e-book Hyphenated techniques in speciation analysis

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Hyphenated separation techniques refer to a combination of two or more techniques to detect and separate chemicals from solutions. Most often the other technique is some form of chromatography. Hyphenated techniques are widely used in chemistry and biochemistry. A slash is sometimes used instead of hyphen, especially if the name of one of the methods contains a hyphen itself. To obtain structural information leading to the identification of the compounds present in a crude sample, liquid chromatography LC , usually a high-performance liquid chromatography HPLC , gas chromatography GC , or capillary electrophoresis CE is linked to spectroscopic detection techniques, e.

GC-MS, which is a hyphenated technique developed from the coupling of GC and MS, was the first of its kind to become useful for research and development purposes. Mass spectra obtained by this hyphenated technique offer more structural information based on the interpretation of fragmentations.

GCMS & LCMS (Gas Chromatography - Mass Spectroscopy & Liquid Chromatography - Mass Spectroscopy)

Sometimes, polar compounds, especially those with a number of hydroxyl groups, need to be derivatized for GC-MS analysis. The most common derivatization technique is the conversion of the analyte to its trimethylsilyl derivative. The time elapsed between injection and elution is called ''retention time'' tR.

The equipment used for GC-MS generally consists. The GC-MS columns can be of two types: capillary columns and macrobore and packed columns. The interface transports efficiently the effluent from the GC to MS. However, in modern GC-MS systems, various other types can be used that allow identification of molecular ion. For example, an orthogonal TOF mass spectrometry coupled with GC is used for confirmation of purity and identity of the components by measuring exact mass and calculating elemental composition.

LC-ICP-MS: The most often used hyphenated system for speciation analysis

Nowadays, a GC-MS is integrated with various on-line MS databases for several reference compounds with search capabilities that could be useful for spectra match for the identification of separated components. In addition, as a detection technique, IR is much less sensitive compared to various other detection techniques, e.

In this case, absorption of the mobile phase induces the interference of the detection of sample component absorption bands, but some transparent region of the mid-IR range produces detection possibility. For example, if one uses a mobile phase of a deuterated solvent such as heavy water or perdeuterated methanol, IR can monitor many organic compounds that have C-H structures in the molecules. The solvent-elimination approach is the preferred option in most of the LC-IR operations, the mobile phase solvent is eliminated, IR detection is carried out in some medium that has a transparency for IR light.

Generally, KBr or KCl salts are used for the collection of sample components in the eluent, and heating up the medium before IR detection eliminates the volatile mobile phase solvents 5, 6. There are two types of interfaces for the solvent-elimination approach:. Instrumentation: A switching valve can help make a working combination of the two techniques.

The diverter generally operates as an automatic switching valve to divert undesired portions of the eluate from the LC system to waste before the sample enters the MS. The ionization techniques used in LC-MS are generally soft ionization techniques that mainly display the molecular ion species with only a few fragment ions. Hence, the information obtained from a single LC-MS run, on the structure of the compound, is rather poor. However, this problem has now been tackled by the introduction of tandem mass spectrometry MS-MS , which provides fragments through collision-induced dissociation of the molecular ions produced.

MS is one of the most sensitive and highly selective methods of molecular analysis, and provides information on the molecular weight as well as the fragmentation pattern of the analyte molecule. The information obtained from MS is invaluable for confirming the identities of the analyte molecules 7, 8, 9.

LC-NMR experiments can be performed in both continuous-flow and stop-flow modes. Magnetic field strengths higher than 9.

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The analytical flow cell was initially constructed for continuous-flow NMR acquisition. However, the need for full structural assignment of unknown compounds, especially novel natural products, has led to the application in the stopped-flow mode. From this detector, the flow is guided into the LC-NMR interface, which can be equipped with additional loops for the intermediate storage of selected LC peaks.

Following passage through the probe-head, the flow is routed to a fraction collector for recovery and further investigation of the various fractions analyzed by NMR. In most of the LC-NMR operations, reversed-phase columns are used, employing a binary or tertiary solvent mixture with isocratic or gradient elution. The protons of the solvents of the mobile phase cause severe problems for obtaining an adequate NMR spectrum.

