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气相色谱离子阱质谱联用仪(GC-ITMS)广泛地应用于药物分析、环境分析、农药检测和食品分析、有机化学品分析、毒品分析以及医学和生物分析等领域。离子阱质谱作为色谱的检测器,决定了色质联用仪的分析性能,包括检出限、分辨率。离子阱质量分析器从传统的双曲型3D离子阱发展到2D线性离子阱,质量歧视效应得到了极大的改善,灵敏度得到了提高。矩形离子阱作为线性离子阱,结构简单,加工和装配容易,因此应用到GCMS系统中将具有非常大的优势。介绍了矩形离子阱质谱仪的设计方案、仪器整机的性能测试、质量分辨和质量歧视效应分析,与Agilent6890组成GCMS联用仪,对实际样品进行了分析。 相似文献
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建立了乳液、霜、水以及油类化妆品中25种邻苯二甲酸酯类化合物的气相色谱-质谱和液相色谱-质谱测定方法。不同基质样品经不同方法净化处理后,采用气相色谱-质谱或液相色谱-质谱进行测定。气相色谱-质谱法采用DB-5MS毛细管色谱柱(30 m,250 mm×0.25μm),程序升温,选择离子模式同时测定21种邻苯二甲酸酯类化合物。液相色谱-质谱采用MN EC-C18色谱柱(4.6×100 mm,2.7μm),以甲醇和0.1%甲酸为流动相,梯度洗脱,流速0.7 mL/min,采用电喷雾电离(ESI+),多反应监测(MRM)模式同时测定24种邻苯二甲酸酯类化合物。25种邻苯二甲酸酯类化合物的线性关系良好,相关系数均大于0.999,回收率实验结果为89.3%~105.6%,RSD为0.4%~4.0%,检出限均小于0.3 mg/kg。方法适用于化妆品中邻苯二甲酸酯类化合物的全面筛查。 相似文献
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气相色谱/离子阱质谱-选择离子方法同时检测大米中百种农药残留 总被引:16,自引:2,他引:16
建立了一种以气相色谱/离子阱质谱(GC/MS),选择离子技术为基础的多种农药同时检测方法。净化采用凝胶渗透色谱(GPC)和F lorisil小柱。通过GC/MS/SIM技术对农药进行检测,在对色谱条件,扫描离子进行优化后,前处理余留下的杂质通过检测的方法得到了进一步的去除,实现了一次进样同时对107种农药进行分析。方法准确灵敏,对于大部分农药回收率保持在70%~110%;相对标准偏差小于20%;检出限保持在0.01~0.2 mg/kg之间(信噪比3)。 相似文献
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固相萃取/离子阱气相色谱质谱联用对血液中多种安眠药物的同时测定 总被引:4,自引:1,他引:3
建立了气相色谱-质谱联用测定血液中多种安眠药物的分析方法,通过固相萃取提取并富集血液样品中的9种常见巴比妥类、吩噻嗪类和苯二氮杂类安眠药物,采用离子阱二级质谱检测其含量。通过优化萃取溶液pH值及气相色谱-质谱联用分析条件,对9种安眠药物进行了定量分析。采用离子阱串联质谱(MS/MS)技术消除基底干扰,给出被测物结构信息。9种安眠药物的检出限为0.04~0.10 mg/L,回收率为78%~93%。方法用于人心血中安眠药物的检测,检出安定0.6 mg/L。该方法高效、简单、灵敏度高,可用于血液中巴比妥类、吩噻嗪类和苯二氮杂类安眠药物的同时测定。 相似文献
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气相色谱-离子阱质谱法测定蔬菜中9种有机磷农药的残留量 总被引:1,自引:0,他引:1
建立气相色谱-离子阱质谱法测定蔬菜中9种有机磷农药残留的方法.样品经乙酸乙酯提取、无水硫酸钠脱水、活性炭小柱净化,浓缩后通过气相色谱-离子阱质谱进行测定.9种有机磷农药的浓度在0.05~1.0μg/mL范围内与其对应的色谱峰面积具有良好的线性关系(r>0.999).在3个不同添加浓度下的平均回收率为76.5%~101.2%,测定结果的相对标准偏差为3.9%~9.4%(n=7).该方法快速、准确、操作简便,能满足蔬菜中有机磷农药残留的检测要求. 相似文献
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建立了凝胶渗透色谱(GPC)-气相色谱-离子阱质谱同时检测桔梗原药和当归提取物中101种农药残留的分析方法。方法采用乙腈超声辅助提取桔梗原药和当归提取物,浓缩提取液至近干后用乙酸乙酯-环己烷(1∶1, v/v)复溶,采用凝胶渗透色谱法(选取40 cm长、内径20 mm的凝胶渗透色谱柱)对样品进行净化,弃去前段含脂类、色素等杂质的流出液,收集17~30 min洗脱液并旋转蒸发浓缩至近干,甲苯1 mL定容上机。选用DB-5MS毛细管色谱柱分离待测物,通过离子阱质谱实现对101种农药残留的高效检测。方法通过优化前处理条件和离子阱二级质谱参数,有效降低了复杂中药基质对待测化合物的干扰,最大限度提高了样品中农药的定量准确性和回收率,101种农药3水平添加的平均回收率为58.3%~108.9%,每个添加水平10次独立重复测定的相对标准偏差为0.4%~16.5%,检出限(LOD)范围为0.2~40.0 μg/kg,可满足当前韩国、日本、欧洲规定的最大残留限量(maximum residue limits, MRLs)要求。方法具有操作简单快速、灵敏度高、重复性好等特点,凝胶渗透色谱技术的应用克服了固相萃取小柱净化容量不足的弊端,离子阱技术的应用可以进一步排除共流出基体杂质的干扰,提高定量和定性的准确性,检测效果优于常用的气相色谱-质谱法,是对中药中同时分析多种农药残留检测方法的有益补充。 相似文献
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研制了一种用于综合录井技术的在线快速气相色谱-四极杆质谱联用仪。采用隔膜泵直接抽取泥浆中脱出的气体样品直接引入气相色谱,通过气驱十通阀实现自动进样;快速分离后,样品中各组分依次进入四极杆质谱进行检测;四极杆质谱采用电子轰击源电离及选择离子扫描的方式,提供对碳氢化合物检测所需要的高灵敏度;仪器通过精确的时序控制实现周期循环进样分析,满足录井现场的实时监测需求。仪器采用安全易得的氮气作载气,对C1-C8烷烃、苯、甲苯、环己烷和甲基环己烷等油气组分进行快速在线分析,结果表明,C1-C5分析周期小于30 s,C1-C8周期小于85 s,最低检测浓度为0.0001%(V/V),线性范围高于5个数量级,适合于录井技术中油气组分分析。 相似文献
