等离子体发射光谱—质谱联用法对几类药食天然产物中锗硒的分析

【作者】 李红；

【导师】 回瑞华； 侯冬岩；

【作者基本信息】 辽宁师范大学 ， 有机化学， 2006， 硕士

【摘要】 采用电感耦合等离子体质谱法(ICP-MS)对药食天然产物中锗硒进行同时测定，为开发富含锗硒的天然产物提供科学依据。 比较了烘箱密闭消解和微波密闭消解两种样品消解方法，它们都具有耗酸少(5～10mL)、对环境污染小、挥发性元素回收率高等优点。此外，微波消解运行一个程序仅需30min，温度变化范围±2℃，具有省时快速、控温精确的特点，与ICP-MS的快速测定相匹配。采用微波密闭消解作为样品前处理的方法，选用硝酸、硝酸／双氧水、硝酸／双氧水／氢氟酸三种消解体系。ICP-MS法具有检出限低、干扰少、快速、线性动态范围宽等特点。测定的28个元素检出限在0.0001390～4.185μg／g之间，以[m]／z~+定量谱线干扰少，测定一个元素仅需0.3～1.5s，测定一个样品需时70～180s，能同时准确测定μg／L级锗、铊、钍等微量元素和mg／L级钾、钙等常量元素。采用仪器本身的半导体控温冷却雾化室技术(2±0.1℃)和小孔径截取锥(1.0／0.4 mm)减少等离子体中水蒸汽的量，减少了干扰。在此基础上，采用调谐仪器各项指标、在线内标校正和干扰校正方程等手段消除干扰，进一步提高了测定结果的准确度。 本文用微波消解／ICP-MS法分析了百余种样品中的锗硒，从中筛选出茶叶类、花类、花粉类、果实类和芦荟系列共5个系列66个样品。锗的方法检出限为0.001696～0.001742μg／g、精密度为2.8％～6.9％、回收率为88.3％～119％；硒的方法检出限为0.01437～0.02829μg／g、精密度为8.3％～12％、回收率为80.8％～113％，获得满意结果。实验结果表明，本方法适合于样品中多种元素的同时测定。更多还原

【Abstract】 Simultaneous detection of germanium and selenium from several officinal and edible natural products by inductively coupled plasma-mass spectrometry （ICP-MS） .It can provide scientific reference for the exploitation of Ge and Se-enriched natural products.Oven and microwave obturation digestion were compared. They both have merits of low acid consume （5¹0mL）,low environment pollution and high recoveries of volatile elements. Microwave obturation process only need 30 minutes. The change range of temperature is ±2 ℃.It can quickly digest, control temperature accurately and match to quick detection by ICP-MS Microwave obturation digestion and the three system of HNO₃, HNO₃/H₂O₂ , HNO₃/H₂O₂/HF were used..This method have merits of low detection limits, little disturbance, wide linearity range. The range of detection of 28 elements was 0.0001390-4.185 ug/g. The spectrum line disturbance was lower by [m]/z⁺ qualify. The detection of one element only need 0.3-1.5s.The detection of one sample only need 70¹80s.It can detect Micro-elements （μg/L） and Macro-elements （mg/L） simultaneously and accuratelyApparatus semiconductor control temperature cooling pulverization chamber technique （2±0.1 ℃） and small aperture wimble （1.0/0.4 mm） was adopted to reduce disturbance. We tuned the parameters of apparatus, used injection-internal standard addition and disturbance correction equation to improve the accuracy of analytical results.The germanium and selenium were analysed by microwave obturation digestion/ICP-MS from teas, flowers, pollens, fruits and aloes. Germanium detection limits are in the range of 0.001696-0.001742 μg/g, with the relative standard deviation of 2.8%-6.9%,the recoveries are 88.3%¹19%. Selenium detection limits are in the range of 0.01437-0.02829 μg/g, with the relative standard deviation of 8.3%¹2%,the recoveries are 80.8%¹13%. The results show that the method is adapt to detect many kinds of element simultaneously.更多还原