Drug product liquid chromatography/mass

Wu Y. The use of liquid chromatography-mass spectrometry for the identification of drug degradation products in pharmaceutical formulations. Biomed Chromatogr 2000 14 384-396. 

The ability to gather more knowledge faster with smaller quantities of complex samples can support these increased demands on pharmaceutical R D. The advanced approaches and technologies associated with liquid chromatography-mass spectrometry (LC-MS) continue to play a significant role within drug discovery because of the inherent sensitivity and selectivity of this analytical platform. Improvements with increased throughput and easier-to-use instruments have allowed researchers unprecedented levels of efficiency and productivity. 

Turnipseed SB, Roybal JE, Pfennig AP, Kijak PJ, Use of ion-trap liquid chromatography-mass spectrometry to screen and confirm drug residues in aquacultured products, Anal. Chim. Acta 2003 483(l-2) 373-386. 

Eckers, C. Laures, A.M. Giles, K. Major, H. Pringle, S. Evaluating the utihty of ion mobility separation in combination with high-pressure liquid chromatography/mass spectrometry to facihtate detection of trace impurities in formulated drug products. Rapid Commun. Mass Spectrom. 2007, 21,1255-1263. 

Liquid chromatography—mass spectroscopy has become one of the most powerful analytical techniques in the drug discovery and development proeess. LC tandem MS is obviously the technique of choice for the identification of metabolites as illustrated in this chapter. Exact mass measurements and elemental composition assignment are essential for the characterization of the metabolites. Accurate mass measurements of the product ions, formed in an MS/MS experiment, greatly facilitate the structure elucidation of the metabolites. With the ever evolving technological advances in mass spectrometry and separation science, LC MS will continue to play an important role in metabolite identification in the future. 

See also Bioassays Overview Microbial Tests Bioautography. Blood and Plasma. Fluorescence Clinical and Drug Applications Food Applications. Food and Nutritional Analysis Dairy Products. Gas Chromatography Mass Spectrometry. Immunoassays, Techniques Enzyme Immunoassays. Liquid Chromatography Normal Phase Reversed Phase Food Applications. Microbiological Techniques. Radiochemical Methods Food and Environmental Applications. Vitamins Fat-Soluble. 

Kasprzyk-Hordern B, Dinsdale RM, Guwy AJ (2008) Multiresidue methods for the analysis of pharmaceuticals, personal care products and illicit drugs in surface water and wastewater by solid-phase extraction and ultra performance liquid chromatography-electrospray tandem mass spectrometry. Anal Bioanal Chem 391(4) 1293-1308... 

Liquid chromatography-electrospray ionization mass spectrometry (LC-ESTMS) for analysis of sildenafil has also been developed and applied to 40 botanical products. About half of the analyzed samples proved to contain undeclared additives of the three drugs sildenafil, vardenafil, and tadalafil <2004JPBA525>. A similar electrokinetic capillary chromatography method to that proposed for the determination of sildenafil 82 has been reported for vardenafil 98 and tadalafile 99. Statistical evaluation of the electrophoretic results was achieved. The described method is thought to be rapid and sensitive <2004JCH231>. 

Jemal, M., Ouyang, Z., Xia, Y. Q., and Powell, M. L. (1999b). A versatile system of high-flow high performance liquid chromatography with tandem mass spectrometry for rapid direct-injection analysis of plasma samples for quantitation of a beta-lactam drug candidate and its open-ring biotransformation product. Rapid Commun. Mass Spectrom. 13 1462-1471. 

Isolation of Processes To minimize cross-contamination and microbiological contamination, the manufacturer may develop special procedures for the isolation of processes. The level of facilities isolation depends on the types of products to be manufactured. For instance, steroids and sulfas require more isolation than over-the-counter (OTC) oral products [6], To minimize exposure of personnel to drug aerosols and loss of product, a sealed pressure vessel must be used to compound aerosol suspensions and emulsions [21], An example of cross-contamination with steroids was the controversial case of a topical drug manufactured for the treatment of skin diseases. Fligh-performance liquid chromatography/ultraviolet and mass spectrometry (FIPLC/UV, FIPLC/MS) techniques were used by the FDA for the detection of clobetasol propionate, a class 1 superpotent steroid, as an undeclared steroid in zinc pyrithione formulations. The product was forbidden and a warning was widely published [22],... 

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