Tutorial review on validation of liquid chromatography-mass spectrometry methods: Part I

Analytica Chimica Acta

Volumn 870, Issue 1, 2015, Pages 29-44

  Kruve, Anneli ^a   Rebane, Riin ^a   Kipper, Karin ^a   Oldekop, Maarja Liisa ^a   Evard, Hanno ^a   Herodes, Koit ^a   Ravio, Pekka ^b   Leito, Ivo ^a  

^a UNIVERSITY OF TARTU   (Estonia)

^b Finnish Customs Laboratory   (Finland)

Author keywords

Electrospray; Ionization suppression; Limit of detection; Liquid chromatography mass spectrometry; Robustness; Validation

Indexed keywords

CHROMATOGRAPHY; ELECTROSPRAY IONIZATION; HIGH PRESSURE LIQUID CHROMATOGRAPHY; IONIZATION; IONIZATION OF LIQUIDS; LIQUIDS; MASS SPECTROMETRY; ROBUSTNESS (CONTROL SYSTEMS); SPECTROMETRY;

ELECTROSPRAYS; LIMIT OF DETECTION; LIMIT OF QUANTIFICATIONS; LIQUID CHROMATOGRAPHY - MASS SPECTROMETRIES; LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY; PERFORMANCE CHARACTERISTICS; PERFORMANCE PARAMETERS; VALIDATION;

LIQUID CHROMATOGRAPHY;

ATMOSPHERIC PRESSURE PHOTO IONIZATION; CONSEQUENT REACTION MONITORING; DIAGNOSTIC PROCEDURE; ELECTROSPRAY; INFRARED SPECTROSCOPY; IONIZATION; LIMIT OF DETECTION; LIMIT OF QUANTITATION; LIQUID CHROMATOGRAPHY; LIQUID LIQUID EXTRACTION; MASS FRAGMENTOGRAPHY; MASS SPECTROMETRY; MEASUREMENT ACCURACY; MEASUREMENT PRECISION; MULTIPLE REACTION MONITORING; NEUTRAL LOSS SCAN; PRIORITY JOURNAL; REVIEW; SELECTED REACTION MONITORING; SIGNAL NOISE RATIO; SOLID PHASE EXTRACTION; TIME OF FLIGHT MASS SPECTROMETRY; ULTRAVIOLET SPECTROPHOTOMETRY; VALIDATION PROCESS;

EID: 84929947828     PISSN: 00032670     EISSN: 18734324     Source Type: Journal    
DOI: 10.1016/j.aca.2015.02.017     Document Type: Review

References (159)

