电感耦合等离子体质谱法( ICP-MS)测定地下水中痕量元素

用电感耦合等离子体质谱法(ICP-MS)测定了地下水中痕量元素(Cd、Co、Cr、Cu、Mn、Mo、Ni、Pb、As、Se、Zn、Ba、Fe),应用在线加入内标校正干扰效应,元素检出限为0.002-0.179 μg,/L,加标回收率为96.50 ％～103.10％,相对标准偏差(RSD)＜2.31％.试验结果表明该法测...     

微波消解-ICP-MS法测定人发中多种必需微量元素的研究

目的：建立微波消解-电感耦合等离子体质谱（ICP-MS）法同时测定人发中锰、钴、镍、铜、锌5种必需微量元素的方法。方法：采用硝酸-过氧化氢消解体系,微波消解法处理样品,直接用ICP-MS同时测定上述5种元素。结果：方法的检出限为0．007-0．036μg/L,标准曲线线性关系良好（r〉0．9999）,相对标准偏差（RSD）小于3％,对人发标准物质的测定值均在标准参考值范围内。结论：应用微波消解-ICP-MS法分析发样,方便快捷,灵敏度高,线性范围宽,准确度好。     

微波消解-电感耦合等离子体质谱法测定金红石矿中15种稀土元素

应用氢氟酸、硝酸做为消解溶剂,通过优化微波消解程序对红金石矿样品进行前处理,电感耦合等离子体质谱法测定红金石矿中的15种稀土元素。试验结果表明,相关系数介于0.999 1~1.000 0之间,测定精密度RSD%低于7.36%,回收率在92.3%~106.9%之间。该方法具有线性范围宽、速度快、检出限低、准确度和精密度高等优点,适合红金石矿中稀土元素的测定。     

微波消解-电感耦合等离子体质谱法测定湿基草莓中15种微量稀土元素

应用微波消解进行样品前处理,电感耦合等离子体质谱法测定湿基草莓中的15种微量稀土元素。试验结果表明,该方法相关系数(r)在0.999 5~1.000 0之间,方法回收率在94.2%~106.4%之间,方法精密度(RSD%)低于6.92%。该方法具有前处理过程简单、引入干扰少、准确度、精密度、检出限满足要求,同时具有线性范围广、测试速度快等特点,适合湿基草莓样品中微量稀土元素的测定。     

抗癌中草药中8种元素的压力密闭消解电感耦合等离子体质谱分析

采用HNO_3-HCl-H_2O_2-HF体系压力密闭消解、电感耦合等离子体质谱法测定了抗癌中草药中的8种元素,分析国家杨树叶标准物质结果与相应标准值一致。该方法准确、快速,适合抗癌中草药中的元素分析。同时还研究了8种元素在12种抗癌中草药中的分部,对抗癌中草药资源开发和临床应用具有一定的参考价值。     

电感耦合等离子体发射光谱法测定白酒的28种微量元素

应用电感耦合等离子体发射光谱仪(ICP-AES),不经消解直接测定8种白酒中的Al,As,B,Ba,Be,Ca,Cd,Co,Cr,Cu,Fe,K,Li,Mg,Mn,Mo,Na,Ni,Pb,Pd,S,Sb,Si,Sr,Ti,V,W,Zn元素并对方法的仪器条件进行了优化。与传统的消解方法进行比较,实验结果表明本方法的测定结果与消解的测定结果基本一致。本方法各元素线性相关系数均大于0.9995,加标回收率在94%~105%之间。本方法不需要消解,大大提高了样品的测试速度并且节省人力物力。本实验为白酒品质的鉴定提供实验数据。     

应用电感耦合等离子体质谱法检测地表水中铅元素的含量

通过电感耦合等离子体质谱法检测地表水中铅元素的含量,方便、快速、准确的得出实验结果,同时进行加标回收实验来验证方法的准确性和可靠性。     

Review about Powerful Combinations of Advanced and Hyphenated Sample Introduction Techniques with Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) for Elucidating Trace Element Species in Pathologic Conditions on a Molecular Level