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《Analytical letters》2012,45(19-20):1963-1971
Abstract FAB-MS/MS methods are used to quantify the neuropeptide leucine enkephalin (LE = YGGFL) in synthetic solutions. Maximum molecular specificity is provided by monitoring two metastable transitions from the LE (M + H)+, 556 → 425 and 556 → 336, in a forward geometry (E, B) mass spectrometer using a B/E linked-field selected reaction monitoring technique. Obtained sensitivity is 40 pg LE, which equals 72 fmol. The statistics of the best-fit straight lines are, for m/z 425: y = 34 + 166 (r = 0.999), and for m/z 336: y = 2.5x + 17.2 (r = 0.996). 相似文献
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同位素质谱与无机质谱分析 总被引:1,自引:0,他引:1
本文是《分析试验室》定期评述中“无机质谱分析”课题的第二篇评述文章,它增加了同位素质谱分析的内容,故将题目改为现今题目,它综述了1985年~1990年间同位素质谱和无机质谱的发展概况。其中包括同位素示踪、同位素稀释、火花源质谱、二次离子质谱、等离子体质谱等。内容以国内为主,也收集了少量代表学科先进水平的外国文献。 相似文献
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Domingues MR Domingues P Reis A Ferrer-Correia AJ Tomé JP Tomé AC Neves MG Cavaleiro JA 《Journal of mass spectrometry : JMS》2004,39(2):158-167
Porphyrin derivatives having a galactose or a bis(isopropylidene)galactose structural unit, linked by ester or ether bonds, were characterized by electrospray tandem mass spectrometry (ES-MS/MS). The electrospray mass spectra of these glycoporphyrins show the corresponding [M + H](+) ions. For the glycoporphyrins with pyridyl substituents and those having a tetrafluorophenyl spacer, the doubly charged ions [M + 2H](2+) were also observed in ES-MS with high relative abundance. The fragmentation of both [M + H](+) and [M + 2H](2+) ions exhibited common fragmentation pathways for porphyrins with the same sugar residue, independently of the porphyrin structural unit and type of linkage. ES-MS/MS of the [M + H](+) ions of the galactose-substituted porphyrins gave the fragment ions [M + H - C(2)H(4)O(2)](+), [M + H - C(3)H(6)O(3)](+), [M + H - C(4)H(8)O(4)](+) and [M + H - galactose residue](+). The fragmentation of the [M + 2H](2+) ions of the porphyrins with galactose shows the common doubly charged fragment ions [porphyrin + H](2+), [M + 2H - C(2)H(4)O(2)](2+), [M + 2H - C(4)H(8)O(4)](2+), [M + 2H - galactose residue](2+) and the singly charged fragment ions [M + H - C(3)H(6)O(3)](+) and [M + H - galactose residue](+). The fragmentation of the [M + H](+) ions of glycoporphyrins with a protected galactosyl residue leads mainly to the ions [M + H - CO(CH(3))(2)](+), [M + H - 2CO(CH(3))(2)](+), [M + H - 