非衍生-气相色谱串级质谱法测定饲料中三聚氰胺

针对衍生化-气相色谱串联质谱(选择离子监测法)的操作繁琐费时、过程不易控制的状况,利用离子阱气相色谱质谱联用仪,建立了非衍生化-气相色谱串级质谱直接分析饲料中三聚氰胺的方法.利用三聚氰胺二级质谱进行定性,以二级质谱的特征离子峰m/z85进行定量,检测效率大大提高,定性更加直接.方法精密度为5.9%,回收率为87%-98%,满足饲料中三聚氰胺的检测要求.     

离子色谱法测定机电塑料产品中卤素

对于机电塑料产品,经液氮粉碎,采用氧仓燃烧离子色谱方法进行定量分析测定,外标法定量。研究了样品前处理条件、离子色谱测定条件以及回收率试验,精密度试验,方法验证试验进行了研究。结果表明,本标准方法科学合理、技术先进,既便于实验室检测,又完全满足国内外用户对检测限量的需要。该检测方法中涉及的卤素种类（氟、氯、溴、碘）已覆盖了国际上相关的电子电气产品法规要求。     

药用溴化丁基橡胶塞中溴离子的提取研究

目的:分析药用溴化丁基胶塞中溴离子的可提取浓度。方法:分别采用纯水、65%乙醇、异丙醇作为提取溶剂,在两种前处理方法下对三个厂家的溴化丁基橡胶塞进行提取,开发离子色谱法对提取液进行溴离子含量的检测。结果:采用不同的提取参数对溴化胶塞进行提取试验,提取效率为:异丙醇65%乙醇水,剪碎浸泡倒置处理,包材接触面积越大提取量越大。开发出的离子色谱法各项方法学性能良好。结论:溴离子的提取量与提取溶剂、前处理方法、胶塞厂家、是否覆膜等因素密切相关,该离子色谱法可用于检测提取液中的溴离子含量。     

猪肉中二溴磷残留量的气相色谱和气相色谱/质谱分析

试样经盐酸酸化,用正己烷提取残留的二溴磷。提取液在-20℃冷冻2小时凝固析出脂肪,净化液经浓缩定容后,用配有电子俘获检测器的气相色谱测定(GC-ECD),外标定量,并用气相色谱—质谱(选择离子监测)(GC/MS(SIM))进行确证。以HP-5大口径毛细管柱和HP-5MS毛细管柱为分离柱,选择出合适的色谱条件,二溴磷的分离效果良好。本方法对猪肉样品的测定低限为0.05mg/kg;添加浓度为0.05mg/kg～1.00mg/kg时,回收率为89％以上;相对标准偏差小于5.0％;标准进样量在0.1～10.0ng范围内,线性关系良好,r=0.9995。样品前处理采用了微量化学法(MiccM)技术,质谱(选择离子监测)确证的监测离子选m/z 301、185、109amu。     

爆炸残留物的现场提取及检验

本文综述了爆炸案件中残留物的现场分布、尘土的收取以及检测方法。传统的检测方法有化学点滴分析、离子选择电极法、薄层色谱法、气相色谱法、色谱-质谱联用分析法等,在传统方法基础上研究了二维气相色谱法、拉曼光谱技术、毛细管离子色谱法在爆炸残留物检测中的应用,为今后的研究提供了方向。     

超声萃取-气相色谱质谱法测定环境和食品中多溴联苯及多溴联苯醚

建立了同时测定环境和食品中10种多溴联苯(PBBs)和多溴联苯醚(PBDEs)的超声萃取-气相色谱质谱方法。在最佳的萃取条件下,该方法的检出限和相对标准偏差s分别为0.97~5.8ng/g和6.3~13.0%,各物质的线性范围达3个数量级,相关系数不低于0.9987。将该方法应用于环境和食品中多溴联苯和多溴联苯醚的分析,均没有检测到目标分析物,各目标分析物的加标回收率为71.5~113.7%,相对标准偏差s)为6.1~13.3%。与索氏提取相比,方法操作简单,快捷,适用于环境和食品中多溴联苯(PBBs)和多溴联苯醚(PBDEs)的测定。     

甘蔗中乐果、特丁磷农药残留的ASE-HPLC-MS/MS-QTRAP定量定性分析方法的建立

本文建立了甘蔗中乐果、特丁磷农药残留的加速溶剂萃取-高效液相色谱串联四级杆线性离子阱质谱（ASE-HPLC-MS/MS-QTRAP）检测方法。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药痕量分析的需要,满足甘蔗中有机磷农药残留检测要求。     

浅析配置EI源三重四极杆气相色谱质谱联用仪校准方法

气相色谱质谱联用仪利用于电厂或磁场中,带电粒子的运动规律,依据质荷比分离物质,从而得到化合物的结构式、元素组成和分子量等信息,其优点是高灵敏度和较强的定性专属性,广泛应用在鉴定农药、兴奋剂、污染物等方面。近几年,由于增加了污染物的种类,提高了检测标准,发展了三重四极杆气相色谱质谱联用仪,其优点是定量定性分析更好、有多种检测离子的方式、更低的定量限和更高的灵敏度。本文主要以配置EI源为例,探究了三重四极杆气相色谱质谱联用仪的校准方法。     

