molecular absorption spectrometry

  • 文章类型: Journal Article
    细菌对抗生素耐药性的持续发展是一个全球性挑战。因此,该领域的研究是必要的。为此目的需要分析技术。从这个角度来看,重点是原子吸收光谱法(AAS)。虽然它很旧,AAS通常提供意想不到的潜力。当然,这应该被利用。因此,目的是证明该技术在抗菌研究中的多功能性。这通过其实际应用的各种示例来说明。可以使用AAS,例如,为了确认抗菌化合物的身份,对于纯度控制,或量化药物制剂中的抗生素。后者允许分析而无需费力的样品制备并且不受其他赋形剂的干扰。此外,AAS可以帮助阐明作用模式或抵抗机制。在这种情况下,量化抗生素药物在(耐药)细菌细胞中的积累似乎起着重要作用。AAS的一般应用不仅限于含金属药物,还能测定一些有机化学抗生素。总之,这种观点提出了AAS在抗菌研究中的一系列应用,旨在提高对该方法的认识,从而可能有助于对抗抵抗。
    The ongoing development of bacterial resistance to antibiotics is a global challenge. Research in that field is thus necessary. Analytical techniques are required for such a purpose. From this perspective, the focus was on atomic absorption spectrometry (AAS). Although it is old, AAS often offers unexpected potential. Of course, this should be exploited. The aim was therefore to demonstrate the versatility of the technique in antibacterial research. This is illustrated by various examples of its practical application. AAS can be used, for example, to confirm the identity of antibacterial compounds, for purity controls, or to quantify the antibiotics in pharmaceutical preparations. The latter allowed analysis without laborious sample preparation and without interference from other excipients. In addition, AAS can help elucidate the mode of action or resistance mechanisms. In this context, quantifying the accumulation of the antibiotic drug in the cell of (resistant) bacteria appears to play an important role. The general application of AAS is not limited to metal-containing drugs, but also enables the determination of some organic chemical antibiotics. Altogether, this perspective presents a range of applications for AAS in antibacterial research, intending to raise awareness of the method and may thus contribute to the fight against resistance.
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  • 文章类型: Journal Article
    氟,取决于它的浓度和化学形式,对人类和动物是必需的或有毒的。因此,能够可靠地确定它是至关重要的。在这项研究中,用HCl(胃液模拟)提取后测定动物饲料中的氟。采用了氟化物选择电极(ISE)的标准电位法和新开发的高分辨率连续源石墨炉分子吸收光谱法(HR-CSGFMAS)。饲料样品被证明是HR-CSGFMAS的挑战。化学干扰(竞争分子的形成,CaF,GaCl,和GaP,而不是目标GaF分子)和光谱效应(包括磷分子光谱和原子线)被鉴定。试剂污染F和记忆效应引起了额外的困难。困难被消除/减少。对ISE分析的质量进行了多方向验证(包括全面的能力测试)。在低F浓度下存在不准确的风险,其中校准关系是非线性的,被调查。两种方法的结果一致,这证实了方法的准确性,并告知提取的氟是氟化物形式。2021-2023年在波兰进行的广泛的ISE测试结果表明,在大多数情况下,氟含量明显低于阈值。
    Fluorine, depending on its concentration and chemical form, is essential or toxic to humans and animals. Therefore, it is crucial to be able to determine it reliably. In this study, fluorine was determined in animal feed after extraction with HCl (gastric juice simulation). The standard potentiometric method with a fluoride-selective electrode (ISE) and newly developed high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GFMAS) method was applied. Feed samples turned out to be a challenge for HR-CS GFMAS. Chemical interferences (formation of competing molecules, CaF, GaCl, and GaP, instead of the target GaF molecule) and spectral effects (including a phosphorous molecule spectrum and atomic lines) were identified. An additional difficulty was caused by reagent contamination with F and memory effects. Difficulties were eliminated/reduced. The quality of ISE analysis was multi-directionally verified (including comprehensive proficiency testing). A risk of inaccuracy at low F concentration, where the calibration relationship is nonlinear, was investigated. The results of both methods were consistent, which confirms the accuracy of the methods and informs that the extracted fluorine is in fluoride form. The results of extensive ISE tests conducted in Poland in 2021-2023 have shown that, in most cases, the fluoride content is significantly lower than the threshold values.
