Quantitative liquid chromatography mass

Takino, M., Daishima, S., Yamaguchi, K., and Nakahara, T. (2003). Quantitative liquid chromatography-mass spectrometry determination of catechins in human plasma by automated on-line extraction using turbulent-flow chromatography. Analyst 128 46-50. 

Zhang ZY, King BM, Wong YN. Quantitative liquid chromatography/mass spectro-metry/mass spectrometry warfarin assay for in vitro cytochrome P450 studies. Anal Biochem 2001 298 40-49. 

Lanckmans K, Sarre S, Smolders I, Michotte Y. Quantitative liquid chromatography/ mass spectrometry for the analysis of microdialysates. Talanta 2008 74 458—69. 

A liquid chromatography-mass spectrometry (LC-MS) method that can quantitatively analyze urinar y normal and modified nucleosides in less than 30 min with a good resolution and sufficient sensitivity has been developed. Nineteen kinds of normal and modified nucleosides were determined in urine samples from 10 healthy persons and 18 breast cancer patients. Compounds were separ ated on a reverse phase Kromasil C18 column (2.1 mm I.D.) by isocratic elution mode using 20 mg/1 ammonium acetate - acetonitrile (97 3 % v/v) at 200 p.l/min. A higher sensitivity was obtained in positive atmospheric pressure chemical ionization mode APCI(-i-). 

Figure 5.67 Reconstructed ion chromatograms for Idoxifene and internal standard (ds-Idoxifene using LC-ToF-MS for (a) double-blank human plasma extract, (b) extract of blank human plasma containing internal standard (IS), and (c) control-blank human plasma spiked with Idoxifene at 5 gml , the LOQ of the method. Reprinted from 7. Chromatogr., B, 757, Comparison between liquid chromatography-time-of-flight mass spectrometry and selected-reaction monitoring liquid chromatography-mass spectrometry for quantitative determination of Idoxifene in human plasma , Zhang, H. and Henion, J., 151-159, Copyright (2001), with permission from Elsevier Science.

Liquid chromatography/mass spectrometry Lower limit of detection Limit of detection Limit of quantitation Florseshoe crab hemocyanin Liquid scintillation counting Matrix-assisted laser desorption/ ionization mass spectrometry m -Maleimidobenzoy 1-A -Hydroxysuccinimide 1 -Cyclohexyl-3-(2-Morptiolino-ethyl)carbodiimide rnetlio-/ -Toluenesulfonate (same as CDI)... 

LC/MS/MS. LC/MS/MS is used for separation and quantitation of the metabolites. Using multiple reaction monitoring (MRM) in the negative ion electrospray ionization (ESI) mode, LC/MS/MS gives superior specificity and sensitivity to conventional liquid chromatography/mass spectrometry (LC/MS) techniques. The improved specificity eliminates interferences typically found in LC/MS or liquid chro-matography/ultraviolet (LC/UV) analyses. Data acquisition is accomplished with a data system that provides complete instmment control of the mass spectrometer. 

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). 

Liquid chromatography/mass spectrometry (LC/MS) analysis Quantitation system Agilent Series 1100 liquid chromatograph Chromsep Omnispher 3 Cig HPLC column, 100 x 4.6-mm i.d., 3- am diameter particle size... 

Gu, S Du, Y Chen, J., Liu, Z Bradbury, E.M., Hu, C.A., Chen, X. (2004). Large-scale quantitative proteomic study of PUMA-induced apoptosis using two-dimensional liquid chromatography—mass spectrometry coupled with amino acid-coded mass tagging. J. Proteome Res. 3, 1191 1200. 

Andreu V, Ferrer E, Rubio JL, Font G, Pico Y (2007) Quantitative determination of octylphenol, nonylphenol, alkylphenol ethoxylates and alcohol ethoxylates by pressurized liquid extraction and liquid chromatography-mass spectrometry in soils treated with sewage sludges. Sci Total Environ 378 124—129... 

High-Throughput Quantitative Pharmaceutical Analysis in Drug Metabolism and Pharmacokinetics Using Liquid Chromatography-Mass Spectrometry... 

Liang, H.R. Foltz, R.L. Meng, M. Bennett, P. Ionization enhancement in atmospheric pressure chemical ionization and suppression in electrospray ionization between target drugs and stable-isotope-labeled internal standards in quantitative liquid chromatography/tandem mass spectrometry. Rapid Commun. Mass Spectrom. 2003, 17, 2815—2821. 

Li C, Hong Y, Tan YX et al. Accurate qualitative and quantitative proteomic analysis of clinical hepatocellular carcinoma using laser capture microdissection coupled with isotope-coded affinity tag and two-dimensional liquid chromatography mass spectrometry. Mo/ Cell Proteomics 2004,3399-409. 

Jansen EEW, Gibson KM, Shigematsu Y, Jakobs C, Verhoeven N (2006) A novel, quantitative assay for homocarnosine in cerebrospinal fluid using stable-isotope dilution liquid-chromatography mass spectrometry. J Chromatogr Analyt Technol Biomed Life Sci 18 196-200... 

SM Musser. Quantitation and identification of fumonisins by liquid chromatography/mass spectrometry. Adv Exp Med Biol 392 65-74, 1996. 

Bakhtiar, R., and Majumdar, T. K. (2007). Tracking problems and possible solutions in the quantitative determination of small molecule chugs and metabolites in biological fluids using liquid chromatography-mass spectrometry. J. Pharmacol. Toxicol. Methods 55 227-243. 

Stokvis, E., Rosing, H., and Beijnen, J. H. (2005). Stable isotopically labeled internal standards in quantitative bioanalysis using liquid chromatography/mass spectrometry Necessity or not Rapid Commun. Mass Spectrom. 19 401-407. 

Zhang, H., and Henion, J. (2001). Comparison between liquid chromatography-time-of-flight mass spectrometry and selected reaction monitoring liquid chromatography-mass spectrometry for quantitative determination of idoxifene in human plasma. J. Chromatogr. B Biomed. Sci. Appl. 757 151-159. 

Ynddal, L., and Hansen, S. H. (2003). On-line turbulent-flow chromatography-high-performance liquid chromatography-mass spectrometry for fast sample preparation and quantitation.. /. Chromatogr. A. 1020 59-67. 

V. Ratsimba, J. M. Garcia Fernadez, J. Defaye, H. Nigay, and A. Voilley, Qualitative and quantitative evaluation of mono- and disaccharides in D-fructose and sucrose caramels by gas-liquid chromatography-mass spectrometry di-D-fructose dianhydrides as tracers of caramel authenticity, J. Chromatogr. A, 844 (1999) 283-293. 

To establish a sensitive and specific liquid chromatography-mass spectrometry (time-of-flight) [LC-MS (TOF)] method for the determination of donepezil in human plasma after an oral administration of 5 mg donepezil hydrochloride tablet [29]. Alkalized plasma was extracted with isopropa-nol-n-hexane (3 97) and loratadine was used as internal standard (IS). Solutes were separated on a Cis column with a mobile phase of metha-nokacetate buffer (pH 4.0) (80 20). Detection was performed on a TOF mass spectrometry equipped with an electrospray ionization interface and operated in positive-ionization mode. Donepezil quantitation was realized by computing the peak area ratio (donepezil-loratadine) (donepezil m/z 380 [M + H]+ and loratadine m/z 383[M + H]+) and comparing them with calibration curve (r = 0.9998). The linear calibration curve was obtained in the concentration range of 0.1-15 jUg/1. The detection limit of donepezil was 0.1 /zg/1. The average recovery was more than 90%. The intra- and inter-run precision was measured to be below 15% of RSD... 

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-... 

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