大米中78种农药残留的GC-MS-SIM确证方法研究

建立了大米中78种农药残留的检测方法。研究中采用乙酸乙酯提取样品,提取液经凝胶渗透色谱(GPC)净化、浓缩、定容后用气相色谱-质谱联用仪(GC-MS)的选择离子模式进行定性,内标法定量。该方法回收率为63.4%～124.1%,相对标准偏差为4.43%～27.73%,测定低限为0.004～0.050mg/kg。     

高温燃烧吸收-离子色谱法测定氟醚橡胶中氟溴

采用高温燃烧吸收仪与离子色谱仪联用技术,建立同时测量氟醚橡胶中氟溴含量的方法。优化的实验条件为:燃烧炉燃烧管进口温度为850℃,出口温度为1 000℃,称样量为10 mg,以0.05 mol/L氢氧化钠为吸收液,0.02 mol/L氢氧化钾为淋洗液,采用抑制型电导检测器。氟离子在1～100 mg/L范围内与其色谱峰面积呈良好的线性关系,线性相关系数r~2=0.999 3,检出限为0.04%,回收率为93.0%～104.1%。溴离子在0.1～10 mg/L范围内与其色谱峰面积呈良好的线性关系,线性相关系数r~2=0.999 6,检出限为0.005%,回收率为94.0%～104.0%。与传统氧瓶燃烧、氧弹燃烧-离子色谱法相比,该方法方便、快捷,可连续处理样品,在30 min之内即可完成样品的检测。     

ICP-MS离子提取模型的建立与传输透镜的参数优化

电感耦合等离子体质谱(ICP-MS)具有对一种或多种基本元素、同位素快速分析的能力,在诸多领域有其广泛应用。本文对ICP-MS接口部分中等离子体气流及离子的运动过程进行了理论分析,基于Child鞘层定律首次建立了正离子提取模型,以确定离子束形成的初始位置。然后在忽略空间电荷效应的前提下,利用电、离子光学模拟软件SIMION计算离子在透镜传输系统中的运动轨迹,通过调整透镜电极电压参数来获取最佳的离子传输效率,并以此作为分析实验前透镜调谐工作的理论依据。     

Speciation and identification of organoselenium metabolites in human urine using inductively coupled plasma mass spectrometry and tandem mass spectrometry

A method for speciation and identification of organoselenium metabolites found in human urine samples using high performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC/ICP-MS) and tandem mass spectrometry (MS/MS) is described. Reversed-phase chromatographic separation was used for sample fractionation with the ICP-MS functioning as an element-selective detector, and six distinct selenium-containing species were detected in a human urine sample. Fractions were then collected and analyzed using a triple quadrupole mass spectrometer with electrospray ionization and collision-induced dissociation to obtain structural information. The first two fractions were identified specifically as selenomethionine and selenocystamine, estimated to be present at approximately 11 and 40 ppb, respectively. To the best of our knowledge, this is the first time these two metabolites have been positively identified in human urine.     

甲醇中8组分苯系物溶液标准物质的研制

介绍甲醇中8组分苯系物溶液标准物质的研制过程。采用气相色谱仪(GC-FID)、电感耦合等离子体质谱仪(ICP-MS)和卡尔·费休水分仪(KF)等检测方法,结合质量平衡法对原料纯度进行验证,其纯度验证结果与证书标示值一致,并在不确定度范围内。经F检验和t检验,结果表明,采用重量-容量法制备的甲醇中8组分苯系物溶液标准物质具有良好的均匀性和稳定性,其定值结果为1000μg/mL,相对扩展不确定度为3%(k=2)。该溶液标准物质可用于环境分析中苯系物含量的测定和量值溯源。     

HPLC-ICP-MS法测定水样中的甲基汞、乙基汞和无机汞

建立了高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用测定环境水样中的甲基汞、乙基汞和无机汞的方法。实验使用的高效液相色谱流动相为含有0.06mol/L乙酸氨,20μg/LBi,0.1%(V/V)2-巯基乙醇的5%(V/V)甲醇-水溶液,色谱柱为C18反相柱(5μm,2.1mm×50mm),经前处理的水样在液相色谱中分离后,进入电感耦合等离子体质谱检测其甲基汞、乙基汞和无机汞的浓度。甲基汞、乙基汞和无机汞检出限分别为0.05μg/L、0.10μg/L和0.10μg/L。     

Proteomic analysis with integrated multiple dimensional liquid chromatography/mass spectrometry based on elution of ion exchange column using pH steps

A novel integrated multidimensional liquid chromatography (IMDL) method is demonstrated for the separation of peptide mixtures by two-dimensional HPLC coupled with ion trap mass spectrometry. The method uses an integrated column, containing both strong cation exchange and reversed-phase sections for two-dimensional liquid chromatography. The peptide mixture was fractionated by a pH step using a series of pH buffers, followed by reversed-phase chromatography. Since no salt was used during separation, the integrated multidimensional liquid chromatography can be directly connected to mass spectrometry for peptide analysis. The pH buffers were injected from an autosampler, and the entire process can be carried out on a one-dimensional liquid chromatography system. In a single analysis, the IMDL system, coupled with linear ion trap mass spectrometry, identified more than 2000 proteins in mouse liver. The peptides were eluted according to their pI distribution. The resolution of the pH fractionation is approximately 0.5 pH unit. The method has low overlapping across pH fractions, good resolution of peptide mixture, and good correlation of peptide pIs with pH steps. This method provides a technique for large-scale protein identification using existing one-dimensional HPLC systems.     