1. Gross J.H. Mass Spectrometry 2011, Springer, Heidelberg. second ed.
2. Korfmacher W.A. Foundation Review: principles and applications of LC-MS in new drug discovery. Drug Discovery Today 2005, 10:1357-1367.
3. Brooks B.W., Huggett D.B. Human Pharmaceuticals in the Environment. Current and Future Perspectives 2012, Springer, New York.
4. Kruve A., Herodes K., Leito I. Optimization of electrospray interface and quadrupole ion trap mass spectrometer parameters in pesticide liquid chromatography/electrospray ionization mass spectrometry analysis. Rapid Commun. Mass Spectrom. 2010, 25:1159-1168.
5. Jemal M., Xia Y.Q. LC-MS development strategies for quantitative bioanalysis. Curr. Drug Metab. 2006, 7:491-502.
6. Taverniers I., De Loose M., Van Bockstaele E. Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance. TrAC Trends Anal. Chem. 2004, 23:535-552.
7. Trullols E., Ruisánchez I., Rius F.X. Validation of qualitative analytical methods. TrAC Trends Anal. Chem. 2004, 23:137-145.
8. Pizzutti I.R., de Kok A., Zanella R., Adaime M.B., Hiemstra M., Wickert C., Prestes O.D. Method validation for the analysis of 169 pesticides in soya grain without clean up, by liquid chromatography-tandem mass spectrometry using positive and negative electrospray ionization. J. Chromatogr. A 2007, 1142:123-136.
9. Van Eeckhaut A., Lanckmans K., Sarre S., Smolders I., Michotte Y. Validation of bioanalytical LC-MS/MS assays: evaluation of matrix effects. J. Chromatogr. B 2009, 877:2198-2207.
10. Rogatsky E., Stein D. Evaluation of matrix effect and chromatography efficiency: new parameters for validation of method development. J. Am. Soc. Mass Spectrom. 2005, 16:1757-1759.
11. ISO/IEC 17025,2005, General requirements for the competence of testing and calibration laboratories.
12. GLP-OECD Series on Principles of Good Laboratory Practice (GLP) and Compliance Monitoring.
13. Commission directive 2009/90/EC: Laying down, pursuant to Directive 2000/60/EC of the European Parliament and of the Council, technical specifications for chemical analysis and monitoring of water status. Off. J. Eur. Union, 2009.
14. Araujo P. Key aspects of analytical method validation and linearity evaluation. J. Chromatogr. B 2009, 877:2224-2234.
15. EurachemGuide: The Fitness for Purpose of Analytical Methods, Eurachem, Teddington, 1998.
16. B. Magnusson and U. Örnemark (Eds.) Eurachem Guide: The Fitness for Purpose of Analytical Methods - A Laboratory Guide to Method Validation and Related Topics, (second ed. 2014). ISBN 978-91-87461-59-0. Available from .
17. Harmonized Guidelines for single-laboratory validation of method of analyses (IUPAC Technical Report), Pure Appl. Chem. 74(5) (2002) 835-855.
18. ICH harmonized tripartite guideline: validation of analytical procedures: text and methodology Q2(R1), International Conference of harmonization of technical requirements for registration of pharmaceuticals for human use, 2005.
19. Guidance for Industry: Bioanalytical method validation, U.S. Department of Health and Human Services Food and Drug Administration, 2001
20. Guidance for Industry: Bioanalytical method validation, Draft Guidance, U.S. Department of Health and Human Services Food and Drug Administration , 2013. http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/UCM368107.pdf.
21. Guidance on Bioanalytical Method Validation, European Medicines Agency, 2011.
22. AOAC Guidelines for Single-Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals, Official Methods of Analysis, nineteenth ed., Appendix K, AOAC, INTERNATIONAL, Gaithersburg, MD, 2012.
23. Chandran S., Singh R.S.P. Comparison of various international guidelines for analytical method validation. Pharmazie 2007, 62:4-14.