The receiver of the NMR spectrometer is not quite able to handle the intense solvent signals and the weak substance signals at the same time. To overcome this problem, solvent signal suppression can be achieved by one of the three major methods: presaturation, soft-pulse multiple irradiation or water suppression enhancement through T1 effects WET presaturation employing a z-gradient It separates species by applying voltage across buffer-filled capillaries, and is generally used for separating ions that move at different speeds when voltage is applied, depending on their size and charge.

The solutes are seen as peaks as they pass through the detector and the area of each peak is proportional to their concentration, which allows quantitative determinations. Analysis includes purity determination, assays, and trace level determinations Application of Hyphenated Technique in Pharmacy 12, 13, 14, 15, 16 : Some examples of the application of hyphenated techniques in natural products analysis are Figure 7. LC-MS, if the ionization technique is chosen appropriately, can be an extremely powerful and informative tool for screening crude plant extracts.

The currently available various types of LC-MS systems allow the analysis of small nonpolar compounds to large polar constituents like oligosaccharides, proteins, and tannins present in natural product extracts. Int J Pharm Sci Res. Article Information Sr No: Download: Cited By: 4. Authors: Rachana R. Gupta and Shitalkumar S. Chromatography - Produces pure or nearly pure fractions of chemical components in a mixture. Shorter analysis time Higher degree of automation Higher sample throughput Better reproducibility Reduction of contamination because it is a closed system Enhanced combined selectivity and therefore higher degree of information Provide excellent separation efficiency as well as acquisition of on-line complementary spectro-scopic data on an LC or GC peak of interest within a complex mixture.

The equipment used for GC-MS generally consists An injection port at one end of a metal column often packed with a sand-like material to promote maximum separation A detector MS at the other end of the column. The analyte must not decompose before entering the MS ion source. The gas load entering the ion source must be within the pumping capacity of the MS.

Hyphenated Techniques in Speciation Analysis (RSC Publishing)

Applications: Useful for research and development purposes. Identification of molecular ion. Compounds that are adequately volatile, small, and stable in high temperature in GC conditions can be easily analyzed by GC-MS. Used for confirmation of purity and identity of the components by measuring exact mass and calculating elemental composition. While HPLC is one of the most powerful separation techniques available today, the IR or FTIR is a useful spectroscopic technique for the identification of organic compounds, because in the mid-IR region the structures of organic compounds have many absorption bands that are characteristic of particular functionalities, e.


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One is a flow-cell approach and Other is a solvent-elimination approach. There are two types of interfaces for the solvent-elimination approach: Diffuse-reflectance infrared Fourier transform DRIFT approach Buffer-memory technique. Hyphenated Techniques in Speciation Analysis.

outer-edge-design.com/components/plus/1705-how-to-tracking.php Joanna Szpunar , Ryszard Lobinski. Speciation analysis is a field of trace element analytical chemistry that deals with detection, identification and determination of individual chemical forms of metals and metalloids. There has been increased awareness of the importance of elemental speciation over the last 20 years and this has lead to growing demand for analytical techniques capable of providing species-specific information. Hyphenated Techniques in Speciation Analysis offers a brief but comprehensive overview of hyphenated techniques and their various applications for the determination of chemical forms of trace elements.

It brings a succinct presentation of the concept of speciation analysis, gives an overview of techniques based on coupling of chromatography with element and molecule specific detection and summarises their applications in the fields of environmental and industrial chemistry, biochemistry, nutrition, toxicology and medicine.

Fully referenced, Hyphenated Techniques in Speciation Analysis is an invaluable introduction to elemental speciation analysis and also provides a practising analyst with a critical overview of research carried out in the field. Element Specific Detection in Chromatography. Electrophoretic Techniques with Element Selective.

Electrospray Mass Spectrometry in Elemental Speciation.

Quality Control and Assurance in Speciation Analysis. Multielement Analysis of Organometallic Species in.