用电感耦合等离子体质谱准确测量锌、硒同位素的研究
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摘要
锌元素和硒元素是人和动物生命活动中必需的微量营养元素。它们广泛分布于机体的各个部分,对生长发育和组织修复过程,增强机体免疫功能以及提高智商等有着重要的作用。研究锌元素和硒元素的准确测量有着至关重要的意义
本论文基于电感耦合等离子体质谱仪准确测量的优势,展开对锌元素和硒元素适用于复杂基体的同位素稀释质谱法的分离技术研究。主要成果有:(1)阴离子交换分离法分离锌元素。对分离效率、树脂柱高度等分离条件进行了讨论,回收率在96%以上。并应用于同位素稀释质谱法测量大豆粉、人血清、牛肝样品中的锌,结果准确可靠。阴离子交换分离法分离锌元素高效、准确、方便;(2)巯基棉分离法分离硒同位素。讨论了分离效率、巯基棉交换容量等分离条件对回收率的影响,回收率在92%以上。成功分离不同丰度的同位素标准溶液及复杂样品中添加硒同位素,未引起明显的同位素分馏。此方法应用于同位素稀释质谱法测量人血清、牛肝样品中的硒,结果准确,在标准值不确定度范围内。此方法也可用于复杂基体中硒同位素的分离。
本论文还涉及了锌同位素基准物质的制备研究,其中应用了锌的分离方法、浮力校正等。将两种高纯度丰度的浓缩同位素按比例定量混合,配制混合同位素基准溶液,用混合后得到的基准对质谱仪的系统偏差进行校正,用来修正样品的测量结果。这是国际上公认的获得准确同位素丰度值的一种方法。
Zinc and selenium are necessary nutrient trace element in the life activity of human and animals which are extensively distributing everywhere in the body. They exert significantly influence on growth and develop, body repairing, body immunity and intelligence quotient.
In present dissertation, experimental studies of separate techniques of zinc and selenium for matrix analysis with isotope dilution mass spectrometry (IDMS) were carried out. The main achievements obtained in this research are: (1) The separation of zinc with anion exchange resin. Separation conditions such as separation efficiency and column height were discussed. The recovery of zinc is above 96%. Combined with IDMS, this method was applied in determination zinc in soybean, human serum and bovine liver. The results are accurate and credible. (2) The separation of selenium isotope with sulphydryl cotton. Separate conditions such as efficiency and exchange capacity were discussed. The recovery of selenium is above 92%. Standard solution of different isotopic abundance were successfully separated. Combined with IDMS, this method was applied in determination selenium in human serum and bovine liver. The result is in the range of uncertainty of standard value. These separate techniques can also be applicated in separation of selenium isotope in compound matrix.
This dissertation also refered to the research of isotopic standard, And the separate technique of zinc was applied and buoyancy correction was considered. Two highly purified and high concentrated isotope were blended to prepare isotope standard samples by gravimetry using exact balance. According to measurement of isotope standards by mass spectrometry, the correction factor of system error of mass spectrometry can be confirmed. The method is accepted by IUPAC to obtain accurate isotopic abundance of samples.
本论文基于电感耦合等离子体质谱仪准确测量的优势,展开对锌元素和硒元素适用于复杂基体的同位素稀释质谱法的分离技术研究。主要成果有:(1)阴离子交换分离法分离锌元素。对分离效率、树脂柱高度等分离条件进行了讨论,回收率在96%以上。并应用于同位素稀释质谱法测量大豆粉、人血清、牛肝样品中的锌,结果准确可靠。阴离子交换分离法分离锌元素高效、准确、方便;(2)巯基棉分离法分离硒同位素。讨论了分离效率、巯基棉交换容量等分离条件对回收率的影响,回收率在92%以上。成功分离不同丰度的同位素标准溶液及复杂样品中添加硒同位素,未引起明显的同位素分馏。此方法应用于同位素稀释质谱法测量人血清、牛肝样品中的硒,结果准确,在标准值不确定度范围内。此方法也可用于复杂基体中硒同位素的分离。
本论文还涉及了锌同位素基准物质的制备研究,其中应用了锌的分离方法、浮力校正等。将两种高纯度丰度的浓缩同位素按比例定量混合,配制混合同位素基准溶液,用混合后得到的基准对质谱仪的系统偏差进行校正,用来修正样品的测量结果。这是国际上公认的获得准确同位素丰度值的一种方法。
Zinc and selenium are necessary nutrient trace element in the life activity of human and animals which are extensively distributing everywhere in the body. They exert significantly influence on growth and develop, body repairing, body immunity and intelligence quotient.
