电感耦合等离子体质谱检测人体血铋浓度方法的建立

目的建立检测人体血液中重金属铋含鼍的检测方法。方法用直接稀释法，采用带碰撞／反应池的电感耦合等离子体质谱仪（ICP-MS）检测血铋浓度。结果该方法最低检出限为0．06ng／L。批内相埘标准偏差（RSD）为2．27％，平均回收率为93．06％。高、低2个水平的质控结果均在允许范围内。结论采用ICP-MS可以快速、简便、准确地测定人体血液中铋含量，为临床治疗提供客观依据，减少毒副反应。     

电感耦合等离子体质谱检测人体血铋浓度方法的建立

目的建立检测人体血液中重金属铋含量的检测方法。方法用直接稀释法,采用带碰撞/反应池的电感耦合等离子体质谱仪(ICP-MS)检测血铋浓度。结果该方法最低检出限为0.06 ng/L。批内相对标准偏差(RSD)为2.27%,平均回收率为93.06%。高、低2个水平的质控结果均在允许范围内。结论采用ICP-MS可以快速、简便、准确地测定人体血液中铋含量,为临床治疗提供客观依据,减少毒副反应。     

电感耦合等离子体质谱仪在血流感染早期诊断中的初步应用

目的使用电感耦合等离子体质谱仪(ICP-MS)研究血流感染患者血清中的金属元素水平,探讨金属元素在血流感染患者血清中的浓度变化以及和感染病原菌之间的相关性,获得差异表达的金属元素图谱,评价将此类质谱仪应用于血流感染早期诊断的可行性。方法收集血流感染患者的血清作为血流感染组,同时分离出血液中的病原菌,按病原菌种类将标本分类,选用健康者血清作为阴性对照组。运用ICP-MS测定患者血清中各类金属元素含量的变化,使用主成分分析(PCA)和偏最小二乘法判别分析(PLS-DA)绘制金属元素图谱,寻找出浓度明显改变的金属元素,组间各金属元素的相关性研究使用Pearson相关性分析。结果一共建立了4个病原菌血流感染的金属元素图谱(包含金黄色葡萄球菌、大肠埃希菌、粪肠球菌和肺炎克雷伯菌),血流感染组与对照组间有浓度明显改变的金属元素,包括钯、金、钍、锡等;Pearson相关性分析显示这些金属元素与血流感染和感染菌种类之间均有相关性,如钙与金黄色葡萄球菌血流感染呈负相关性(r=-0.788),钯和金均与大肠埃希菌的血流感染呈正相关性(r=0.906、0.748)。结论从上述研究结果看,具有差异性的金属元素图谱可以作为血流感染早期诊断、预防和预后的潜在标志物,其应用性值得进一步的深入研究。     

电感耦合等离子体质谱法测定透析用水中微量元素

目的 建立一种同时测定透析用水中多种微量元素的方法.方法 以Rh、Ir为内标,采用电感耦合等离子体-质谱法（ICP-MS）同时测定透析用水中As、Ag、Ba、Cr、Cu、Cd、Pb、Se、Sn、Znl0种微量元素.结果 本方法的线性范围宽,灵敏度高,线性相关系数均不低于0.999,相对标准偏差在1.28％-5.69％之内,各个元素的加标回收率在97.4％-100.9％之间.结论 本方法准确、快速、便捷,能为透析用水安全提供有力保障.     

电感耦合等离子体原子发射光谱法测定血锰及儿童血锰含量调查

目的探索电感耦合等离子体原子发射光谱(ICP-AES)法测定血锰的方法,及对南京地区儿童血锰含量的调查分析.方法全血经1 mol/L 硝酸处理后用ICP-AES法测定.结果方法精密度为1.42%～2.39%,回收率为95.9%～98.9%,南京地区1 027名健康儿童血锰含量为(4.89±2.67)μg/L.结论全血经硝酸处理后测定血锰,精密度及回收率均较理想,可以作为测定血锰的参考方法,并初步提出该方法的南京地区儿童血锰含量参考范围为2.22～7.56 μg/L(1岁以下儿童除外),供临床参考.     