2CO(CH(3))(2) - CO](+), [M + H - C(10)H(16)O(4)](+) and [M + H - protected galactose](+). The doubly charged ions [M + 2H](2+) fragment to give the doubly charged ions [porphyrin + H](2+) and the singly charged ions [M + H - protected galactose residue](+) and [M + H - CO(CH(3))(2)](+). For the porphyrins where the sugar structural unit is linked by an ester bond, [M + 2H](2+), ES-MS/MS showed a major and typical fragmentation corresponding to combined loss of a sugar structural unit and further loss of water, leading to the ion [M + 2H - sugar residue - H(2)O](2+), independently of the structure of the sugar structural unit. These results show that ES-MS/MS can be a powerful tool for the characterization of the sugar structural unit of glycoporphyrins, without the need for chemical hydrolysis. 相似文献
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Williams JP Nibbering NM Green BN Patel VJ Scrivens JH 《Journal of mass spectrometry : JMS》2006,41(10):1277-1286
The rapid desorption electrospray ionisation (DESI) of some small molecules and their fragmentation using a triple-quadrupole and a hybrid quadrupole time-of-flight mass spectrometer (Q-ToF) have been investigated. Various scanning modes have been employed using the triple-quadrupole instrument to elucidate fragmentation pathways for the product ions observed in the collision-induced dissociation (CID) spectra. Together with accurate mass tandem mass spectrometry (MS/MS) measurements performed on the hybrid Q-ToF mass spectrometer, unequivocal product ion identification and fragmentation pathways were determined for deprotonated metoclopramide and protonated aspirin, caffeine and nicotine. Ion structures and fragmentation pathway mechanisms have been proposed and compared with previously published data. The necessity for elevated resolution for the differentiation of isobaric ions are discussed. 相似文献
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Rai DK Green BN Landin B Alvelius G Griffiths WJ 《Journal of mass spectrometry : JMS》2004,39(3):289-294
Within a mixture of proteins, minor polymorphic components are difficult to identify using a conventional proteomic approach. Their identification generally requires multi-dimensional separation steps, before or after proteolytic cleavage, followed by sequence analysis of the proteolytic products. In this study, we investigated the potential of tandem mass spectrometry for protein characterization by identifying the delta-beta hybrid human hemoglobin variant Lepore-Boston-Washington using electrospray ionization tandem mass spectrometry. Hemoglobin Lepore-Boston-Washington occurs mainly in heterozygotes, where it comprises approximately 10% of the