摘要
[目的]建立全自动石墨消解-电感耦合等离子体发射光谱(ICP-OES)、电感耦合等离子体质谱(ICP-MS)分析方法对马奶中的常量及痕量矿物质元素进行测定。[方法]采用全自动石墨消解仪对样品进行前处理,采用电感耦合等离子体发射光谱法对马奶中钾、钠、钙、磷4种常量元素进行测定,利用重量法配制标准溶液,以铑元素作为内标,采用电感耦合等离子体质谱法对马奶中铝、砷、硼、钡、铍、镉、钴、铬、铜、铁、锂、镁、锰、镍、铅、锑、锡、锶、钛、铊、钒、锌、硒共23种元素进行测定。利用生物成分分析标准物质对结果进行质量控制。[结果]常量元素在0~20μg/mL、痕量元素在0~200 ng/mL具有良好的线性关系,标准曲线相关系数均可达到0.999以上,ICP-MS法各元素检出限在0.00110~1.578 ng/mL,ICP-OES法各元素检出限在0.0100~0.0688μg/mL;多次对生物成分分析标准物质中矿物质元素含量测定结果的相对标准偏差均小于11%(n=6),且测定结果与标准值相符。[结论]该方法线性相关性、检出限、准确度等方面能够满足准确、高效测定马奶中矿物质元素含量的要求。
[Objective]To establish a determinative method for macro-elements and trace-mineral elements in mare′s milk samples based on full-automatic graphite digestion and inductively coupled plasma-optical emission spectroscopy(ICP-OES)as well as inductively coupled plasma-mass spectrometry(ICP-MS).[Method]The pre-treatment of milk samples was carried out with full-automatic graphite digester;the contents of four macro-elements including kalium,natrium,calcium and phosphorus in the milk samples were determined by using ICP-OES;the standard solutions were prepared with gravimetric method,and the contents of a total of 23 trace-mineral elements including aluminum,arsenic,boron,barium,beryllium,cadmium,cobalt,chromium,copper,iron,lithium,magnesium,manganese,nickel,lead,antimony,tin,strontium,titanium,thallium,vanadium,zinc and selenium were quantitatively analyzed with ICP-MS using rhodium as internal standard;the standard substances for analysis of food bio-components were used to validate the method.[Result]There was a good linear relationship in the range of 0-20μg/mL for macro-elements and 0-200 ng/mL for trace-elements,and the correlation coefficients of the standard curves were all higher than 0.999;the detection limit for macro-elements by ICP-OES ranged from 0.0100 to 0.0688μg/mL,and that for trace-elements by ICP-MS ranged from 0.00110 to 1.578 ng/mL;the relative standard deviations(RSDs)of the mineral elements of the standard substances for analysis of food bio-components were less than 11%(n=6);the determination results were all with the allowable deviation range of the value.[Conclusion]The good linear correlation,detection limit,accuracy and other aspects of the established method can meet the requirements for accurate,efficient and simultaneous determination of mineral elements contents in mare′s milk.
作者
吴云芳
王宏慧
杨喆
于林
郭元晟
WU Yun-fang;WANG Hong-hui;YANG Zhe;YU Lin;GUO Yuan-sheng(Xilin Gol Vocational College,Xilinhot 026000,China;Xilin Gol Institute of Bioengineering,Xilinhot 026000,China;Xilin Gol Food Inspection,Testing and Risk Assessment Center,Xilinhot 026000,China)
出处
《畜牧与饲料科学》
2020年第1期42-47,65,共7页
Animal Husbandry and Feed Science
基金
锡林郭勒职业学院院级科研课题（YB-2019-10）
