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苏宇亮 《理化检验(化学分册)》2009,45(5)
对高效液相色谱-电感耦合等离子体质谱联用技术在水质分析中的应用作了评述,对高效液相色谱-电感耦合等离子体质谱联用技术的发展前景作了展望.引用文献48篇. 相似文献
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利用外部触发装置实现了毛细液相和超高效液相与静电场轨道阱高分辨质谱(LTQ-Orbitrap XL)的交互联用,建立了全方位的液相色谱-质谱联用分析以及液相色谱多级串联质谱联用分析平台.通过平台的应用大大提高了大型仪器的使用效率,促进了公共仪器平台的科研服务能力. 相似文献
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质谱联用技术在生物大分子分析中的应用 总被引:1,自引:0,他引:1
本文评述了近年来质谱联用技术在生物大分子分析应用中的最新进展。着重评述了由于ESI接口的出现而推动的高效液相色谱一连续流动快速原子轰击质谱(HPLC-cfFABMS )、高效取代色谱一连续流动快速原子轰击质谱(HPDC-cfFABMS ) ,凝胶渗透色谱一诱导祸合等离子体质谱(GPC-1CPMS )、毛细管电泳一质谱(CE-MS )和毛细管电泳一飞行时间质谱(CE-TOFMS)等方面近两年的动向及成果。本文较广泛地展示了质谱联用技术在生物大分子分析中的重要作用和独特的地位。 相似文献
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枸杞组分特征检测及产地溯源技术研究进展 总被引:1,自引:0,他引:1
特色农产品的特征组分检测和溯源技术是政府职能部门进行市场监管和地理标志产品保护的重要手段。该文介绍了色谱技术(高效液相色谱及凝胶渗透色谱)、质谱及其联用技术(气相色谱-质谱联用技术及液相色谱-质谱联用技术)、红外光谱技术(傅立叶变换红外光谱及近红外光谱)、电感耦合等离子体原子发射光谱技术和电感耦合等离子体质谱技术在枸杞有机化学成分和矿质元素检测中的应用以及枸杞溯源技术的研究进展,并简要概述了其中应用较多的化学计量学方法。旨在为不同产地枸杞的质量控制和来源追溯提供参考,进而推动我国枸杞消费市场的良性发展。 相似文献
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Jean-Claude Alvarez Isabelle Etting Islam Amine Larabi 《Biomedical chromatography : BMC》2022,36(8):e5391
An LC-MS/MS method for hair testing of glyphosate and aminomethylphosphonic acid (AMPA), its main biodegradation product, has been developed. After decontamination, 50 mg of hair was ground and sonicated in water for 2 h. The method was fully validated in the 5–500 pg/mg range for glyphosate and 10–500 pg/mg for AMPA, and the limits of detection were 2 and 5 pg/mg, respectively. Matrix effect for glyphosate and AMPA was compensated by an isotope-labeled internal standard. Hair samples from four farmers who regularly used glyphosate and one farmer who used glyphosate but not his wife and 14 hair samples from nonoccupationally exposed subjects were tested. Glyphosate was found in head hair of three farmers, with concentration in the range 14–188 pg/mg. The fourth was found negative but with hair colored in red. Glyphosate was detected in 10 of 14 hair samples from nonoccupationally exposed subjects at concentrations of 11.5 pg/mg or lower and only in one segment (0–3 cm) of the farmer's spouse (6 pg/mg). AMPA was detected in five subjects, above the limit of quantification only in two of three occupationally exposed subjects with positive glyphosate. Further studies should be conducted to validate this potential new biomarker that could be useful for assessing long-term exposure to glyphosate. 相似文献
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液相色谱-串联质谱法检测贝类产品中的原多甲藻酸贝类毒素 总被引:4,自引:0,他引:4
建立了一种贝类组织中原多甲藻酸(azaspiracid, AZA)贝类毒素主要成分AZA1的高效液相色谱-串联质谱检测方法。本方法采用甲醇-水(80:20, v/v)溶液对贝类组织中AZA1进行提取,并用MAX阴离子交换固相萃取(SPE)柱富集净化,使用Atlantis dC18(150 mm×4.6 mm, 5.0 μm)色谱柱分离,以含有50 mmol/L甲酸和2 mmol/L甲酸铵的乙腈-水溶液(80:20, v/v)为流动相进行等度洗脱,质谱采用选择反应监测(SRM)模式。AZA1在5 min内获得完全分离,且在48.85~2 442 ng/L范围内线性良好,相关系数为0.998 1。该方法检出限(S/N=3)为11.00 pg/g,添加水平为36.64、73.27、146.54 pg/g时的平均回收率为75.8%~82.5%(n=6),相对标准偏差小于10%。利用该方法对采自大连、青岛、广州水产品市场上的112个贝类样品进行了分析,发现采自大连和广州的部分贝类样品中含有AZA1。结果表明,该方法具有简单、快速、灵敏度高等特点,能充分满足贝类中AZA1检测的要求。 相似文献
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Ciminiello P Dell'Aversano C Fattoruss E Forino M Magno S Poletti R 《Journal of chromatography. A》2002,968(1-2):61-69
A liquid chromatography mass spectrometry (LC-MS) method is proposed for the sensitive, specific and direct detection of yessotoxin and its analogues, marine biotoxins which are associated with diarrhetic shellfish poisoning (DSP) and which have been found in the North Adriatic sea since 1995. The LC-MS method provided a detection limit of 70 pg for yessotoxin in full scan mode and was applied to determine the toxic profiles of a number of extracts or partially purified fractions of toxic mussels collected along the Emilia Romagna coasts (Italy) in the period 1995-1999. Detection of a desulfo-yessotoxin derivative from Mytilus galloprovincialis collected in 1998 is also reported. 相似文献
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Determination of scutellarin in Erigeron breviscapus extract by liquid chromatography-tandem mass spectrometry. 总被引:2,自引:0,他引:2