Element analysis in clinical or biological samples is important due to the essential role in clinical diagnostics, drug development, and drug-effect monitoring. Particularly, the specific forms of element binding, actual redox state, or their spatial distribution in tissue or in single cells are of interest in medical research. This review summarized exciting combinations of sophisticated sample delivery systems hyphenated to inductively coupled plasma-mass spectrometry (ICP-MS), enabling a broadening of information beyond the well-established outstanding detection capability. Deeper insights into pathological disease processes or intracellular distribution of active substances were provided, enabling a better understanding of biological processes and their dynamics. Examples were presented from spatial elemental mapping in tissue, cells, or spheroids, also considering elemental tagging. The use of natural or artificial tags for drug monitoring was shown. In the context of oxidative stress and ferroptosis iron, redox speciation gained importance. Quantification methods for Fe²⁺, Fe³⁺, and ferritin-bound iron were introduced. In Wilson’s disease, free and exchangeable copper play decisive roles; the respective paragraph provided information about hyphenated Cu speciation techniques, which provide their fast and reliable quantification. Finally, single cell ICP-MS provides highly valuable information on cell-to-cell variance, insights into uptake of metal-containing drugs, and their accumulation and release on the single-cell level.     

电感耦合等离子体质谱法(ICP-MS)测定莫西沙星侧链中钯金属残留

建立了电感耦合等离子体质谱(ICP-MS)测定莫西沙星侧链-(S,S)-2,8-二氮杂双环[4,3,0]壬烷中钯金属残留的方法。样品经强酸高温消解后,采用ICP-MS测定。钯在2.0～20μg/L范围内线性关系良好(r>0.999),在4、10和16μg/kg添加浓度下,方法回收率为87.3～98.5%,RSD为1.86～6.39%。方法检出限和定量限分别为2μg/kg、40μg/kg。该法快速、准确、灵敏高,可以用于莫西沙星侧链中钯元素测定。     

ICP-OES法测定印染废水中多种金属元素

建立了电感耦合等离子体发射光谱(ICP-OES)测定印染废水中Al、Cr、Mn、Fe、V、Ni、Cu、Zn、As、Pb等金属元素的分析方法。样品经微波消解后直接用ICP-OES测定,对影响测定的各种因素进行了较为详细的研究,确定了仪器的最佳工作参数,选择了合适的分析谱线。研究结果表明,10种金属元素的检出限在0.26～58.24μg/L之间;线性关系良好,线性相关系数R2≥0.999 9;精密度良好,RSD<3.1%;回收率为90.48%～108.46%。     

Determination of Anti-Tumor Constitute Mollugin from Traditional Chinese Medicine Rubia cordifolia: Comparative Study of Classical and Microwave Extraction Techniques

Abstract

Rubia cordifolia is a common traditional Chinese medicine (TCM) used for centuries for the treatment of cough, inflammation of the joints, uterine hemorrhage, and uteritis. Mollugin is a major active component present in R. cordifolia and recognized as a potential anti-tumor compound. In this work, a microwave-assisted extraction (MAE) method has been developed for extracting mollugin from R. cordifolia. Several variables that can potentially affect the extraction yield, namely extracting solvent, microwave power, extraction time, and solid-liquid ratio were optimized. The separation and quantitative determination of mollugin was carried out by HPLC with UV detection at 254 nm. Under appropriate MAE conditions, such as extraction time of 4 min, ethanol concentration of 70% (v/v), microwave power of 460 W, and solid-liquid ratio of 1:20 (g/mL), the extraction yield of mollugin from R. cordifolia with MAE was higher than conventional extraction methods such as Soxhlet extraction, heat reflux extraction, and ultrasonic-assisted extraction. Due to the considerable saving in time and its higher extraction yield, the proposed MAE procedure was obviously a more rapid and effective sample preparation technique.     

用先进适用技术和高新技术提升我国传统法尿素装置(3)--改进型高效组合法

介绍了瑞士Casale公司开发的高效组合法(HEC)尿素装置改造工艺,用综合学科研究法讨论了HEC工艺高压合成区和亚高压汽提区的工艺参数,探讨了HEC工艺氨碳摩尔比的适宜值,结果表明,该值的优化数值解为3.3~3.5。探讨了对HEC工艺的改进,提出了改进型高效组合法新工艺,阐述了用该工艺改造我国传统法尿素装置的工艺参数、技术特点、扩产性能和关键技术,认为改进型高效组合法新工艺可以优化甲铵冷凝器的操作,使之输出1.0~1.1 MPa的副产蒸汽,其第一合成塔转化率比HEC工艺提高1%~2%。