For fat extraction different solvents and solvent mixtures were investigated considering both extraction yield and sample adequacy for further AAS measurement. Acid digestions were carried out with mixtures of HNO_3 and HC1O_4. After digestion, selenium was measured either by Hydride Generation (HGAAS) or by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). For the reduction of Se(VI) prior to the HGAAS determination, 8% (w/v) NaBr, 6 mol/1 HC1 (both with and without sulfamic acid), as well as UV radiation were investigated. Tests with spiked samples have shown that either UV radiation (pH 8) or NaBr/sulfamic acid presented good recoveries. In this way the HGAAS determination of selenium in tissue was carried out without interference whereas for the fatty fraction the results were satisfactory only if GFAAS was used. The results showed that drying the sample and extracting the fat prior to digestion is advantageous once the amount of acid necessary can be significantly reduced. The precision, expressed as relative standard deviation, was about 6.5% and 0.8% for GFAAS and HGAAS measurements, respectively. The limits of detection for HGAAS and GFAAS, based on three times the standard deviation of the blanks were 1 μg/1 and 0.6 μg/1, respectively. The results have shown that in chicken meat 59% of the selenium is found in the muscle tissue while the skin responds for 41%.
机译:研究了原子吸收光谱法测定鸡肉中硒的四种不同方法。它们包括在样品干燥之前和之后进行的常规环境压力酸消解,无论是否与脂肪提取有关。对于所有程序,分别分析肌肉和皮肤。在常规烤箱中于65℃干燥24小时。对于脂肪提取,研究了不同的溶剂和溶剂混合物,同时考虑了提取产率和进一步进行AAS测量的样品充分性。用HNO_3和HClO_4的混合物进行酸消化。消化后,通过氢化物发生(HGAAS)或石墨炉原子吸收光谱法(GFAAS)测量硒。为了在HGAAS测定之前还原Se(VI),研究了8%(w / v)的NaBr,6 mol / 1 HCl(含或不含氨基磺酸)和紫外线辐射。加标样品的测试表明,紫外线辐射(pH 8)或NaBr /氨基磺酸均可提供良好的回收率。通过这种方法,可以在无干扰的情况下进行HGAAS测定组织中的硒,而对于脂肪级分,只有使用GFAAS才能获得令人满意的结果。结果表明,一旦可以显着减少所需酸的量,在消化之前干燥样品和提取脂肪是有利的。对于GFAAS和HGAAS测量,精度以相对标准偏差表示,分别约为6.5%和0.8%。基于空白标准偏差的三倍,HGAAS和GFAAS的检出限分别为1μg/ 1和0.6μg/ 1。结果表明,鸡肉中59%的硒存在于肌肉组织中,而皮肤中的硒占41%。

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