A quantitative assay for scutellarin by LC-MS-MS (negative ion mode) was developed. The scutellarin was extracted from dry Erigeron breviscapus. Significant ion suppression was observed, which could be eliminated by increasing the turboionspray interface temperature to 350 degrees C and by 1000-fold dilution of the extract with solvent. The calibration curve of scutellarin showed excellent linearity over a wide concentration range (0.01-100 microg/ml) (r=0.998), and the limit of detection was 15 pg/ml using a 10-microl injection volume. The analysis time was 4 min/sample. 相似文献
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M. Francisca Portilha-Cunha Teresa I. A. Gouveia Alicia L. Garcia-Costa Arminda Alves Mnica S. F. Santos 《Molecules (Basel, Switzerland)》2021,26(18)
Cytostatics are toxic pharmaceuticals, whose presence in surfaces puts healthcare workers at risk. These drugs might also end up in hospital effluents (HWW), potentially damaging aquatic ecosystems. Bicalutamide is a cytostatic extensively consumed worldwide, but few analytical methods exist for its quantification and most of them require advanced techniques, such as liquid chromatography mass spectrometry (LC-MS), which are very complex and expensive for large monitoring studies. Therefore, a simple but reliable multi-matrix high performance liquid chromatographic method, with fluorescence detection, was developed and validated to rapidly screen abnormal concentrations of bicalutamide in HWW and relevant contamination levels of bicalutamide in indoor surfaces (>100 pg/cm2), prior to confirmation by LC-MS. The method presents good linearity and relatively low method detection limits (HWW: 0.14 ng/mL; surfaces: 0.28 pg/cm2). Global uncertainty was below 20% for concentrations higher than 25 ng/mL (HWW) and 50 pg/cm2 (surfaces); global uncertainty was little affected by the matrix. Therefore, a multi-matrix assessment could be achieved with this method, thus contributing to a holistic quantification of bicalutamide along the cytostatic circuit. Bicalutamide was not detected in any of the grab samples from a Portuguese hospital, but an enlarged sampling is required to conclude about its occurrence and exposure risks. 相似文献
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In this work, an electrochemiluminescence (ECL) immunosensor for ultrasensitive detection of α-fetoprotein (AFP) was fabricated using Ru(bpy)(3)(2+)-encapsulated liposome as the label and electrodeposited gold nanoparticles (GNPs) as the immobilizing support. Great signal amplification was achieved since liposome could encapsulate large amount of reporter molecules and GNPs could provide large active surface. Under optimized conditions, with sandwich type format, a linear range of AFP from 0.005 to 0.2 pg/mL and an extremely low detection limit of 0.001 pg/mL was obtained, much lower than that in previous reports. The proposed ECL immnuosensor showed high sensitivity, specificity, and good stability, which may open a new door to ultrasensitive detection of proteins in clinical analysis. 相似文献
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Liquid chromatography--multiple tandem mass spectrometry for the determination of ten azaspiracids, including hydroxyl analogues in shellfish 总被引:2,自引:0,他引:2
Lehane M Fidalgo Sáez MJ Magdalena AB Ruppén Cañás I Díaz Sierra M Hamilton B Furey A James KJ 《Journal of chromatography. A》2004,1024(1-2):63-70
Azaspiracids (AZAs) are a group of polyether toxins that cause food poisoning in humans. These toxins, produced by marine dinoflagellates, accumulate in filter-feeding shellfish, especially mussels. Sensitive liquid chromatography-electrospray ionisation mass spectrometry (LC-ESI-MS(n)) methods have been developed for the determination of the major AZAs and their hydroxyl analogues. These methods, utilising both chromatographic and mass resolution, were applied for the determination of 10 AZAs in mussels (Mytilus edulis). An optimised isocratic reversed phase method (3 microm Luna-2 C18 column) separated 10 azaspiracids using acetonitrile/water (46:54, v/v) containing 0.05% trifluoroacetic acid (TFA) and 0.004% ammonium acetate in 55 min. Analyte determination using MS3 involved trapping and fragmentation of the [M + H]+ and [M + H - H2O]+ ions with detection of the [M + H - 2H2O]+ ion for each AZA. Linear