High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry for the Determination of Arsenic Content and Speciation in Enteromorpha

使用高效液相色谱-电感耦合等离子体质谱(HPlC-ICP-MS)联用技术对浒苔中的砷总量及其存在的化学形态进行分析。总量分析结果表明,青岛海域的浒苔样品中砷总量介于3.0~9.7μg/g之间。在总量测定的基础上,对浒苔样品的水煮提取液进行形态分析。结果表明,浒苔中主要含有无机五价砷和一种疑为砷糖的物质以及少量的二甲基胂酸(dMA)和无机三价砷。鉴于这些砷形态的毒性或潜在毒性,将其应用于食品及药物方面尚需谨慎。This study analyzed arsenic content and speciation in Enteromorpha sampled from various coastal zones of Qindao using high performance liquid chromatography coupled to inductively coupled plasma-mass spectrometry(HPLC-ICP-MS).The results showed that the total arsenic content in Enteromorpha was ranged from 3.0 to 9.7 μg/g.The speciation analysis of hot water extract of Enteromorpha indicated that the major arsenic forms in Enteromorpha were inorganic quinquevalence arsenate and a substance suspected as arsenic sugar.Besides,there were small amounts of inorganic trivalence arsenite and dimethylarsenate(DMA) in the extract.Due to the toxicity or potential toxicity of these arsenic forms,it should be paid great caution in the application of Enteromorpha as a material for food and medicine.国家自然科学基金项目(20675021);海洋一所基本科研专项(GY-022008T32

Determination of five poisonous elements in holothurian sold on the market by Microwave Digestion with ICP—MS

建立了微波消解—电感耦合等离子体质谱法测定海参中Cu,AS,Cd,Hg,Pb 5种有毒元素含量的方法,采用In元素为内标,利用其回收率对以上5种元素的测定结果进行校正,该方法变异系数(CV%)为0.2%--4.0%,In元素加标回收率为96.7%--104.5%,说明该方法灵敏度高,结果准确可信。利用该方法对10批不同市售海参中5种有毒元素含量进行了测定,结果表明10批市售海参中的AS含量均超标,部分批次海参中的Cd、Pb超标,说明市售海参确实存在有毒元素超标的问题。A method based on microwave sample digestion and inductively coupled plasma-mass spectrometry(ICP—MS) detection was established for determination of Cu,As,Cd,Hg and Pb in holothurian sold on the market.Indium was used as internal standard element to calibrate the results of determination of these five elements.Determination limits of these five elements were in the range of 0.006～0.063 μg/g,coefficient of variation(CV%)were in the range of 0.2%～4.0%,and the recovery of In was in the range of 96.7%～104.5%.The method has been applied to determine the five poisonous elements in ten holothurian samples sold on the market.The results indicated that the over-standard problem of poisonous elements in holothurian sold on the market existed.The content of total arsenic was over standard in all the ten samples,but the over standard problem of lead and cadmium was only found in part of the samples.国家自然科学基金(20675021);中国近海海洋综合调查与评价908专项(908-02-05-04)资

Determination of Trace Metal Elements in Crude Oils by Microwave Digestion-Inductively Coupled Plasma-Mass Spectrometry Assisted with Organic Solvent

李景喜( 1980 － ) ，男，山东临沂市人，研究实习员，从事分析化学研究。E-mail: jxli@fio．org． cn。[中文摘要]建立了二氯甲烷溶剂辅助微波消解-电感耦合等离子体质谱法测定原油中V、Cr、Fe、Ni、Cu、Zn、Mo、Co、Pb等16种微量金属元素。研究表明,用CH2Cl2分散原油样品,以浓HNO3-H2O2为消解体系,采用CEM微波消解系统消解样品,各元素线性关系良好,相关系数≥0.9995;检出限可达ng/L;方法精密度较高,相对标准偏差(RSD,n=3)<5.0%;回收率为92%～110%。以w(Ni)/w(V)与w(Fe)/w(V)比值为变量参数对不同原油样品进行聚类分析,表明国内与国外不同地区原油样品中各金属元素含量差异较大。[英文文摘]A method for determination of V,Cr,Fe,Ni,Cu,Zn,Mo Co,Pb,etc in different crude oils was established by inductively coupled plasma-mass spectrometry assisted with organic solvent microwave digestion.The oil sample was digested by microwave using HNO3-H2O2 as oxidant after dispersing in organic solvent(CH2Cl2).The results showed that the detection limits of the method reached ng/L level for sixteen elements.The linear correlation of the method was preferable with the correlation coefficient of better than 0.9995． The recoveries of the method were in the range of 92% ～ 110% with the precision of less than 5.0% RSD (n=3)．The ratios of w(Ni)/w(V) and w(Fe)/w(V) were distinct in different crude oil samples from oversea and domestic，and the index can be used to the cluster analysis for differencing the crude oil samples．国家海洋局第一海洋研究所基本科研业务费专项资助(2010G23);海洋公益性行业科研专项资助(200705011);海洋溢油鉴别与损害评估技术重点实验室开放基金资助(200920

Nonradioactive Iodine-Labeled Antibodies-Inductively Coupled Plasma Mass Spectrometry for Immunoassay