电感耦合等离子体原子发射光谱法测定血锰及儿童血锰含量调查

目的探索电感耦合等离子体原子发射光谱(ICP-AES)法测定血锰的方法,及对南京地区儿童血锰含量的调查分析。方法全血经1 mol/L硝酸处理后用ICP-AES法测定。结果方法精密度为1.42%~2.39%,回收率为95.9%~98.9%,南京地区1 027名健康儿童血锰含量为(4.89±2.67)μg/L。结论全血经硝酸处理后测定血锰,精密度及回收率均较理想,可以作为测定血锰的参考方法,并初步提出该方法的南京地区儿童血锰含量参考范围为2.22~7.56μg/L(1岁以下儿童除外),供临床参考。     

电感耦合等离子体质谱技术直接测定全血中微量元素的方法及检测过程的质量控制

<正>目前,微量元素分析尤其是对毒性较大的重金属元素和一些有益微量元素的分析,受到越来越多的关注和重视[1-4]。人体血液中的微量元素可分为几类:1)有毒有害重金属元素:砷、镉(Cd)、铅(Pb)、汞、铊、铍(Be);2)潜在的有毒元素:铝(Al)、     

同位素稀释电感耦合等离子体质谱分析及其在临床检验中的应用

电感耦合等离子体质谱（ICP-MS）是20世纪80年代发展起来的分析测试技术，它以独特的接口将电感耦合等离子体的高温电离特性与四极杆质谱仪的灵敏快速扫描特性相结合，近年来已成为痕量、超痕量无机成分及同位素分析公认的可靠分析技术。该技术具有检出限低、动态线性范围宽、谱线简单、分析精密度高、分析速度快、可提供同位素信息以及可同时测定多种元素等特征，已广泛应用于地质、环境、生物、医学、冶金和化工等多种研究领域。     

电感耦合等离子质谱法检测儿童末梢血多种元素

目的建立同时检测儿童末梢血多种元素的电感耦合等离子质谱(ICP-MS)法。方法采用ICP-MS法检测湖南地区474例健康儿童(6个月至12岁)末梢血标本钙、镁、铁、铜、锌、铅6种元素水平,并建立各元素的参考区间。结果健康儿童末梢血钙、镁、铁、铜、锌、铅水平均呈偏态分布,且男女儿童末梢血各元素水平比较,差异均无统计学意义(P0.05);该地区健康儿童末梢血钙、镁、铁、铜、锌、铅参考区间分别为57.30~81.40 mg/L、30.40~44.80 mg/L、361.20~531.40 mg/L、848.10~1 469.20μg/L、2.68~6.54mg/L和0.00~100.00μg/L。结论成功建立了同时检测儿童末梢血钙、镁、铁、铜、锌、铅6种元素的ICP-MS法,以及各元素的参考区间。     

肝豆状核变性患者青霉胺治疗期间晨尿金属元素谱分析

目的了解肝豆状核变性（WD）患者应用青霉胺治疗期间晨尿中多种金属元素的变化。方法收集WD患者23例,青霉胺治疗时间3个月～180个月以上并低铜饮食;正常对照者18名,分别收集晨起尿液。使用电感耦合等离子体质谱仪（ICP-MS）分析尿液中铬、铁、钴、硒、锰、铜、锌、钙、镁、锂、铝、钒、镍、镓、砷、锶、镉、铯和钡19种元素。结果晨尿中7种必需微量元素（铬、铁、钴、硒、锰、铜和锌）检测结果显示WD组的尿铬、铜和锌浓度明显高于对照组（P〈0.01）。晨尿中10种非必需微量元素（锂、铝、钒、镍、镓、砷、锶、镉、铯和钡）检测结果显示WD组的尿砷、镉、镓、锶、铯和钡明显高于对照组（P〈0.05）。WD组晨尿中宏量元素尿钙明显高于对照组（P〈0.01）。结论在肝豆状核变性患者使用青霉胺驱铜治疗期间,除了晨尿中的尿铜增高外,晨尿中尿铬、锌、砷、镉、镓、锶、铯、钡和钙也明显高于对照组。晨尿铜可以作为一个监测WD患者驱铜疗效的指标。     