24. Bonfilio R., Cazedey E.C.L., de Araújo M.B., Salgado H.R.N. Analytical validation of quantitative high-performance liquid chromatographic methods in pharmaceutical analysis: a practical approach. Crit. Rev. Anal. Chem. 2012, 42:87-100.
25. Rozet E., Marini R.D., Ziemons E., Boulanger B., Hubert P. Advances in validation, risk and uncertainty assessment of bioanalytical methods. J. Pharm. Biomed. 2011, 55:848-858.
26. Shabir G.A. Validation of high-performance liquid chromatography methods for pharmaceutical analysis: understanding the differences and similarities between validation requirements of the US Food and Drug Administration, the US Pharmacopeia and the International Conference on Harmonization. J. Chromatogr. A 2003, 987:57-66.
27. Peters F.T. Method validation using LC-MS. Applications of Liquid Chromatography-Mass Spectrometry in Toxicology 2006, 71-96. Pharmaceutical Press, London. A. Polettini (Ed.).
28. NordVal Protocol No. 2, Guide in validation of alternative propietary chemical methods, 2010.
29. González O., Blanco M.E., Iriarte G., Bartolomé L., Maguregui M.I., Alonso R.M. Bioanalytical chromatographic method validation according to current regulations with a special focus on the non-well defined parameters limit of quantification, robustness and matrix effect. J. Chromatogr. A 2014, 1353:10-27.
30. International Vocabulary of Metrology-Basic and General Concepts and Associated Terms (VIM), JCGM 200:2012.
31. A. Kruve, R. Rebane, K. Kipper, M.-L. Oldekop, H. Evard, K. Herodes, P. Ravio, I. Leito, Tutorial review on validation of liquid chromatography-mass spectrometry methods: Part II Anal. Chim. Acta, . http://dx.doi.org/10.1016/j.aca.2015.02.016.
32. Smith R.D., Loo J.A., Endmonds C.G., Barinaga C.J., Udseth H.R. New developments in biochemical mass spectrometry: electrospray ionization. Anal. Chem. 1990, 62(9):882-899.
33. Cech N.B., Enke C.G. Practical implications of some recent studies in electrospray ionization fundamentals. Mass Spectrom. Rev. 2001, 20:362-387.
34. Kostiainen R., Kotiaho T., Kuuranne T., Auriola S. Liquid chromatography/atmospheric pressure ionization-mass spectrometry in drug metabolism studies. J. Mass Spectrom. 2003, 38(4):357-372.
35. Raffaell A., Saba A. Atmospheric pressure photoionization mass spectrometry. Mass Spectrom. Rev. 2003, 22(5):318-331.
36. Robb D.B., Blades M.W. State-of-the-art in atmospheric pressure photoionization for LC/MS. Anal. Chem. 2008, 627:34-49.
37. Kruve A., Kaupmees K., Liigand J., Leito I. Sodium adduct formation efficiency in ESI source. J. Mass Spectrom. 2013, 48:695-702.
38. Choi B.K., Gusev A.I., Hercules D.M. Postcolumn introduction of an internal standard for quantitative LC-MS analysis. Anal. Chem. 1999, 71:4107-4110.
39. Lagerwerf F.M., van Dongen W.D., Steenvoorden R.J.J.M., Honing M., Jonkman J.H.G. Exploring the boundaries of bioanalytical quantitative LC-MS-MS. Trends Anal. Chem. 2000, 19(7):418-427.
40. Niessen W.M.A., Manini P., Andreoli R. Matrix effects in quantitative pesticide analysis using liquid chromatography-mass spectrometry. Mass Spectrom. Rev. 2006, 25:881-899.
41. Guilbault G.G., Hjelm M. Nomenclature for automated and mechanised analysis. Pure Appl. Chem. 1989, 61:1657-1664.
42. Matuszewski B.K., Constanzer M.L., Chavez-Eng C.M. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Anal. Chem. 2003, 75:3019-3030.
43. Taylor P.J. Matrix effects: the Achilles heel of quantitative high-performance liquid chromatography-electrospray-tandem mass spectrometry. Clin. Biochem. 2005, 38:328-334.
44. Trufelli H., Palma P., Famiglini G., Capiello A. An overview of matrix effects in liquid chromatography-mass spectrometry. Mass Spectrom. Rev. 2011, 30:491-509.