In present dissertation, experimental studies of separate techniques of zinc and selenium for matrix analysis with isotope dilution mass spectrometry (IDMS) were carried out. The main achievements obtained in this research are: (1) The separation of zinc with anion exchange resin. Separation conditions such as separation efficiency and column height were discussed. The recovery of zinc is above 96%. Combined with IDMS, this method was applied in determination zinc in soybean, human serum and bovine liver. The results are accurate and credible. (2) The separation of selenium isotope with sulphydryl cotton. Separate conditions such as efficiency and exchange capacity were discussed. The recovery of selenium is above 92%. Standard solution of different isotopic abundance were successfully separated. Combined with IDMS, this method was applied in determination selenium in human serum and bovine liver. The result is in the range of uncertainty of standard value. These separate techniques can also be applicated in separation of selenium isotope in compound matrix.
This dissertation also refered to the research of isotopic standard, And the separate technique of zinc was applied and buoyancy correction was considered. Two highly purified and high concentrated isotope were blended to prepare isotope standard samples by gravimetry using exact balance. According to measurement of isotope standards by mass spectrometry, the correction factor of system error of mass spectrometry can be confirmed. The method is accepted by IUPAC to obtain accurate isotopic abundance of samples.
引文
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[2]储著银,郭春华.地球科学中热电离质谱法的进展[J].现代仪器,2003,1:8-11
[3]周涛,李金英,赵墨田.质谱的无机痕量分析进展[J].分析测试学报,2004,23(2):110-u5
[4]Gary,A.L.The evolution of the ICP as an ion source for mass spectrometry[J].J.Anal.Atom.Spectrom.,1986,1:403-405
[5]章连香,符斌,李华昌.电感耦合等离子体质谱法应用的进展[J].矿冶,2004,13(1):101-106
[6]李金英,郭冬发,姚继军,等.电感耦合等离子体质谱(ICP-MS)新进展[J].质谱学报,2002,23(3):164-179
17]李金英,姚继军。电感耦合等离子体质谱分析的应用[M].北京:原子能科学出版社,1998:35-89
[8]陈成祥,庄峙厦,刘海波,等.同位素稀释电感耦合等离子体质谱测定环境和生物样品中的镉[J].分析试验室,2006,25(9):44-48
[9]李冰,杨红霞.电感耦合等离子体质谱(ICP-MS)技术在地学研究中的应用[J].地学前沿,2003,10(2):367-378
[10]徐先顺,张新荣,澎玉秀.电感耦合等离子体质谱在水质分析中的应用[J].中国卫生检验杂志,2006,16(6):763-766
[11]陈杭亭,曹淑琴,曾宪津.电感耦合等离子体质谱方法在生物样品分析中的应用[J].分析化学,2001,29(5):592-600
[12]Rittenberg D,Ziff Morris,Chargaff Ervin.Determination of the bases of phospholipids by the isotope dilution method[J].J.Biol.Chem.,1940,133:737
[13]Gest H,Kamen M D,Reiner J M.The theory of isotope[J].Arch.Biochem.,1947,12(2):273
[14]Hintenberger H.Electromagnetically Enriched Isotopes and Mass Spectrometry[M].Lundon:Butter-worth Publication,1956:123-198
[15]赵墨田,曹永明,陈刚,等.无机质谱概论[M].北京:化学工业出版社,2006:10-126
[16]Moens L.Applications of mass spectrometry in the trace element analysis of biological materials[J].J.Anal.Chem.,1997,359(4-5):309-316
[17]Johanna S B.State-of-art and progress in precise and accurate isotope ratio measurements by ICP-MS and LA-ICP-MS[J].J.Anal.At.Spectrom.,2002,17:1172-1185
[18]Heumann K G.Isotope dilution mass spectrometry[J].Int.J.Mass Spectrom.Ion Processes,1992,118:575-592
[19]刘炳寰等.质谱学方法与同位素分析[M].北京:科学出版社,1983:133-209
[20]刘雪梅,刘钊,杨天丽,等.电感耦合等离子体质谱人发中的微量锌[J].质谱学报,2005,26(suppl):3-4
[21]Sturup S.Application of HR-ICP-MS for the simultaneous measurement of zinc isotope ratios and total zinc content in human samples[J].Anal.At.Spectrom.,2000,15:315-321
[22]潘海燕,陆梅.原子吸收法测定土壤中铜和锌的不同消解方法比较[J].贵州环保科技,2004,10(4):45-46
[23]刘立行,赵国利.消解氨溶-火焰原子光谱法测定氯丁橡胶中的钠、镁、锌[J].冶金分析,2003,23(3):22-25
[24]傅明,陈新焕,杨万彪,等.微波消解ICP-AES法测定茶叶中铅、砷、铜、铁、锌、硒等12种元素的含量[J].食品科学,2001,22(11):76-78
[25]Bou R,Guardiola F,Padro A,et al.Validation of mineralization procedures for the determination of selenium,zinc,iron and copper in chicken meat and feed samples by ICP-AES and ICP-MS[J].J.Anal.At.Spectrom.,2004,19:1361-1369
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