Tandem mass spectrometry validation

Cawood, M.L., Field, H.P., Ford, C.G., Gillingwater, S., Kiernan, A., Cowan, D. and Barth, J.H. (2005). Testosterone measurement by isotope-dilution liquid chromatography-tandem mass spectrometry validation of a method for routine clinical practice. Clin. Chem., 51, 1472-1479. 

Chance DH, Adam BW, Smith SJ, Alexander JR, Hillman SL, Hannon WH (1999) Validation of accuracy-based amino acid reference materials in dried-blood spots by tandem mass spectrometry for newborn screening assays. Clin Chem 45 1269-1277. 

Full acceptance of HPLC/MS methods by the US EPA OPP as enforcement methods occurred between 1998 and 2001. For example, in 1998, the EPA OPP accepted HPLC/MS (without MS/MS) methods as primary enforcement methods, and high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) only was suitable for confirmatory methods. However, in 2001, HPLC/MS/MS methods also became acceptable for primary enforcement. Table 4 summarizes the types of methods that were validated by the EPA OPP method validation program, for both food tolerance enforcement methods and environmental chemistry methods. 

The analyses of illicit drugs and metabolites in the sampled waters were performed following a previously described and validated fully automated method based on on-line solid phase extraction-liquid chromatography-tandem mass spectrometry (on-line SPE-LC-MS/MS) [19]. 

Chu, I. et al. 2000. Validation of higher throughput high-performance liquid chromatography/atmo-spheric pressure chemical ionization tandem mass spectrometry assays to conduct cytochrome P450s... 

King, R.C. et al. 2002. Description and validation of a staggered parallel high performance liquid chromatography system for good laboratory practice level quantitative analysis by liquid chromatography/tandem mass spectrometry. Rapid Commun. Mass Spectrom. 16 43. 

Keevil, B.G. et al. 2004. Validation of an assay for voriconazole in serum samples using liquid chromatography-tandem mass spectrometry. Ther Drug Monit. 26 650. 

F. Calbiani, M. Careri, L. Elviri, A. Mangia, L. Pistara and I. Zagnoni, Development and in-house validation of a liquid chromatography-electrospray-tandem mass spectrometry method for the simultaneous determination of Sudan I, Sudan II, Sudan II and Sudan IV in hot chili products. J. ChromatogrA, 1043 (2004) 123-130. 

Borman, P. J., Chatfield, M. J., Crowley, E. L., Eckers, C., Elder, D. P., Francey, S. W., Laures, A. M-F., Wolff, J-C. Development, validation and transfer into a factory environment of a liquid chromatography tandem mass spectrometry assay for the highly neurotoxic impurity FMTP (4-(4-flurophenyl)-l-methyl-l,2,3,6-tetrahydropyridine) in paroxetine active pharmaceutical ingredient (API). J. Pharm. Biomed. Anal., 48, 2008, 1082-1089. 

Jemal, M., Schuster, A., and Whigan, D. B. (2003). Liquid chromatography/tandem mass spectrometry methods for quantitation of mevalonic acid in human plasma and urine method validation, demonstration of using a surrogate analyte, and demonstration of unacceptable matrix effect in spite of use of a stable isotope analog internal standard. Rapid Commun. Mass Spectrom. 17, 1723-1734. 

As analytical and bioanalytical methods must be validated before using them for routine sample analysis and after changing method parameters (see Chapter 8), instruments such as liquid chromatography coupled with mass spectrometry (LC-MS) or tandem mass spectrometry (LC-MS/MS), which are utilized to perform the analysis, should be calibrated and qualified. In addition, an instrument s performance should be tested for suitability prior to use on practically a day-to-day basis. 

Stewart PM, Murray BA, Mason JI (1994) Human kidney 1 l/ -hydroxysteroid dehydrogenase is a high affinity nicotinamide adenine dinucleotide-dependent enzyme and differs from the cloned type I isoform. J Clin Endocrinol Metab 79 480-484 Taylor RL, Machacek D, Singh RJ (2002) Validation of a high-throughput liquid chromatography-tandem mass spectrometry method for urinary cortisol and cortisone. Clin Chem 48 1511-1519... 

Yang, L., Clement, R. P., Kantesaria, B., Reyderman, L., Beaudry, F., Grandmaison, C., Di Donato, L., Masse, R., and Rudewicz, P. J. (2003). Validation of a sensitive and automated 96-well solid-phase extraction liquid chromatography-tandem mass spectrometry method for the determination of desloratadine and 3-hydroxydesloratadine in human plasma.. /. Chromatogr. B Anal. Technol. Biomed. Life Sci. 792 229-240. 

W.W. Bullen, R.A. Miller, R.N. Hayes, Development and validation of a high-performance liquid chromatography tandem mass spectrometry assay for atorvastatin, ortho-hydroxy atorvastatin, and para-hydroxy atorvastatin in human, dog, and rat plasma, J. Am. Soc. Mass Spectrom. 10 (1999) 55-66. 

A liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed [33] and validated for the determination of donepezil in human plasma samples. Diphenhydramine was used as the IS. The collision-induced transition m/z 380 > 91 was used to analyze donepezil in selected reaction monitoring mode. The signal intensity of the m/z 380 —> 91 transition was found to relate linearly with donepezil concentrations in plasma from 0.1 to 20.0 ng/ml. The lower limit of quantification of the LC/MS/MS method was 0.1 ng/ml. The intra- and inter-day precisions were below 10.2% and the accuracy was between 2.3% and +2.8%. The validated LC/MS/MS method was applied to a pharmacokinetic study in which healthy Chinese volunteers each received a single oral dose of 5 mg donepezil hydrochloride. The non-compartmental pharmacokinetic model was used to fit the donepezil plasma concentration-time curve. Maximum plasma concentration was... 