45. Mei H., Hsieh Y., Nardo C., Xu X., Wang S., Ng K., Korfmacher W.A. Investigation of matrix effects in bioanalytical high-performance liquid chromatography/tandem mass spectrometric assays: application to drug discovery. Rapid Commun. Mass Spectrom. 2003, 17:97-103.
46. Alder L., Lüderitz S., Lindtner K., Stan S.-H. The ECHO technique-the more effective way of data evaluation in liquid chromatography-tandem mass spectrometry analysis. J. Chromatogr. A 2004, 1058:67-79.
47. Kruve A., Herodes K., Leito I. Combating matrix effects in LC/ESI/MS: the extrapolative dilution approach. Anal. Chim. Acta 2009, 651:75-80.
48. Kruve A., Leito I. Comparison of different methods aiming to account for/overcome matrix effects in LC/ESI/MS on the example of pesticide analyses. Anal. Methods 2013, 5:3035-3044.
49. Bonfiglio R., King R.C., Olah T.V., Merkle K. The effects of sample preparation methods on the variability of the electrospray ionization response for model drug compounds. Rapid Commun. Mass Spectrom. 1999, 13:1175-1185.
50. Souverain S., Rudaz S., Veuthey J.-L. Matrix effect in LC-ESI-MS and LC-APCI-MS with off-line and on-line extraction procedure. J. Chromatogr. A 2004, 1058:61-66.
51. Dams R., Huestis M.A., Lambert W.E., Murphy C.M. Matrix effect in bio-analysis of illicit drugs with LC-MS/MS: influence of ionization type, sample preparation, and biofluid. J. Am. Soc. Mass Spectrom. 2003, 14:1290-1294.
52. Keski-Rahkonen P., Huhtinen K., Desai R., Harwood D.T., Handelsman D.J., Poutanen M., Auriola S. LC-MS analysis of estradiol in human serum and endometrial tissue: comparison of electrospray ionization, atmospheric pressure chemical ionization and atmospheric pressure photoionization. J. Mass Spectrom. 2013, 48:1050-1058.
53. Ismaiel O.A., Halquist M.S., Elmamly M.Y., Shalaby A., Karnes H.T. Monitoring phospholipids for assessment of ion enhancement and ion suppression in ESI and APCI LC/MS/MS for chlorpheniramine in human plasma and the importance of multiple source matrix effect evaluations. J. Chromatogr. B 2008, 875:333-343.
54. Beltrán E., Ibánez M., Sancho J.V., Hernández F. Determination of patulin in apple and derived products by UHPLC-MS/MS. Study of matrix effects with atmospheric pressure ionisation sources. Food Chem. 2014, 142:400-407.
55. Thurman E.M., Ferrer I., Barcelo D. Choosing between atmospheric pressure chemical ionization and electrospray ionization interfaces for the HPLC/MS analysis of pesticides. Anal. Chem. 2001, 73:5441-5449.
56. Kloepfer A., Quintana J.B., Reemtsma T. Operational options to reduce matrix effects in liquid chromatography-electrospray ionization-mass spectrometry analysis of aqueous environmental samples. J. Chromatogr. A 2005, 1067:153-160.
57. Chambers E., Wagrowski-Diehl D.M., Lu Z., Mazzeo J.R. Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses. J. Chromatogr. B 2007, 852:22-34.
58. Sancho J.V., Pozo O.J., Lopez F.J., Hernandez F. Different quantitation approaches for xenobiotics in human urine samples by liquid chromatography/electrospray tandem mass spectrometry. Rapid Commun. Mass Spectrom. 2002, 16:639-645.
59. Garcia-Valcarcel A.I., Tadeo J.L. A combination of ultrasonic assisted extraction with LC-MS/MS for the determination of organophosphorus pesticides in sludge. Anal. Chim. Acta 2009, 641:117-123.
60. Stahnke H., Kittlaus S., Kempe G., Alder L. Reduction of matrix effects in liquid chromatography-electrospray ionization-mass spectrometry by dilution of the sample extracts: how much dilution is needed?. Anal. Chem. 2012, 84:1474-1484.