total non-alpha-chains, the dominant non-alpha-chain being the normal beta (approximately 90%). Furthermore, Hemoglobin Lepore-Boston-Washington has an average molecular mass (15,865.23 Da) that is only 2 Da lower than that of the normal beta-chain (15,867.24 Da). Consequently, it cannot be resolved from the normal beta-chain by mass spectrometry. Here we show how Hemoglobin Lepore-Boston-Washington was identified directly from the diluted blood of a heterozygote by analyzing the product ions from the Lepore-Boston-Washington and normal beta-chain ions without prior separation of the individual chains. This study shows the potential of the tandem mass spectrometry for identifying a minor component in an unseparated mixture of proteins. 相似文献
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将数字化离子阱技术和矩形离子阱(RIT)技术相结合,建立了数字化矩形离子阱质谱仪.此技术和装置既具有数字化电源的结构简单、输出稳定和易精确控制等特点,又结合了矩形离子阱的高离子存储效率、结构简单以及加工和装配容易等优点.构建了基于电喷雾(ESI)电离源的数字化矩形离子阱质谱仪系统,并使用Fenfluramine和PPG2000分别对此系统的质量分辨率和质量范围进行了测试.研究结果表明:一个用印刷线路板(PCB)制作的简单矩形离子阱,在200 V(半峰值)的数字束缚电压的驱动下,获得了大于500的质量分辨率和超过2600 Th的质量范围.实验证明,数字化离子阱技术的应用可以显著提高矩形离子阱的性能,特别是质量范围等关键的质谱仪指标. 相似文献
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M. Ubieto-Díaz D. Rodríguez S. Lukic Sz. Nagy S. Stahl K. Blaum 《International journal of mass spectrometry》2009,288(1-3):1-5
The KArlsruhe TRItium Neutrino experiment KATRIN aims at improving the upper limit of the mass of the electron antineutrino to about 0.2 eV (90% c.l.) by investigating the -decay of tritium gas molecules . The experiment is currently under construction to start first data taking in 2012. One source of systematic uncertainties in the KATRIN experiment is the formation of ion clusters when tritium decays and decay products interact with residual tritium molecules. It is essential to monitor the abundances of these clusters since they have different final state energies than tritium ions. For this purpose, a prototype of a cylindrical Penning trap has been constructed and tested at the Max-Planck-Institute for Nuclear Physics in Heidelberg, which will be installed in the KATRIN beam line. This system employs the technique of Fourier-Transform Ion-Cyclotron-Resonance in order to measure the abundances of the different stored ion species. 相似文献
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该文总结了二次离子质谱、基质辅助激光解吸电离质谱和常压敞开式离子化质谱三大类型质谱分子成像(MSI)技术的概况、技术与方法及其应用新进展。MSI技术作为免标记、高覆盖、高灵敏、检测范围广的可视化分析手段,不局限于生物组织或细胞中某种特定分子的检测,可对已知和未知多种分子进行同时成像分析,获得不同分子的空间分布、相对含量及结构信息,实现其分子的定性、定量与定位分析;还可提供不同生理及病理过程中功能分子的动态时空变化信息等。因此,MSI技术成为质谱领域以及分析化学等领域的研究前沿与热点方向之一,并在化学、医学、生命科学、药学和环境科学等领域显示出重大应用前景。此外,MSI技术是单细胞可视化分析和空间分辨代谢组学的强有力分析手段,可从动物或器官组织的整体、微区、单细胞等不同空间尺度,获取具有空间分布特征、时空动态变化的功能分子全景轮廓信息等而备受关注。 相似文献