Method validation for a multi-element panel in serum by inductively coupled plasma mass spectrometry (ICP-MS)

BackgroundLaboratory testing for trace and toxic elements is important to diagnose metal toxicity and nutritional deficiency. There are several essential elements that are necessary for biological function and non-essential elements that can pose risk from exposure. Both essential and nonessential elements can be toxic if concentrations exceed a certain threshold.MethodsAn aliquot of serum was diluted in a diluent solution, which contained iridium (Ir) as the internal standard, gold (Au), 0.05% Triton X-100, and 1% nitric acid (HNO3). The diluted specimen was aspirated into an inductively coupled plasma-mass spectrometer for quantitative elemental analysis of chromium (Cr), cobalt (Co), copper (Cu), manganese (Mn), nickel (Ni), selenium (Se) and zinc (Zn). The sample was introduced into the instrument spray chamber to form aerosol droplets, then atomized and ionized in argon plasma. The ions exited the plasma, passed through the interface of the instrument, then arrived at the entrance of the collision cell where helium gas was introduced to remove polyatomic interferences by kinetic energy discrimination (KED). After exiting the collision cell, the ions were filtered by a quadrupole mass spectrometer.ResultsThe analytical measurement range was determined specifically for each element. Imprecision was <20% CV for the lowest limit of quantification for each element and accuracy was within ±15%.ConclusionsThis method was validated for the quantification of seven elements in serum to assess nutritional deficiency and toxicity. The multi-element panel by ICP-MS met the validation criteria for biological monitoring of trace and toxic elements in patient specimens.     

基于电感耦合等离子体质谱法血清钙离子检测候选参考方法的建立

目的基于电感耦合等离子体质谱法(ICP-MS),建立一种检测血清钙离子的候选参考方法。方法方法学建立.将从医院收集到的血清标本以0.3%硝酸溶液直接稀释100倍,在血清标本基质溶液中添加不同浓度钙标准溶液,配制含血清基质的标准品溶液。以锗(Ge)为内标,采用标准加入法,计算血清钙离子浓度。对所建立的候选参考方法进行线性、精密度、正确度的性能评估和方法比对。结果血清钙离子浓度在0.000~20.400 mmol/L内(稀释后浓度为0.000~0.204 mmol/L)线性良好(R2>0.9999);批内不精密度为0.22%~0.47%,批间不精密度为0.64%~0.77%,总不精密度为0.98%~1.09%;检测3个浓度SRM 956d,结果均在证书要求的不确定度范围内,相对偏移分别为-0.16%,0.04%,0.23%;该方法参加2017年参考实验室外部质量评价计划(RELA),比对通过。与检验医学溯源联合委员会(JCTLM)所列参考方法进行比较,结果一致性良好。本研究所建立的候选参考方法与临床常规电极方法进行比较,具有良好的相关性。结论成功建立血清钙离子检测候选参考方法,线性范围宽、具有良好的精密度与准确度。     

电感耦合等离子体质谱测定血清钠

目的 建立一种应用电感耦合等离子体质谱(ICP-MS)测定血清中钠(Na)元素含量的候选参考方法.方法 以铝(Al)作为Na的内标用重量法加入到标准溶液和血清中,样品经过硝酸消解、稀释,以ICP-MS测定其23Na/27Al同位素比值,应用标准曲线法定量.结果 应用ICP-MS测定2份血清中Na的平均分析回收率分别为100.67%和100.15%,精密度分别为0.08%和0.04%.标准参考物质(SRM)909b两水平血清Na浓度的总变异系数分别为0.18%和0.22%,结果与认定值的中间值偏差分别为0.17%和0.14%,SRM956b 3水平血清Na浓度的总变异系数分别为0.41%、0.41%和0.66%,结果与认定值的中间值偏差分别为-0.09%、-1.05%和-0.48%.结论 建立了ICP-MS测定血清Na的方法,此法操作简单快速、准确、精密,有望成为血清Na测定的参考方法.     