61. Zrostlikova J., Hajšlova J., Pouska J., Begany P. Alternative calibration approaches to compensate the effect of co-extracted matrix components in liquid chromatography-electrospray ionisation tandem mass spectrometry analysis of pesticide residues in plant materials. J. Chromatogr. A 2002, 973:13-26.
62. Kaufmann A., Butcher P. Segmented post-column analyte addition; a concept for continuous response control of liquid chromatography/mass spectrometry peaks affected by signal suppression/enhancement. Rapid Commun. Mass Spectrom. 2005, 19(5):611-617.
63. Murray K.K., Boyd R.K., Eberlin M.N., Langley G.J., Li L., Naito Y. Definitions of terms relating to mass spectrometry (IUPAC recommendations 2013). Pure Appl. Chem. 2013, 85(7):1515-1609.
64. Singleton A. Recent advances in bioanalytical sample preparation for LC-MS analyses. Bioanalysis 2012, 4(9):1123-1140.
65. Tan A., Hussain S., Musuku A., Masse R. Internal standard response variations during incurred sample analysis by LC-MS/MS: case by case trouble-shooting. J. Chromatogr. B 2009, 877(27):3201-3209.
66. Peters F.T., Drummer O.H., Musshoff F. Validation of new methods. Forensic Sci. Int. 2007, 165:216-224.
67. SANCO/12571/2013, Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. 2013.
68. European Commission Decision 2002/657/EC implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results, Off. J. Eur. Commun. L221 (2002) 8-36.
69. Miller E.I., Wylie F.M., Oliver J.S. Simultaneous detection and quantification of amphetamines, diazepam and its metabolites cocaine and its metabolites, and opiates in hair by LC-ESI-MS-MS using a single extraction method. J. Anal. Toxicol. 2008, 32:457-469.
70. Ramani A.V., Sengupta P., Mullangi R. Development and validation of a highly sensitive and robust LC-ESI-MS/MS method for simultaneous quantitation of simvastatin acid, amlodipine and valsartan in human plasma: application to a clinical pharmacokinetic study. Biomed. Chromatogr. 2009, 23:615-622.
71. Feng J., Yang X.-W., Huang R.-B., Zhang H.-Y., He M., Huang Q.-C. Development and validation of an LC-ESI-MS/MS method for the determination of nitidine chloride in rat plasma. J. Chromatogr. B 2012, 887-888:43-47.
72. Beyer J., Peters F.T., Kraemer T., Maurer H. Detection and validated quantification of nine herbal phenalkylamines and methcathinone in human blood plasma by LC-MS/MS with electrospray ionization. J. Mass Spectrom. 2007, 42:150-160.
73. Gupta A., Singhal P., Shrivastav P.S., Sanyal M. Application of a validated ultra performance liquid chromatography-tandem mass spectrometry method for the quantification of darunavir in human plasma for a bioequivalence study in Indian subjects. J. Chromatogr. B 2011, 879:2443-2453.
74. Mistri H.N., Jangid A.G., Pudage A., Gomes N., Sanyal M., Shrivastav P. High throughput LC-MS/MS method for simultaneous quantification of lamivudine, stavudine and nevirapine in human plasma. J. Chromatogr. B 2007, 879:320-332.
75. Schröder H.F., Gebhardt W., Thevis M. Anabolic doping, and lifestyle drugs, and selected metabolites in wastewater-detection, quantification, and behaviour monitored by high-resolution MS and MSn before and after sewage treatment. Anal. Bioanal. Chem. 2010, 398:1207-1229.
76. Yeniceli D., Sener E., Korkmaz O.T., Dogrukol-Ak D., Tuncel N. A simple and sensitive LC-ESI-MS (ion trap) method for the determination of bupropion and its major metabolite, hydroxybupropion in rat plasma and brain microdialysates. Talanta 2011, 84:19-26.
77. Gomes F.P., García P.L., Alves J.M.P., Singh A.K., Kedor-Hackmann E.R.M., Santoro M.I.R.M. Development and validation of stability-indicating HPLC methods for quantitative determination of pravastatin fluvastatin, atorvastatin, and rosuvastatin in pharmaceuticals. Anal. Lett. 2009, 42:1784-1804.
