反射式飞行时间质谱仪结合纳升电喷雾电离源研究金属簇合物

An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-flight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the “ionization” process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au₂₀(PPhpy₂)₁₀Cl₂](SbF₆)₄, where PPhpy₂=bis(2-pyridyl)phenylphosphine, and [Au₆Ag₂(C)L₆](BF₄)₄, where L=2-(diphenylphosphino)-5-methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi-nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.     

电感耦合等离子体质谱中有机试剂的基体效应研究

研究了乙醇、丙醇、丙三醇、乙酸、乙二胺和三乙醇胺等与水互溶的有机试剂对不同质量和电离曜闰元素质谱信号的影响。在优化的工作条件下,溶液中加入少量的乙醇、丙醇、丙三醇、乙酸、乙二胺或三乙醇胺对电离能在９～１１ｅＶ的元素的信号有不同程度的增强,附加乙二胺或三乙醇胺对Ｈｇ信号的增强效应显著大于乙醇、丙醇和丙三醇等试剂;探讨了乙二胺和三乙醇胺对Ｈｇ的信号增强机理。利用乙二胺或三乙醇胺对Ｈｇ的信号增强的特性,     

Thermal Ionization and Inductively Coupled Plasma Mass Spectrometry: Potential for Application to Studies on the Biokinetics of Molybdenum in Humans

Abstract

The use of stable isotopes as tracers in biokinetic investigations provides a means to obtain important metabolic data directly in humans without exposing the subjects to undue risks. In this work, three types of mass spectrometers are compared with regard to the determination of the abundances of stable isotopes of molybdenum in natural and enriched aqueous samples. The data show a good response of thermal ionization mass spectrometry (TIMS) and of high-resolution inductively coupled plasma mass spectrometry (ICPMS) to the isotopic enrichment of the samples, whereas conventional quadrupole ICPMS shows an unsatisfactory reproducibility of the results. Moreover, only TIMS can achieve an accuracy of better than 1% for the obtained isotopic ratios. Although a tedious procedure for the preparation of the biological samples is required and less sensitivity is achieved as compared to ICPMS, TIMS still seems to be method of choice for the accurate assessment of isotope ratios as required in multitracer studies on human biokinetics of trace metals.     

液液萃取-高效液相色谱-电感耦合等离子体质谱同时测定海水中的多种有机锡

利用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP/MS)联用技术对海水中的五种有机锡[三甲基氯化锡(TMT)、二丁基氯化锡(DBT)、三丁基氯化锡(TBT)、二苯基氯化锡(DPhT)和三苯基氯化锡(TPhT)]进行了分离,采用Agilent TC-C18色谱柱,流动相为乙腈/水/乙酸(65∶23∶12, φ),0.05%三乙胺,pH 3.0,流速为0.6 mL·min-1, 测定了0.5～100 μg·L-1范围内五种有机锡化合物的混合标准工作曲线,其相关系数R2优于0.998,方法的检出限均小于3 ng·L-1。100 mL海水样品用10 mL含有0.2% Tropolone的CH₂Cl₂萃取两次后,有机相合并氮吹浓缩至最后一滴,加入1 mL的乙腈,用0.2 2 μm的有机滤膜过滤后分析。结果表明,海水中只检测到TPhT,含量为53.2 ng·L-1。样品的加标证明DBT, DPhT, TBT和TPhT的加标回收率均优于80%。TMT可能存在吸附或降解问题,回收率仅为50%。     

超声浸提-No Gas-电感耦合等离子体质谱法测定工作场所空气中铊及其化合物

铊(Thallium,Tl)是一种有毒的金属元素,主要用于半导体、电子设备、农药和灭鼠剂的生产,会对职业人群的身体健康造成潜在的威胁,工作场所空气中铊及其化合物浓度的测定对保证职业人群的健康具有重要意义.虽然工作场所空气中痕量铊的毒性高于其他有毒金属元素,但对其研究却很少.目前工作场所空气中铊及其化合物浓度检测方法主要...     

基于电感耦合等离子体质谱法和化学计量学鉴别蜂蜜品种研究

开展了一种用电感耦合等离子体质谱仪(ICP-MS)结合主成分分析(principle component analysis)和判别分析(discrimination analysis)识别蜂蜜品种的研究。实验选取三种不同品种的蜂蜜: 洋槐蜜, 葵花蜜和油菜蜜, 经湿法消解等预处理后, 利用ICP-MS分别测得蜂蜜样品中20种矿质元素的含量。结果表明电感耦合等离子体质谱法的精密度, 准确度以及回收率等满足要求, 洋槐蜜在主成分得分图上呈现一定的聚集趋势, 而葵花蜜和油菜蜜的聚集趋势不明显, Na, Mg, K, Ca, Sr, Ba, V, Fe, Ni, Sb等十种矿质元素能够成为鉴别蜂蜜品种的特征元素;通过逐步判别分析筛选出Mg, Sr, Ba, Ni, Sb, Cr和Na等七种矿质元素, 并利用贝叶斯判别对这些元素建立线性判别函数, 其中洋槐蜜的判别率为100%, 葵花蜜的判别率为80.8%, 有两个葵花蜜样品误判为油菜蜜, 油菜蜜的判别率为 90.9%, 有一个油菜蜜样品误判为洋槐蜜, 模型交叉验证总判别率为90.3%, 说明矿质元素对蜂蜜品种鉴别具有良好的分类和鉴别效果, 能够为研究蜂蜜品种与矿质元素之间的关系提供理论依据, 该方法具有简单、准确、稳定等特点, 可作为蜂蜜品种鉴别的可靠方法。     

基于电感耦合等离子体质谱法和化学计量学鉴别蜂蜜品种研究

开展了一种用电感耦合等离子体质谱仪(ICP-MS)结合主成分分析(principle component analysis)和判别分析(discrimination analysis)识别蜂蜜品种的研究。实验选取三种不同品种的蜂蜜：洋槐蜜,葵花蜜和油菜蜜,经湿法消解等预处理后,利用ICP-MS分别测得蜂蜜样品中20种矿质元素的含量。结果表明电感耦合等离子体质谱法的精密度,准确度以及回收率等满足要求,洋槐蜜在主成分得分图上呈现一定的聚集趋势, 而葵花蜜和油菜蜜的聚集趋势不明显,Na,Mg,K,Ca,Sr,Ba,V,Fe,Ni,Sb等十种矿质元素能够成为鉴别蜂蜜品种的特征元素;通过逐步判别分析筛选出Mg,Sr,Ba,Ni,Sb,Cr和Na等七种矿质元素,并利用贝叶斯判别对这些元素建立线性判别函数,其中洋槐蜜的判别率为100%,葵花蜜的判别率为80.8%,有两个葵花蜜样品误判为油菜蜜,油菜蜜的判别率为 90.9%,有一个油菜蜜样品误判为洋槐蜜,模型交叉验证总判别率为90.3%,说明矿质元素对蜂蜜品种鉴别具有良好的分类和鉴别效果,能够为研究蜂蜜品种与矿质元素之间的关系提供理论依据,该方法具有简单、准确、稳定等特点, 可作为蜂蜜品种鉴别的可靠方法。