Frerichs et al. [128] developed and validated a method for the quantitation of omeprazole and hydroxyomeprazole from one 250 [A sample of human plasma using HPLC coupled to tandem mass spectrometry. The method was validated for a daily working range of 0.4-100 ng/ml, with limits of detection between 2 and 15 pg/ml. The interassay variation was less than 15% for all analytes at four control concentrations and the samples were stable for three freeze-thaw cycles under the analysis conditions and 24 h in the postpreparative analysis matrix. The method was used to analyze samples in support of clinical studies probing the activity of the cytochrome P-450 enzyme system. 

Song and Naidong [129] analyzed omeprazole and 5-hydroxyomepra-zole in human plasma using hydrophilic interaction chromatography with tandem mass spectrometry. Omeprazole and its metabolite 5-hydroxy omeprazole and the internal standard desoxyomeprazole were extracted from 0.05 ml of human plasma using 0.5 ml of ethyl acetate in a 96-well plate. A portion (0.1 ml) of the ethyl acetate extract was diluted with 0.4 ml of acetonitrile and 10 /il was injected onto a Betasil silica column (5 cm x 3 mm, 5 /rm) and detected by atmospheric pressure ionization 3000 and 4000 with positive electrospray ionization. Mobile phase with linear gradient elution consists of acetonitrile, water, and formic acid (from 95 5 0.1 to 73.5 26.5 0.1 in 2 min). The flow-rate was 1.5 ml/min with total rim time of 2.75 min. The method was validated for a low limit of quantitation at 2.5 ng/ml for both analytes. The method was also validated for specificity, reproducibility, stability, and recovery. 

Ashwin, H.M., S.L. Stead, J.C. Taylor, et al. 2005. Development and validation of screening and confirmatory methods for the detection of chloramphenicol and chloramphenicol glucuronide using SPR biosensor and liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta 529 103-108. 

Jemal M, Schuster A, Whigan DB (2003) Liquid chromatography/tandem mass spectrometry methods for quantitation of mevalonic acid in human plasma and urine method validation,... 

Lankheet AG et al (2009) A validated assay for the quantitative analysis of vatalanib in human EDTA plasma by liquid chromatography coupled with electrospray ionization tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci 877 3625-3630... 

Beer B et al (2010) Development and validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of tamoxifen, anastrozole, and letrozole in human plasma and its application to a clinical study. Anal Bioanal Chem 398 1791-1800... 

Deventer K, Delbeke FT (2003) Validation of a quantitative screening method for corticosteroids by liquid chromatography tandem mass spectrometry. In Shanzer W, GeyerH, Gotzmann A, Mareck U (eds) Recent advances in doping analysis, vol 11, Spert and Buch Straub, Koln,... 

Harwood DT, Handelsman DJ (2009) Development and validation of a sensitive liquid chromatography-tandem mass spectrometry assay to simultaneously measure androgens and estrogens in serum without derivatization. Clin Chim Acta 409 78-84... 

Stout PR, Bynum ND, Mitchell JM, Baylor MR, Ropero-Miller JD (2009) A comparison of the validity of gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry analysis of urine samples for morphine, codeine, 6-acetylmorphine, and benzoylecgonine. J Anal Toxicol 33(8)398 108... 

Kala SV, Harris SE, Freijo TD, Gerlich S (2008) Validation of analysis of amphetamines, opiates, phencyclidine, cocaine, and benzoylecgonine in oral fluids by liquid chromatography-tandem mass spectrometry. J Anal Toxicol 32(8) 605—611... 

Chi C, Liang L, Padovani P et al. (2003) Development and validation of a liquid chromatography-mass spectrometric method for the determination of DPC 423, an antithrombotic agent, in rat and dog plasma. J Chromatogr B Analyt Technol Biomed Life Sci 783( 1) 163—172 Zimmer D, Muschalek V, Muller C (2000) Determination of met-rifonate enantiomers in blood and brain samples using liquid chromatography on a chiral stationary phase coupled to tandem mass spectrometry. Rapid Commun Mass Spec-trom 14(15) 1425-1432... 

Sottani C, Zuchetti M, Zaffaroni M et al. (2004) Validated procedure for simultaneous trace level determination of the anti-cancer agent gemcitabine and its metabolite in human urine by high-performance liquid chromatography with tandem mass spectrometry. Rapid Communications in Mass Spectrometry 18 1017-1023... 

Hou W, Watters JW, McLeod HL (2004) Simple and rapid docetaxel assay in human plasma by protein precipitation and high-performance liquid chromatography-tandem mass spectrometry. Journal of Chromatography B 804 263-267 Schuhmacher J, Zimmer D, Tesche F, Pickard V (2003) Matrix effects during analysis of plasma samples by electrospray and atmospheric pressure chemical ionization mass spectrometry practical approaches to their elimination. Rapid Communications in Mass Spectrometry 17 1950-1957 Shah PW (2001) Guidance for Industry Bioanalytical Method Validation U.S. Department of Health and Human Services, Food and Drug Administration... 

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