78. Calbiani F., Careri M., Elviri L., Mangia A., Pistara L., Zagnoni I. Development and in-house validation of a liquid chromatography-electrospray-tandem mass spectrometry method for the simultaneous determination of Sudan I, Sudan II Sudan III and Sudan IV in hot chilli products. J. Chromatogr. A 2004, 1042:123-130.
79. Angioni A., Porcu L., Pirisi F. LC/DAD/ESI/MS Method for the determination of imidacloprid thiacloprid, and spinosad in olives and olive oil after field treatment. J. Agric. Food Chem. 2011, 59:11359-11366.
80. Ascari J., Dracz S., Santos F.A., Lima J.A., Diniz M.H.G., Vargas E.A. Validation of an LC-MS/MS method for malachite green (MG) leucomalachite green (LMG), crystal violet (CV) and leucocrystal violet (LCV) residues in fish and shrimp. Food Addit. Contam. 2012, 29:602-608.
81. Careri M., Corradini C., Elviri L., Nicoletti I., Zagnoni I. Liquid chromatography-electrospray tandem mass spectrometry of cis-resveratrol and trans-resveratrol: development, validation, and application of the method to red wine, grape, and winemaking byproducts. J. Agric. Food Chem. 2004, 52:6868-6874.
82. Smienk H.G.F., Calvo D., Razquin P., Domínguez E., Mata L. Single laboratory validation of a ready-to-use phosphatase inhibition assay for detection of okadaic acid toxins. Toxins 2012, 4:339-351.
83. Cordero B., Canale F., Del Rio D., Bicchi C. Identification quantitation,and method validation for flavan-3-ols in fermented ready-to-drink teas from the Italian market using HPLC-UV/DAD and LC-MS/MS. J. Sep. Sci. 2009, 32:3643-3651.
84. Giron A.J., Deventer K., Van Eenoo P. Development and validation of an open screening method for diuretics, stimulants and selected compounds in human urine by UHPLC-HRMS for doping control. Anal. Chim. Acta 2012, 721:137-146.
85. Mattarozzi M., Milioli M., Cavalieri C., Bianchi F., Careri M. Rapid desorption electrospray ionization-high resolution mass spectrometry method for the analysis of melamine migration from melamine tableware. Talanta 2012, 10:453-459.
86. Montoro P., Maldini M., Russo M., Postorino S., Piacente S., Pizza C. Metabolic profiling of roots of liquorice (Glycyrrhiza glabra) from different geographical areas by ESI/MS/MS and determination of major metabolites by LC-ESI/MS and LC-ESI/MS/MS. J. Pharm. Biomed. Anal. 2011, 54:535-544.
87. Rumpler M.J. Quantitative analysis of 11-nor-9-carboxy-tetrahydrocannbinol(THC-COOH) in urine by LC-MS/MS following a simple filtration. J. Chromatogr. B 2014, 957:77-83.
88. Venisse N., Grignon C., Brunet B., Thévenot S., Bacle A., Migeot V., Dupuis A. Reliable quantification of bisphenol A and its chlorinated derivatives in human urine using UPLC-MS/MS method. Talanta 2014, 125:284-292.
89. Ediage E.N., Di Mavungu J.D., Monbaliu S., Van Peteghem C., De Saeger S. A validated multianalyte LC-MS/MS method for quantification of 25 mycotoxins in cassava flour, peanut cake and maize samples. J. Agric. Food Chem. 2011, 9:5173-5180.
90. Utture S.C., Banerjee K., Dasgupta S., Patil S.H., Jadhav M.R., Wagh S.S., Kolekar S.S., Anuse M.A., Adsule P.G. Dissipation and Distribution Behavior of Azoxystrobin, Carbendazim, and Difenoconazole in Pomegranate Fruits. J. Agric. Food Chem. 2011, 59:7866-7873.
91. De Zan M.M., Cámara M.S., Robles J.C., Kergaravat S.V., Goicoechea H.C. Development and validation of a simple stability-indicating high performance liquid chromatographic method for the determination of miconazole nitrate in bulk and cream formulations. Talanta 2009, 79:762-767.
92. Kmelláŕ C., Fodor P., Pareja L., Ferrer C., Martínez-Uroz M.A., Valverde A., Fernandez-Alba A.R. Validation and uncertainty study of a comprehensive list of 160 pesticide residues in multi-class vegetables by liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 2008, 1215:37-50.