Analysis of 17 elements in cow,goat, buffalo,yak, and camel milk by inductively coupled plasma mass spectrometry (ICP-MS)

We analyzed the concentrations of 17 elements including arsenic (As), lead (Pb), cadmium (Cd), chromium (Cr), copper (Cu), nickel (Ni), zinc (Zn), strontium (Sr), tin (Sn), aluminum (Al), potassium (K), calcium (Ca), magnesium (Mg), iron (Fe), manganese (Mn), sodium (Na), and selenium (Se) in cow, goat, buffalo, yak, and camel milk in China using inductively coupled plasma mass spectrometry. The concentrations of the elements varied and depended on the milk type. K, Ca, Na, and Mg were the most abundant elements. Fe and Zn concentrations ranged from 1 to 6 μg g⁻¹, while Cu, Al, and Mn concentrations ranged from 0.1 to 1 μg g⁻¹. Trace elements, especially toxic trace elements, were present at very low concentrations; however, Pb concentrations in cow milk reached the MRLs established by the Codex Alimentarius Commission. Data were analyzed by chemometrics to evaluate the correlations between elements in the milk samples. PCA and factor analysis highlighted the relationship between element distribution and milk type. The LDA model correctly identified most milk types. Element analysis combined with chemometrics can be used to distinguish milk types.

17 elements in cow, goat, buffalo, yak, and camel milk were determined by ICP-MS; element analysis combined with chemometrics can be used to distinguish milk types.     

Use of flow field-flow fractionation and single particle inductively coupled plasma mass spectrometry for size determination of selenium nanoparticles in a mixture

Various analytical techniques have been used for size analysis of selenium nanoparticles (SeNPs). These include flow field-flow fractionation (FlFFF), single particle inductively coupled plasma mass spectrometry (SP-ICP-MS), dynamic light scattering (DLS) and transmission electron microscopy (TEM). For hydrodynamic diameter estimation, the FlFFF technique was used and the results were compared with those analyzed by DLS. For core diameter estimation, the results obtained from SP-ICP-MS were compared with those from TEM. Two types of FlFFF channel were employed, i.e., symmetrical FlFFF (Sy-FlFFF) and asymmetrical FlFFF (Asy-FlFFF). Considering the use of FlFFF, optimization was performed on a Sy-FlFFF channel to select the most appropriate carrier liquid and membrane in order to minimize problems due to particle membrane interaction. The use of FL-70 and 10 kDa RC provided an acceptable compromise peak quality and size accuracy for all samples of SeNPs which were coated by proteins (positively charged SeNPs) and sodium dodecyl sulfate (negatively charged SeNPs). FlFFF always yielded the lower estimate of the hydrodynamic size than DLS as a reference method. The results obtained by SP-ICP-MS were consistent with the TEM method for the core diameter estimation. The results from FlFFF and the DLS reference method were significantly different as confirmed by paired t-test analysis, while the results provided by SP-ICP-MS and the TEM reference method were not significantly different. Furthermore, consecutive size analysis by SP-ICP-MS for the fractions collected from FlFFF was proposed for sizing of SeNP mixtures. The combined technique helps to improve the size analysis in the complex samples and shows more advantages than using only SP-ICP-MS.

Various analytical techniques have been used for size analysis of selenium nanoparticles (SeNPs).     