calibrations were obtained for AZA1, using spiked shellfish extracts, in the range 0.05-1.00 microg/ml (r2 = 0.997) with a detection limit of 5 pg (signal : noise = 3). The major fragmentation pathways in hydroxylated azaspiracids were elucidated using hydrogen/deuterium (H/D) exchange experiments. An LC-MS3 method was developed using unique parent ions and product ions, [M + H - H2O - CgH10O2R1R3]+, that involved fragmentation of the A-ring. This facilitated the discrimination between 10 azapiracids, AZA1-10. Thus, this rapid LC-MS3 method did not require complete chromatographic resolution and the run-time of 7 min had detection limits better than 20 pg for each toxin. 相似文献
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Manuel A. A. Mertens Hans-Gerd M. Janssen Carel A. Cramers Wim J. L. Genuit Ger J. van Velzen Henk Dirkzwager Herman van Binsbergen 《Journal of separation science》1996,19(1):17-22
An interface for coupling supercritical fluid chromatography to a magnetic sector mass spectrometer was developed and evaluated. The interface is based on direct introduction of the mobile phase, carbon dioxide, into the ion-source of the mass spectrometer. The SFC-MS system was optimized with respect to the signal-to-noise ratio. Under optimized conditions, the estimated detection limit for n-pentadecane is approximately 30 ppm. Spectra obtained in the electron-impact ionization mode show a very good similarity with library spectra. The performance of the SFC-MS system was evaluated by the analysis of a number of test mixtures. A sample containing several low molecular mass, thermally unstable compounds, which could neither be analyzed by GC-MS nor by LC-MS, was analyzed. Also for the analysis of high molecular mass compounds, the coupled system showed a good performance. 相似文献
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Shyang Pei Hong Noor Faizah Mohd-Naim Natasha Ann Keasberry Minhaz Uddin Ahmed 《Electroanalysis》2022,34(4):684-691
A label-free electrochemical immunosensor was developed for the ultra-sensitive detection of β-lactoglobulin (β-LG). The novel nanocomplex of carbon nanochips, colloidal gold nanoparticles and titanium dioxide nanoparticles TiO2/CNC/AuC were constructed on conducting polymer, chitosan, and were characterised using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). This nanocomplex interface was studied using cyclic voltammetry (CV) and showed great improvement at the gold electrode surface with enhanced electrochemical performance, sensitivity and selectivity for β-lactoglobulin. Under optimal parameters, the square wave voltammetry (SWV) response curve was determined from 0.01 pg/mL to 500 pg/mL using [Fe(CN)6]3−/4−] redox probe. The calibration plot illustrates a linear relationship between log β-LG concentration and SWV current, with the limit of detection determined to be 0.01 pg/mL. This immunosensor displayed high sensitivity, selectivity, reproducibility and stability, and can be utilised for the detection of β-LG in real food samples. 相似文献
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An LC-MS method for the determination of picric acid (2,4,6-trinitrophenol), its reductive transformation products picramic acid (2-amino-4,6-dinitrophenol) and iso-picramic acid (4-amino-2,6-dinitrophenol) and hexyl (2,2',4,4',6,6'-hexanitrodiphenylamine) has been developed. The analytes were separated using ion-pairing chromatography with a volatile ion-pairing reagent suitable for subsequent MS detection. The performance of an atmospheric pressure chemical ionisation (APCI) and an electrospray ionisation (ESI) interface was compared. ESI-MS is more sensitive for the analytes, especially for hexyl and picric acid, APCI-MS delivered more fragments necessary for unequivocal identification. With LC-ESI-MS limits of detection using single ion monitoring (SIM) mode are 4 ng (iso-picramic acid), 800 pg (picramic acid), 400 pg (picric acid) and 80 pg (hexyl). For quantification, 15N-picric acid was used as an internal standard. Using this new method, the degradation of picric acid in soil was monitored in a laboratory study. Furthermore, the presence of picramic acid was for the first time verified in soil samples from a former ammunition plant. 相似文献