摘要
微波等离子体发射光谱(MP-AES)作为一种新型原子发射光谱法,具有动态线性范围宽、分析灵敏度高、多元素分析的特点,同时可利用氮气作为载气,极大地节约了运行成本。本研究采用微波消解法对饲料样品进行前处理,建立了测定饲料样品中K、Ca、Na、Mg、P、Cu、Fe、Mn、Zn、Co、Mo等11种元素的MP-AES法。在最优条件下,各元素的方法定量限(LOQ)在0.13 mg/kg(Mo)~3.37 mg/kg(P),线性范围可达3~6个数量级,线性回归系数(R~2)>0.996,对典型饲料样品多次测定的RSD<10%(n=6)。针对鱼粉、精料补充料、微量元素预混料的加标回收率在94.9%~118.4%,精密度RSD<10%,对饲料质控样品(配合料)中各元素的测定值均在标定值范围内,对豆粕、鱼粉、预混料、配合料等真实饲料样品中各元素的MP-AES测定值与电感耦合等离子体发射光谱法(ICP-AES)之间的相对偏差均<10%。
引文
[1]张志薇,石玉祥,毛雪飞,等.我国饲料元素检测方法标准体系建设现状探讨[J].农产品质量与安全,2016(3):20-26.
[2]朱伟星,雎敏,何亚丁,等.钾在水产动物中的生理作用和营养代谢功能[J].动物营养学报.2014,26(5):1174-1179.
[3]Lall S P.The Minerals[A].In:Halver J E,Hardy R W(Eds.),Fish Nutrition(3rd edition)[C].Amsterdam:Academic Press,2002,259-308.
[4]Shear erkd.Dietary potassium requirement of juvenile hinook salmon[J].Aquaculture,1988,73(1/2/3/4):119-129.
[5]Shiau S Y,Hsieh J F.Quantifying the dietary potassium requirement of juvenile hybrid tilapia(Oreochromis niloticus×O.aureus)[J].British Journal of Nutrition,2001,85(2):213-218.
[6]Priego-Capote F,Luque de Castro M D.Dynamic ultrasound-assisted leaching of essential macro and micronutrient metal elements from animal feeds prior to flame atomic absorption spectrometry[J].Analytical and bioanalytical chemistry,2004,378(5):1376-1381.
[7]翟毓秀,郝林华.氢化物发生原子荧光光谱法测定食品和饲料中的铅[J].分析化学,2000,28(2):176-179.
[8]艾明.氢化物发生-原子吸收光谱法测定食品中的汞[J].中国无机分析化学,2013(1):74-76.
[9]Phuong Truong,John Cauduro.微波等离子体原子发射光谱法(MP-AES)测定果汁中的常量元素[J].中国无机分析化学,2014(4):62-64.
[10]Licata P,Di Bella G,Potorti A G,et al.Determination of trace elements in goat and ovine milk from Calabria(Italy)by ICP-AES[J].Food Additives and Contaminants,Part B.Surveillance,2012,5(4):268-271.
[11]Andrea M Pless,Benjamin W Smith,Mikhail A Bolshov,et al.A capacitively coupled microwave plasma atomic emission spectrometer for the determination of trace metals in microsamples[J].Spectrochimica Acta Part B.,1996,51:55-54.
[12]Su L,Kumar R,Ogungbesan B,et al.Experimental investigation of gas heating and dissociation in a microwave plasma torch at atmospheric pressure[J].Energy Conversion&Management,2014,78(2):695-703.
[13]Liu S,Kumar R,Ogungbesan B,et al.Experimental investigation of gas heating and dissociation in a microwave plasma torch at atmospheric pressure[J].Energy Conversion and Management,2014,78:695-703.
[14]韩枫,孟卓然,刘轶群,等.微波等离子体发射光谱法同时测定食品中13种元素[J].卫生研究,2016(1):76-80.
[15]Li W,Simmons P,Shrader D,et al.Microwave plasma-atomic emission spectroscopy as a tool for the determination of copper,iron,manganese and zinc in animal feed and fertilizer[J].Talanta,2013,112C(15):43-48.
[16]李应东,余晶晶,刘耀敏,等.MP-AES法测定水产饲料中多种金属元素[J].光谱学与光谱分析,2015(1):234-237.
[17]安徽省质量技术监督局.DB 34/T 1999-2013饲料中铜、铁、锰、锌、钙、钾、镁、钠、铅、铬、镉、钴、镍测定ICP-AES法[S].北京:中国标准出版社,2013.