分析与检测
中国酿造
2016年第35卷第4期
总第290期
微波消解-ICP-MS测定石阡苔茶中17种矿物质元素
熊冬华李刚凤*周振华?罗静
·167.
（1.铜仁学院生物与农林工程学院贵州铜仁5543002.厦门市出入境检验检疫局检验检疫技术中心福建厦门361026）摘要建立微波消解-电感耦合等离子体质谱(ICP-MS)法测定石阡菩茶中Na、Mg、K、Ca、Cr、Mn、Fe、Co、Cu、Zn、As、Se、Mo、Cd、Sb. Hg、Pb等17种矿物质元素。结果表明17种元素在0~1000ng/mL范围内呈良好的线性关系(R≥0.9990)检出限为0.001~23.720ng/mL，加标回收率为91.63%~104.45%相对标准偏差(RSD)为1.26%~5.34%精密度试验结果RSD值为0.002%~8.450%，该方法快速简单、准确、灵敏度高能满足石阡苔茶中17种矿物质元素的检测需求。石阡菩茶样品中K元素含量最高其次是Ca元素必需微量元素
关键词电感耦合等离子体质谱法石阡苔茶微波消解矿物质元素
中图分类号.0657.31
文章编号0254-5071(2016)04-0167-04
doi:10.11882/j.issn.02545071.2016.04.037
Determination of seventeen mineral elements in Shiqian moss tea bymicrowave digestion-ICP-MS
XIONG Donghua', LI Gangfeng'*, ZHOU Zhenhua', LUO Jing
(1.College of Biology & Agro-forestry Engineening, Tongren University, Tongren 554300 China;
2.Inspection and Quarantine Technology Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 36 1026, China)
Abstract :The determination method of 17 mineral elements (such as Na, Mg, K, Ca, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Mo, Cd, Sb, Hg and Pb) in Shiqian moss tea was established by microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS). The results showed the 17 miner-al elements had a good linear relationship in the rage of 0-1 000 ng/ml (R ≥ 0.999 0). The limit of detection was 0.001-23.720 ng/ml. The adding stan-dard recover rate was 91.63%-104.45% and the relative standard deviation (RSD) was 1.26%-5.34%. The RSD of precision experiments results was 0.002%-8.450%. The method had fast speed, simple operation, good accuracy and high sensitivity, which can meet the determination requirement of 17 kinds of mineral elements in Shiqian moss tea. The K content was the highest in Shiqian moss tea, and the second was Ca. The essential trace ele ments content from high to low in order was Fe, Zn, Cu, Cr, Co, Se, Mo. And Hg, Pb, Cd as four kinds of heavy metal elements content conformed the national standard and the agriculture industry standards.
Key words ICP-MS; Shiqian moss tea; microwave digestion; mineral elements
石阡县隶属于贵州省东北部地处湘西丘陵向云贵高原过渡的梯级大斜坡地带境内属中亚热带湿润季风气候区日照充足，气候温和雨量丰沛土层深厚、微酸性、有机质含量丰富得天独厚的环境特别适合茶树生长。苔茶属山茶料山茶属灌木型牙叶毛多富含锌、硒、钾等对人体有益的矿物质和微量元素是现代热捧的保健饮品(24)。 2009年9月石阡苔茶获得国家地理标志产品保护。
自前测定矿物质元系的方法主要有火焰原子吸收光谱(flame atomic absorption spectrometry FAAS)法、石墨炉原子吸收光谱(graphite furnace atomic absorption spectrometry GFAAS)法、电感耦合等离子体发射光谱(inductivelycou-pled plasma-atomic emission spectrometry ICP-AES)法、电感耦合等离子体质谱(inductivelycoupledplasmamassspec-
收稿日期2016-01-28
trometryICP-MS)法等围原子吸收法一次只能测一个元素且易受机体干扰的影响ICP-AES法可同时测定多种元素，但若不进行富集检出限无法满足痕量检出限的测定要求ICP-MS法测定矿质元素具有线性宽、灵敏度高、干扰少等优点可同时测定多种元素而且可测定痕量或超痕量矿物质元素。游富英等研究表明灰化法和湿法消解的时间较长、操作环节较多、不能满足快速分析的要求微波消解法操作步骤简单、二次污染小、时间短等优点")。 ICP-MS法广泛用于许多技术领域，是痕量元素测定的关键分析技术之—[]。
目前对于石阡苔茶的研究大都停留在发展现状、资源调查和保护方面1214而对其矿物质元素分析的研究相对较少。因此本研究以石阡苔茶为研究对象采用微波消
基金项目贵州省科技厅农业攻关项目（黔科合NY[2015]3011-1号）贵州省教育厅重点学科建设项目（黔学位合字ZDXK[2013]09号）贵州
省教育厅125重大专项项目（黔教合重大专项字[2012]018号）
作者简介熊冬华(1993-)女本科生研究方向为食品科学与工程
*通讯作者李刚风(1988-）文进师硕士研究方向为民族特色食品开发与食品营养
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