水中汞的电感耦合等离子体-质谱法测定

为解决水中汞不稳定以及易吸附而引起记忆效应的问题,建立分析水中汞的电感耦合等离子体质谱新方法,汞标准溶液中加金形成金汞齐,采用200μg/LAu2＋-5%HNO3溶液作为清洗液,选取Rh103作为内标元素。结果标明：在79d内,汞溶液的标准曲线稳定,其相关系数在0.9993~0.9998之间,仪器检出限在1.15×10-3~3.11×10-2μg/L范围内。该方法分析水中痕量汞具有检出限低、数据准确性高、再现性好的特点,所用试剂种类少且毒性小。     

HPLC/ICP-MS in combination with "reverse" online isotope dilution in drug metabolism studies

During the development of a new drug compound, its metabolism needs to be unraveled. For quantification of the metabolites formed, the drug under investigation is traditionally synthesized with a radiolabel ((14)C or (3)H) and the metabolites present in different matrixes (blood, urine, feces) upon drug administration are determined by means of high-performance liquid chromatography (HPLC) coupled to radiodetection. This approach allows for quantification of the metabolites formed and enables a straightforward distinction between exogenous (i.e., drug-related) and endogenous species (as only the radiolabeled species are detected). However, in some cases, the use of a radiolabeled compound in human in vivo studies is not advisible, e.g., for drug compounds or their metabolites showing a long plasma or tissue half-life. In cases where the candidate drug molecule contains an element detectable by means of inductively coupled plasma mass spectrometry (ICP-MS), HPLC/ICP-MS is a promising alternative approach. However, the method lacks specificity when a distinction between drug-related species and endogenous compounds containing the same target element needs to be accomplished. As a result, we have developed an HPLC/ICP-MS-based method combined with "reverse" online isotope dilution ("reverse" online ID) for metabolite quantification. The methodology was evaluated by the analysis of feces samples from rats dosed with a (81)Br-labeled drug compound. The method allows for both (i) valid quantification of the drug metabolites and (ii) distinction among endogenous, exogenous, and "mixed" species, based on their isotopic "fingerprint". A good repeatability (relative standard deviation of 4.2%) and limit of detection (0.35 mg of drug compound L(-1) of feces extract), of the same order of magnitude as those observed for "normal" online ID HPLC/ICP-MS and HPLC/radiodetection, were achieved.     

PET膜中26种化学元素向酸性食品模拟物的迁移

目的 研究4种印刷不同油墨的PET薄膜在酸性条件下26种化学元素的迁移行为。方法 采用电感耦合等离子体发射光谱（ICP-OES）,测定铅、镉、铬等26种化学元素在PET薄膜中的初始含量;采用电感耦合等离子体质谱（ICP-MS）测定这26种化学元素向食品模拟物（体积分数为3%的乙酸）的迁移量。结果 铅、镉、铬等26种元素的迁移量随着温度和时间的增加而增大,并且均能达到各自的迁移平衡。ICP-OES方法的加标回收率为80.2%~109.7%,其相对标准偏差（RSD）为0.3%~12.9%;ICP-MS方法的加标回收率为83.1%~118.6%,其相对标准偏差为0.7%~14.8%。结论 26种化学元素向体积分数为3%乙酸的最大迁移量均低于标准限量值。     

Inductively coupled plasma-mass spectrometry (ICP-MS) for quantitative analysis in environmental and life sciences: a review of challenges, solutions, and trends

This focal point review provides an overview of recent developments and capabilities of inductively coupled plasma mass spectrometry (ICP-MS) coupled with different separation techniques for applications in the fields of quantitative environmental and bio-analysis. Over the past years numerous technical improvements, which are highlighted in this review, have helped to promote the evolution of ICP-MS to one of the most versatile tools for elemental quantification. In particular, the benefits and possibilities of using state-of-the-art hyphenated ICP-MS approaches for quantitative analysis are demonstrated with a focus on environmental and bio-analytical applications.     

燃烧氧化偶联离子色谱法检测甲醇中有机氯

本文提出采用燃烧氧化偶联离子色谱法测定甲醇中有机氯含量的新方法。方法先用离子色谱法直接定量甲醇中无机氯含量,再用离子色谱法测量甲醇中所含的总氯在燃烧氧化过程生成的Cl_2、HCl、气态的无机氯化合物被I吸收生成的Cl~-来定量甲醇中总氯含量。由测得的总氯含量和无机氯含量,计算得甲醇中有机氯含量。实验结果表明该方法经济、简单、准确、灵敏。