93. Yánez K.P., Martin M.T., Bernal J.L., Nozal M.J., Bernal J. Determination of spinosad at trace levels in bee pollen and beeswax with solid-liquid extraction and LC-ESI-MS. J. Sep. Sci. 2014, 37:204-210.
94. Rao R.N., Maurya P.K., Ramesh M., Srinivas R., Agwane S.B. Development of a validated high-throughput LC-ESI-MS method for determination of sirolimus on dried blood spots. Biomed. Chromatogr. 2010, 24:1356-1364.
95. Bogusz M.J., Hassan H., Al-Enazi E., Ibrahim Z., Al-Tufail M. Application of LC-ESI-MS-MS for detection of synthetic adulterants in herbal remedies. J. Pharm. Biomed. Anal. 2006, 41:554-564.
96. Yamaguchi H., Fujikawa A., Ito H., Tanaka T., Furugen A., Miyamori K., Takahashi N., Ogura J., Kobayashi M., Yamada T., Mano N., Iseki K. A rapid and sensitive LC/ESI-MS/MS method for quantitative analysis of docetaxel in human plasma and its application to a pharmacokinetic study. J. Chromatogr. B 2012, 893-894:157-161.
97. Claus A., Weisz G.M., Kammerer D.R., Carle R., Schieber A. A method for the determination of acrylamide in bakery products using ion trap LC-ESI-MS/MS. Mol. Nutr. Food Res. 2005, 49:918-925.
98. Gros M., Petrović M., Barceló D. Development of a multi-residue analytical methodology based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for screening and trace level determination of pharmaceuticals in surface and wastewaters. Talanta 2006, 70:678-690.
99. Sannino A., Bolzoni L., Bandini M. Application of liquid chromatography with electrospray tandem mass spectrometry to the determination of a new generation of pesticides in processed fruits and vegetables. J. Chromatogr. A 2004, 1036:161-169.
100. Wang J. Determination of Five Macrolide Antibiotic Residues in Honey by LC-ESI-MS and LC-ESI-MS/MS. J. Agric. Food Chem. 2004, 52:171-181.
101. Shabir G.A., Lough W.J., Arain S.A., Bradshaw T.K. Evaluation and application of best practice in analytical method validation. J. Liq. Chromatogr. Relat. Technol. 2007, 20:311-333.
102. Rozet E., Ceccato A., Hubert C., Ziemons E., Oprean R., Rudaz S., Boulanger B., Hubert P. Analysis of recent pharmaceutical regulatory documents on analytical method validation. J. Chromatogr A. 2007, 1158:111-125.
103. IUPAC, Compendium of Chemical Terminology, 2nd ed., (the Gold Book). Compiled by A.D. McNaught, A. Wilkinson. Blackwell Scientific Publications, Oxford (1997). XML on-line corrected version: (2006-) created by M. Nic, J. Jirat, B. Kosata, updates compiled by A. Jenkins. ISBN 0-9678550-9-8. doi:10.1351/goldbook, last update: 24-02-2014; version: 2.3.3. http://goldbook.iupac.org.
104. Anagnostopoulos C.J., Aplada Sarli P., Liapis K., Haroutounian S.A., Miliadis G.E. Validation of two variations of the QuEChERS method for the determination of multiclass pesticide residues in cereal-based infant foods by LC-MS/MS. Food Anal. Method 2012, 5:664-683.
105. Richardson S.D. Environmental mass spectrometry: emerging contaminants and current issues. Anal. Chem. 2010, 82(12):4742-4774.
106. Diaz R., Ibáñez M., Sancho J.V., Hernández F. Qualitative validation of a liquid chromatography-quadrupole-time of flight mass spectrometry screening method for organic pollutants in waters. J. Chromatogr. A 2013, 1276:47-57.
107. Nácher-Mestre J., Ibáñez M., Serrano R., Pérez-Sánchez J., Hernández F. Qualitative screening of undesirable compounds from feeds to fish by liquid chromatography coupled to mass spectrometry. J. Agric. Food Chem. 2013, 61(9):2077-2087.
108. Macarthur R., von Holst C. A protocol for the validation of qualitative methods of detection. Anal. Methods 2012, 4:2744-2754.