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  • 文章类型: Journal Article
    一个可靠的,快速,讨论了确定水中非常低的六价铬(Cr)浓度的低成本程序。该程序基于Cr6与二苯基碳酰肼的经典反应。一旦这种反应发生,添加十二烷基硫酸钠以获得离子对,和TritonX-114合并。接下来,混合物的加热允许在浊点微萃取(CPE)过程中获得可通过离心分离的两相。凝聚层含有水样中原来存在的所有Cr6+,以便通过分子吸收分光光度法进行测量可以计算金属的浓度。不需要有害的有机溶剂。六价和三价形式的区分通过包括Ce4+的氧化阶段来实现。为了充分利用凝聚过程固有的预浓缩效应,以及尽量减少试剂消耗和废物产生,使用与微体积液体样品兼容的便携式迷你分光光度计。预浓缩因子为415,可以检测到低至0.02µgL-1的铬浓度。该方法显示出良好的再现性(相对标准偏差接近3%)。
    A reliable, rapid, and low-cost procedure for determining very low concentrations of hexavalent chromium (Cr) in water is discussed. The procedure is based in the classical reaction of Cr6+ with diphenylcarbazide. Once this reaction has taken place, sodium dodecylsulfate is added to obtain an ion-pair, and Triton X-114 is incorporated. Next, the heating of the mixture allows two phases that can be separated by centrifugation to be obtained in a cloud point microextraction (CPE) process. The coacervate contains all the Cr6+ originally present in the water sample, so that the measurement by molecular absorption spectrophotometry allows the concentration of the metal to be calculated. No harmful organic solvents are required. The discrimination of hexavalent and trivalent forms is achieved by including an oxidation stage with Ce4+. To take full advantage of the pre-concentration effect inherent to the coacervation process, as well as to minimize reagent consumption and waste generation, a portable mini-spectrophotometer which is compatible with microvolumes of liquid samples is used. The preconcentration factor is 415 and a chromium concentration as low as 0.02 µg L-1 can be detected. The procedure shows a good reproducibility (relative standard deviation close to 3%).
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  • 文章类型: Journal Article
    Chemical oxygen demand (COD) is important for water quality assessment as it represents the level of reductive organic pollution from eutrophication in aquatic systems. For surface water quality monitoring, permanganate is usually applied as an oxidizing reagent, and the routine CODMn determination is mostly achieved by titration method. However, this titration method is tedious and time consuming, and the results suffer from environmental temperature fluctuations and complicated operation techniques. In this study, a novel CODMn determination method was developed using gas-phase molecular absorption spectrometry equipped with an online automated digestion device for the first time. The effects of digestion temperature, digestion time and sulfuric acid content were thoroughly studied. This method exhibited good linearity (0.35 to 12 mg/L), a low detection limit (0.12 mg/L), and good RSD from various water samples (0.71 - 2.37%). When used for CODMn determination in routine water quality monitoring, this automated GPMAS can considerably improve analysis speed, efficiency, accuracy and stability compared to the traditional titration method.
