LI Xiu-ping,ZHAO Rong-xiang,LI Li-hua,et al.Determination of Metallic Element in Soybean Coat by Fermentation-Microwave Digestion-Microwave after Semi-Ashing Plasma Torch Atomic Emission Spectrometry[J].Soybean Science,2011,30(02):314-317.[doi:10.11861/j.issn.1000-9841.2011.02.0314]
半灰化-微波消解-MPT-AES测定大豆皮中的金属元素
- Title:
- Determination of Metallic Element in Soybean Coat by Fermentation-Microwave Digestion-Microwave after Semi-Ashing Plasma Torch Atomic Emission Spectrometry
- 文章编号:
- 1000-9841(2011)02-0314-04
- 关键词:
- 微波消解等离子体炬原子发射光谱法; 大豆种皮; 金属元素
- Keywords:
- MPT-AES; Soybean coat; Metal element
- 分类号:
- TS214.2
- 文献标志码:
- A
- 摘要:
- 采用半灰化HNO3-H2O2消解大豆皮,微波等离子体矩原子发射光谱(MPT-AES)测定其中铁、镍、镁、钙、锌和铜的含量,同时详细考察了测定各金属元素的最佳试验条件以及介质酸和共存离子的影响。结果表明:测定铁、镍、镁、钙、锌、铜的检出限分别为22.94、7.55、0.36、0.92、16.27、2.1 ng·mL-1,RSD小于3.2%,说明方法精密度较高,线性范围分别为0~12、0~12、0~35、0~32、0~7、0~12 μg·mL-1,加标回收率分别为96.8%~101.3%、98.4%~103.7%、95.9%~99.6%、96.3%~103.5%、99.8%~103.5%、97.6%~105.3%。与常规试验方法相比,MPT-AES法与半灰化和微波消解处理样品相结合具有快速、准确性和重复性高的特点,适用于样品分析。
- Abstract:
- Soybean coat samples were digested by H2O2-HNO3 solution after semi-ashing in a closed microwave system and the determination of iron,nickel,magnesium,calcium zinc and copper in soybean coat has been performed by MPT-AES. Experimenta1 conditions were optimized and established. The effects of acid concentration and coexisting ions(K,Na,Fe,Ni,Al,Zn,M g,Ca)on determination of iron,nickel,magnesium,calcium zinc and copper were investigated. The results showed that the detection limits of iron,nickel,magnesium,calcium, zinc and copper were 22.94,7.55,0.36,0.92,16.27 and 2.1 ng·mL-1, respectively. The RSD was no more than 3.2%, it showed the adopted method had good precision. The linear ranges of iron,nickel,magnesium,calcium, zinc and copper were 0-12, 0-12, 0-35, 0-32, 0-7 and 0-12 μg·mL-1,respectively. The recoveries were 96.8%-101.3%,98.4%-103.7%, 95.9%-99.6%, 96.3%-103.5%, 99.8%-103.5% and 97.6%-105.3%, respectively. Compared with conventional test methods, MPT combined with half ash and microwave digestion samples was efficient with high accuracy and repeatability and applicable to sample analysis.
参考文献/References:
[1]孟庆翔, 鲁琳, 阂晓梅, 等. 大豆皮替代产奶牛日粮精料中玉米与小麦麸对产奶性能和干物质与纤维消化特性的影响[J]. 饲料广角, 2006(2):31-33. (Meng Q X, Lu L, He X M, et al. Soybean husk replace the corn in concentrated food and wheat gluten, which influence on milk production performance produce, dry matter and fiber digestive of milking cow[J]. Feed China, 2006(2):31-33.) [2]侯世忠, 祝平, 井长伟. 大豆皮的营养价值及在饲料中的应用[J]. 吉林畜牧兽医, 2007, 28 (9):18-21. (Hou S Z, Zhu P, Jing C W. Nutrition value and application in feed of soybean hulls[J]. Jilin Animal and Veterinary Sciences, 2007, 28 (9):18-21.) [3]Belyea R L, Stevens B J, Restrepo R J, et al.Variation in composition of by-product feeds[J]. Dairy Science, 1989, 72:2339-2345. [4]Ludden P A, Cecava M J, Hendrix K S. The value of soybean hulls as a replacement for corn in beef cattle diets formulated with or without added fat[J]. Animal Science, 1995, 73:2706-2718. [5]Anderson S J, Merril1 J K, McDonnell M L, et al. Digestibility and utilization of mechanically processed soybean hulls by 1ambs and steers[J]. Animal Science, 1988, 66:2965-2976. [6]Acgergor C A, Owen F G, McGill L D.Effect of increasing ration fiber with soybean mill run on digestibility and lactation performance[J]. Journal of Dairy Science, 1976, 59:682-689. [7]陈颖. 茶叶中8种元素的初步形态研究[J]. 分析测试通报, 1992, 11(2):61-63. (Chen Y. Analysis of primary speciation of eight elements in tea[J]. Bulletin Analysis and Testing, 1992, 11(2):61-63.) [8]杨京蓉. 微波消解ICP-AES法测定粮食中的常量及微量元素[J]. 光谱实验室, 1997, 14(3):22-25. (Yang J R. Determination of content of major and trace elements in grain crops by microwave digestion and ICP-AES method[J]. Chinese Journal of Spectroscopy Laboratory, 1997, 14(3):22-25.) [9]马晓国, 成晓玲. 微波消解-ICP-AES法测定茶叶中的微量元素[J]. 广州微量元素科学, 1999, 6(4):59-63. ( Ma X L, Chen X L. Determination of trace elements in tea samples by microwave digestion and ICP-AES[J]. Guangzhou Trace Elements Science, 1999, 6(4):59-63.)
备注/Memo
第一作者简介:李秀萍(1975-),女,讲师,从事分析化学相关研究。E-mail:lipingfushun@tom.com。