Simultaneous determination of alpha-fetoprotein and free beta-human chorionic gonadotropin by element-tagged immunoassay with detection by inductively coupled plasma mass spectrometry

BACKGROUND: An inductively coupled plasma mass spectrometry (ICP-MS)-based immunoassay has been proposed independently by Baranov et al. (Anal Chem 2002;74:1629-36) and our group, but the applicability of this method for multianalyte analysis in clinical samples has not been fully illustrated. We developed a dual-label immunoassay method for the simultaneous determination of alpha-fetoprotein (AFP) and free beta-human chorionic gonadotropin (hCGbeta) in human serum. METHODS: Monoclonal antibodies immobilized on microtiter plates captured AFP and hCGbeta, which were detected by use of Eu(3+)-labeled anti-AFP and Sm(3+)-labeled anti-hCGbeta monoclonal antibodies. Eu(3+) and Sm(3+) were dissociated from the immunocomplex with HNO(3) solution (10 mL/L) and delivered by peristaltic pump to the ICP mass spectrometer. RESULTS: The measurable ranges of AFP and hCGbeta were 4.6-500 and 5.0-170 microg/L, respectively, with detection limits of 1.2 and 1.7 microg/L (3 SD above mean of zero calibrator), respectively. The intraassay imprecision (CV) for AFP was 8.3%, 4.0%, and 2.7% at 16.3, 86, and 354 microg/L, respectively, and the interassay CV was 10%, 5.7%, and 3.5%. For hCGbeta, the intraassay CV was 5.4%, 6.4%, and 3.1%, respectively, at 10.5, 45.2, and 105 microg/L, and the interassay CV was 7.2%, 8.0%, and 3.7%. Comparison with IRMAs for AFP and hCGbeta yielded correlation coefficients (r(2)) of 0.97 and 0.95. CONCLUSIONS: Two proteins can be measured simultaneously by immunoassays using two rare earth elemental tags (Eu(3+) and Sm(3+)) and ICP-MS detection. The multielement capability and the multiple potential elemental labels make ICP-MS attractive for multianalyte immunoassays. Implementation of ICP-MS-linked immunoassays may be relatively straightforward because the labeling and immunoreaction procedures have been well developed for clinical time-resolved immunofluorometric assays.     

ICP-AES法测定全血锰的方法学评价

目的对电感耦合等离子体发射光谱法(ICP-AES)测定血锰进行方法学评价,并应用于日常检测工作。方法全血样本经1 mol/L硝酸处理后吸取上清液,采用ICP-AES在279.544 nm处测定样本,评价其精密度、回收率、灵敏度及抗干扰能力;同时采用ICP-AES测定1 027名健康体检儿童的全血锰浓度,确定正常参考范围。结果 ICP-AES测定血锰的批内变异系数(CV)为6.2%～6.6%,批间CV为7.1%～7.6%,总CV为7.2%～7.8%,相对偏差(RSD)为1.66%～2.36%,加标回收率为95.0%～96.9%,线性方程为Y=7 035.6X+759.02,r=0.999 7;在水空白和100μg/L锰标准储备液中按1∶1分别加入25 mg/L钾、钠、氯、钙、镁标准溶液和2 mg/L铁标准溶液后未检测出锰浓度有明显变化。1 027名健康体检儿童的全血锰正常参考范围为(4.89±2.67)μg/L。结论 ICP-AES检测全血锰未发现明显系统误差,且精密度高、准确度好,可作为检测全血锰的常规方法。     

Determination of aluminum in bone in haemodialyzed patients, using inductively coupled argon plasma emission spectrometry

We propose a new method for measuring aluminium in bone tissue, using argon plasma emission spectrophotometry. The detection limit in the bone nitric digestion liquid was 0.015 mumol/l (corresponding to 0.0075 mumol/g, i.e. 0.2 microgram/g for a tissue sample with 1.0 g wet weight). Within-run CVs were 4.66% and 1.43% for tissues containing 0.15 and 0.64 mumol/g, respectively. Other bone constituents such as calcium, phosphorus, magnesium, sodium, potassium, do not affect aluminum results. Normal values obtained in bone of subjects not suspected of aluminium intoxication were: mean +/- SD; 0.09 +/- 0.044 mumol/g (n = 24). In dialysis patients we found a mean bone aluminium content of 0.75 mumol/g for concentrations ranging between 0.16 and 3.38 mumol/g.