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  • 文章类型: Journal Article
    通过使用基于碳一硫化物(CS)分子蒸发的高分辨率连续源电热分子吸收光谱法测定杏和葡萄样品中的硫。CS在气相中形成,不添加任何分子形成元素,因为石墨比色皿含有大量的碳以及食物样品。在溶液中使用15μgPd+10μgMg的混合物作为化学改性剂。用K2SO4校准溶液在900°C的热解温度下获得最佳灵敏度。校准图绘制了50至1600ng硫之间的线性路径,检测限为23ng。使用标准参考材料(米粉,NISTSRM1568a)。化学干燥的杏样品中的硫含量(1987±45mg/kg)被确定为高于在阳光下干燥的杏样品。
    The determination of sulfur in apricot and grape samples was performed by using high-resolution continuum source electrothermal molecular absorption spectrometry based on vaporization of the carbon monosulfide (CS) molecule. CS forms in the gas phase without the addition of any molecule-forming element, since graphite cuvette contains plenty of carbon as well as food samples. A mixture of 15 μg Pd + 10 μg Mg was used in solution as the chemical modifier. The best sensitivity was obtained at 900°C of the pyrolysis temperature with a K2SO4 calibration solution. The calibration plot drew a linear path between 50 and 1600 ng of sulfur, and the limit of detection was found to be 23 ng. The accuracy of the method was confirmed with the use of a standard reference material (Rice Flour, NIST SRM 1568a). The sulfur content in chemically dried apricot samples (1987 ± 45 mg/kg) was determined to be higher than that of apricot samples dried under sunshine.
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  • 文章类型: Journal Article
    A new method to determine iodine in drug samples by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The method measures the molecular absorption of a diatomic molecule, CaI or SrI (less toxic molecule-forming reagents), at 638.904 or 677.692nm, respectively, and uses a mixture containing 5μg of Pd and 0.5μg of Mg as chemical modifier. The method employs pyrolysis temperatures of 1000 and 800°C and vaporization temperatures of 2300 and 2400°C for CaI and SrI, respectively. The optimized amounts of Ca and Sr as molecule-forming reagents are 100 and 150µg, respectively. On the basis of interference studies, even small chlorine concentrations reduce CaI and SrI absorbance significantly. The developed method was used to analyze different commercial drug samples, namely thyroid hormone pills with three different iodine amounts (15.88, 31.77, and 47.66µg) and one liquid drug with 1% m v-1 active iodine in their compositions. The results agreed with the values informed by the manufacturers (95% confidence level) regardless of whether CaI or SrI was determined. Therefore, the developed method is useful for iodine determination on the basis of CaI or SrI molecular absorption.
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  • 文章类型: Journal Article
    Sulphur was determined in various vegetables via molecular absorption of carbon monosulphide (CS) at 258.056 nm using a solid sampling high resolution continuum source electrothermal atomic absorption spectrometer (SS HR-CS ETAAS). Samples were dried, ground and directly introduced into the ruthenium coated graphite furnace as 0.05 to 0.50mg. All determinations were performed using palladium+citric acid modifier and applying a pyrolysis temperature of 1000 °C and a volatilisation temperature of 2400 °C. The results were in good agreement with certified sulphur concentrations of various vegetal CRM samples applying linear calibration technique prepared from thioacetamide. The limit of detection and characteristic mass of the method were 7.5 and 8.7 ng of S, respectively. The concentrations of S in various spinach, leek, lettuce, radish, Brussels sprouts, zucchini and chard samples were determined. It was showed that distribution of sulphur in CRM and grinded food samples were homogeneous even in micro-scale.
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  • 文章类型: Journal Article
    Molecular absorption spectrometry (MAS), originally developed in the 1970s, is a technique to determine non-metals in flames and graphite furnaces by monitoring the absorbance of diatomic molecules. Early studies employed low resolution instruments designed for line source atomic absorption, which provided a limited choice of analytical wavelengths, insufficient spectral resolution, and spectral interferences. However, the development of high-resolution continuum source atomic absorption spectrometry (HR-CS AAS) instrumentation has allowed the analysis of challenging samples for non-metals as well as some difficult elements to determine by AAS, such as aluminum and phosphorus. In this review, theory and analytical considerations for MAS are discussed. The principles and limitations of low resolution MAS are described, along with its applications. HR-CS AAS instrumentation is reviewed, emphasizing performance characteristics most relevant for MAS. Applications of flame and HR-CS GFMAS are reviewed, highlighting the most significant work to date. The paper concludes with an evaluation of the enhanced analytical capabilities provided by HR-CS MAS.
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