Liquid chromatography-mass spectrometry analytical method

Dohta, Y, Yamashita, T, Horiike, S., Nakamura, T. and Kukami, T. (2007) A system for logD screening of 96-weIl plates using a water-plug aspiration/ injection method combined with high-performance liquid chromatography-mass spectrometry. Analytical Chemistry, 79, 8312-8315. 

Robb DB, Covey TR, Bruins AP (2000) Atmospheric Pressure Photoionization An Ionization Method for Liquid Chromatography-Mass Spectrometry. Analytical Chemistry 72 3653-3659... 

The method for chloroacetanilide soil metabolites in water determines concentrations of ethanesulfonic acid (ESA) and oxanilic acid (OXA) metabolites of alachlor, acetochlor, and metolachlor in surface water and groundwater samples by direct aqueous injection LC/MS/MS. After injection, compounds are separated by reversed-phase HPLC and introduced into the mass spectrometer with a TurboIonSpray atmospheric pressure ionization (API) interface. Using direct aqueous injection without prior SPE and/or concentration minimizes losses and greatly simplifies the analytical procedure. Standard addition experiments can be used to check for matrix effects. With multiple-reaction monitoring in the negative electrospray ionization mode, LC/MS/MS provides superior specificity and sensitivity compared with conventional liquid chromatography/mass spectrometry (LC/MS) or liquid chromatography/ultraviolet detection (LC/UV), and the need for a confirmatory method is eliminated. In summary,... 

The need to understand the fate of pesticides in the environment has necessitated the development of analytical methods for the determination of residues in environmental media. Adoption of methods utilizing instrumentation such as gas chro-matography/mass spectrometry (GC/MS), liquid chromatography/mass spectrometry (LC/MS), liquid chromatography/tandem mass spectrometry (LC/MS/MS), or enzyme-linked immunosorbent assay (ELISA) has allowed the detection of minute amounts of pesticides and their degradation products in environmental samples. Sample preparation techniques such as solid-phase extraction (SPE), accelerated solvent extraction (ASE), or solid-phase microextraction (SPME) have also been important in the development of more reliable and sensitive analytical methods. 

For method tryout, run a control sample and two fortifications from each site. One fortification should be done at the LOQ and the other at the highest expected residue level, perhaps 1000 x LOQ. If the recoveries are within the acceptable range of 70-120% and there are no interferences, proceed with the method validation. If interferences are present which prevent quantitation of the analyte, try additional cleanup steps with SPE or use a more selective detection method such as liquid chromatography/mass spectrometry (LC/MS). 

Nowadays, ESI is the leading member of the group of atmospheric pressure ionization (API) methods and the method of choice for liquid chromatography-mass spectrometry coupling (LC-MS, Chap. 12). [10-13] Currently, ESI and MALDI (Chap. 10) are the most commonly employed ionization methods and they opened doors to the widespread biological and biomedical application of mass spectrometry. [5,10,11,13-17] Moreover, ESI serves well for the analysis of ionic metal complexes [18,19] and other inorganic analytes. [20-22]... 

The year 2002 was an extraordinary year for liquid chromatography-mass spectrometry (LC/MS) practitioners. On October 9, 2002, the Royal Swedish Academy of Sciences annonnced their decision to award the Nobel Prize in Chemistry to John B. Fenn, Koichi Tanaka, and Kurt Wiithrich for their development of analytical methods for the identification and structnral analysis of biological macromolecnles. Fenn and Tanaka shared the prize for developing electrospray and soft-laser desorption, respectively. These soft-ionization techniqnes allow macromolecules to be ionized withont fragmentation. 

Important progress in terms of higher throughput in ADME/PK work was realized recently by wider use of liquid chromatography/mass spectrometry (LC/MS), which has now become a standard analytical tool [26]. Flow NMR spectroscopy has become a routine method to resolve and identify mixtures of compounds and has found applications in drug metabolism and toxicology studies [27]. 

High-throughput liquid chromatography/Mass spectrometry method for the determination of the chromatographic hydrophobicity index. Analytical Chemistry, 73, 3716-3722. 

Internal reflection spectroscopy is widely applied for on-line process control. In this type of application, the chemical reactor is equipped with an internal reflection probe or an IRE. The goal of this type of application is the quantification of reactant and/or product concentrations to provide real-time information about the conversion within the reactor. In comparison with other analytical methods such as gas chromatography, high-pressure liquid chromatography, mass spectrometry, and NMR spectroscopy, ATR spectroscopy is considerably faster and does not require withdrawal of sample, which can be detrimental for monitoring of labile compounds and for some other applications. 

T Gomyo, M Ozawa, S Kobayashi. Analytical method for determining the total content of methyl benzimidazole carbamate fungicides in water by column switching liquid chromatography mass spectrometry. Anal Sci 8 687-690, 1992. 

RD Voyksner, T Cairns. Application of liquid chromatography-mass spectrometry to the determination of pesticides. In J Sherma, ed. Analytical methods for pesticides and plant growth regulators. New York Academic Press, 1989, pp 119-166. 

Liquid chromatography/mass spectrometry (LC/MS)-based techniques provide unique capabilities for pharmaceutical analysis. LC/MS methods are applicable to a wide range of compounds of pharmaceutical interest, and they feature powerful analytical figures of merit (sensitivity, selectivity, speed of analysis, and cost-effectiveness). These analytical features have continually improved, resulting in easier-to-use and more reliable instruments. These developments coincided with the pharmaceutical industry s focus on describing the collective properties of novel compounds in a rapid, precise, and quantitative way. As a result, the predominant pharmaceutical sample type shifted from nontrace/pure samples to trace mixtures (i.e., protein digests, natural products, automated synthesis, bile, plasma, urine). The results of these developments have been sig-... 

As an instrumental approach to conventional electrophoresis, capillary electrophoresis offers the capability of on-line detection, micropreparative operation and automation (6,8,45-47). In addition, the in tandem connection of capillary electrophoresis to other spectroscopy techniques, such as mass spectrometry, provides high information content on many components of the simple or complex peptide under study. For example, it has been possible to separate and characterize various dynorphins by capillary electrophoresis-mass spectrometry (33). Therefore, the combination of CE-mass spectrometry (CE-MS) provides a valuable analytical tool useful for the fast identification and structural characterization of peptides. Recently, it has been demonstrated that the use of atmospheric pressure ionization using Ion Spray Liquid Chromatography/ Mass Spectrometry is well suited for CE/MS (48). This approach to CE/MS provides a very effective and straightforward method which allow the feasibility of obtaining CE/MS data for peptides from actual biological extracts, i.e., analysis of neuropeptides from equine cerebral spinal fluid (33). 

An extensive list that defines acronyms and abbreviations in the field of mass spectrometry was published in 2002 [6], A single analytical technique or a type of instrument is abbreviated without hyphens or slashes. However, it is customary to use hyphens for a description of an instrument whereas an abbreviation that describes the method uses slashes. For example, LC-MS is an instrument where a liquid chromatograph is coupled with a mass spectrometer, while LC/MS is the method of liquid chromatography/mass spectrometry. Thus, one uses an LC-MS instrument to obtain a LC/MS spectrum. 

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