研究了非放射性碘标记-电感耦合等离子体质谱免疫分析体系,该体系以兔抗大肠杆菌作为模型抗原,羊抗兔Igg蛋白为抗体,建立了一种新的免疫分析方法。实验中采用溴代琥珀酰胺(nbS)为氧化剂,实现非放射性127I标记羊抗兔Igg蛋白,探索了标记的最佳条件,标记率为63.12%;标记物在SEPHAdEX g50柱上分离纯化后,研究了I-羊抗兔蛋白的稳定性,结果表明,标记物在4℃放置96 H后几乎没有碘脱落,并保持一定的活性。实验中采用聚苯乙烯96孔板作为固相载体进行免疫反应,以电感耦合等离子体质谱为检测手段,方法的检出限为0.12 Mg.l-1,rSd(n=9)为3%;该体系也可适用于其他活性蛋白、核酸等的标记和分析。In the present study,the system of nonradioactive iodine-labeled-antibodies linking inductively coupled plasma mass spectrometry for immunoassay was reported.The goat-anti-Escherichia coli and goat anti rabbit were considered as simulant antigen and antibody respectively in order to establish a new method of immunoassay by inductively coupled plasma mass spectrometry which has the advantage of high sensitivity,low detection limit and preferable linearity range.During the experiment,the N-bromosuccinimide,a mild oxidant,was used to oxidize the non-radioactive iodine(127I) that labeled the protein.The method of nonradioactive iodine labeled protein was established and the best labeling condition was explored.The compound of I was purified by Sephadex G50 column chromatography,then the stability and activity were examined.The results showed that the labeling program was simple,reaction time was within two minutes,the labeling yield achieved 63.12% and none of I shed from the compound after 96 hours.The simulant antigen and antibody reacted on polystyrene microtiter plate and the I was detected by ICP-MS,the detection limit of the method was 0.12 mg·L-1,relative standard deviation(n=9) was less than 3% and the linearly dependent coefficient was 0.998 7.This system can also be used in analysis of other protein,nucleic acid and so on.海洋公益性行业科研专项项目(200705011);中国海监技术支撑体系项目;2008年海洋环境保护及节能减排专项项目资

7000m sea trials test of the deep manned submersible “JIAOLONG”

蛟龙号载人潜水器研制是国家863计划重大专项之一,其目标是建造出一台可以执行规定使命任务的产品。海上试验是载人潜水器重大专项的关键阶段,2009年8～10月、2010年5～7月和2011年7～8月,分别完成了1000米、3000米和5000米级的海上试验任务。文章主要介绍了在2012年6月3日～7月16日之间完成的7000米级海上试验,内容包括海上试验的基本情况、海试取得的主要技术和应用成果、海试过程中发现的故障及处理情况以及对今后投入应用的启示,最后给出7000米级海上试验的主要结论

Determination of Trace Metal Elements in Different Crude Oils and Their Cluster Analysis

采用二氯甲烷溶解、分散原油样品,以浓HnO3-H2O2为消解体系,采用微波法对原油进行消解,利用电感耦合等离子体质谱法(ICP-MS)测定原油中的V、nI、Cu、fE、Cr、zn、Pb、CO、MO、Ag等17种微量金属元素;并以6lI、45SC、72gE、89y、115In、159Tb、209bI为内标元素,补偿基体效应,选择适当的待测元素同位素克服质谱干扰,优化了实验条件。结果表明,原油中大多微量金属元素的检出限达到ng/l,仅fE、AS、Sb 3种元素的检出限相对较高;各元素线性关系良好,相关系数r不低于0.999 5;方法精密度较高,相对标准偏差(rSd)不大于5.0%,准确度较好,相对误差不高于10%。对不同原油样品以nI/V与fE/V值为变量进行聚类分析,结果发现,国内与国外不同地区原油样品具有明显差异性。An inductively coupled plasma mass spectrometric(ICP-MS) method was developed for the determination of V,Ni,Cu,Fe,Cr,Zn,Pb,Co,Mo,Ag,etc.in different crude oil.The oil sample dispersed firstly in organic solvent(CH2Cl2) and was digestded by microwave using HNO3-H2O2 as oxidant.6Li,45Sc,72Ge,89Y,115In,159Tb and 209Bi were selected as the internal standard elements.The matrix effect was compensated and the MS interference was corrected by selecting the suitable isotope of the elements.The experimental conditions were optimized.The results showed that,except for Fe,As and Sb,the detection limit of other elements could reached ng/L level.The correlation coefficients were not less than 0.999 5.The RSDs were no more than 5.0%,and the relative error was no more than 10%.The ratios of Ni/V and Fe/V of different crude oils were further analyzed by cluster analysis.The result showed that a big difference exisited in different crude oils from domestic and overseas.海洋公益性行业科研专项资助项目(200705011);国家海洋局第一海洋研究所基本科研业务费专项资金资助项目(2010G23);海洋溢油鉴别与损害评估技术重点实验室开放基金资助项目(200920

Measurement of integrated luminosity of data collected at 3.773 GeV by BESIII from 2021 to 2024

We present a measurement of the integrated luminosity e+e- of collision data collected by the BESIII detector at the BEPCII collider at a center-of-mass energy of Ecm = 3.773 GeV. The integrated luminosities of the datasets taken from December 2021 to June 2022, from November 2022 to June 2023, and from October 2023 to February 2024 were determined to be 4.995±0.019 fb-1, 8.157±0.031 fb-1, and 4.191±0.016 fb-1, respectively, by analyzing large angle Bhabha scattering events. The uncertainties are dominated by systematic effects, and the statistical uncertainties are negligible. Our results provide essential input for future analyses and precision measurements