109. Mol H.G., Zomer P., de Koning M. Qualitative aspects and validation of a screening method for pesticides in vegetables and fruits based on liquid chromatography coupled to full scan high resolution (orbitrap) mass spectrometry. Anal. Bioanal. Chem. 2012, 403(10):2891-2908.
110. Kadar H., Veyrand B., Antignac J.P., Durand S., Monteau F., Le Bizac B. Comparative study of low- versus high-resolution liquid chromatography-mass spectrometric strategies for measuring perfluorinated contaminants in fish. Food Addit. Contam. A 2011, 28(9):1261-1273.
111. Singh R.J., Taylor R.L., Satyanarayana Reddy G., Grebe S.K.G. C-3 Epimers can account for a Significant proportion of total circulating 25-hydroxyvitamin D in infants, complicating accurate measurement and interpretation of vitamin D status. J. Clin. Endocr. Metab. 2006, 91(8):3055-3061.
112. Gentili A., Caretti F., Bellante S., Rocca L.M., Curini R., Venditti A. Development and validation of two multiresidue liquid chromatography tandem mass spectrometry methods based on a versatile extraction procedure for isolating non-steroidal anti-inflammatory drugs from bovine milk and muscle tissue. Anal. Bioanal. Chem. 2012, 404:1375-1388.
113. Domenech A., Cortes-Francisco N., Palacios O., Franco J.M., Riobo P., Lierena J.J., Vichi S., Caixach J. Determination of lipophilic marine toxins in mussels. Quantification and confirmation criteria using high resolution mass spectrometry. J. Chromatogr. A 2014, 1328:16-25.
114. Pozo Ó.J., Sancho J.V., Ibáñez M., Hernández F., Niessen W.M.A. Confirmation of organic micropollutants detected in environmental samples by liquid chromatography tandem mass spectrometry: achievements and pitfalls. TrAC Trends Anal Chem. 2006, 25(10):1030-1042.
115. Bethem R., Boison J., Gala J., Heller D., Lehotay S., Loo J., Musser S., Price P., Stein S. Establishing the fitness for purpose of mass spectrometric methods. J. Am. Soc. Mass Spectrom. 2003, 14:528-541.
116. Van Leeuwen J.A., Buydens L.M.C., Vandeginste B.G.M., Kateman G., Schoenmakers P.J., Mulholland M. RES, an expert system for the set-up and interpretation of a ruggedness test in HPLC method validation. Part 1: the ruggedness test in HPLC method validation. Chemom. Intell. Lab. Syst. 1991, 10:337-347.
117. Karageorgou E., Samanidou V. Youden test application in robustness assays during method validation. J. Chromatogr. A 2014, 65:234-240.
118. Youden W.J., Steiner E.H. Statistical manual of the association of official. Anal. Chem. 1975, 50-55.
119. Boque R., Maroto A., Riu J., Rius X. Validation of analytical methods. Grasas Aceites 2002, 53(1):128-143.
120. Heyden V.V., Nijhuis A., Smeyers-Verbeke J., Vandeginste B.G.M., Massart D.L. Guidance for robustness/ruggedness tests in method validation. J. Pharm. Biomed. Anal. 2001, 24:723-753.
121. Cuadros-Rodriguez L., Romero R., Bosque-Sendra J.M. Studies in research and development of analytical processes. Crit. Rev. Anal. Chem. 2005, 35(1):57-69.
122. Caporal-Gautier J., Nivet J.M., Algranti P., Guilloteau M., Histe M., Lallier M., N'Guyen-Huu J.J., Russotto R. Guide de validation analytique, rapport d'une commission SFSTP. S. T. P. Pharma. Pratiques 1992, 2:205-239.
123. The United States Pharmacopeia, 23rd ed., National Formulary 18, United States Pharmacopeial Convention, Rockville, USA, 1995.
124. The United States Pharmacopeia, 35th ed., Rockville, The United States Pharmacopeial Convention, Inc., 2012, 3261-3279.
125. Aguilera E., Lucena R., Cardenas S., Valcarcel M., Trullols E., Ruisanchez I. Robustness in qualitative analyses: a practical approach. Trac-Trend Anal. Chem. 2006, 25(6):621-627.
126. Sundström B., Johansson G., Kokkonen H., Cederholm T., Wållberg-Jonsson S. Plasma phospholipid fatty acid content is related to disease activity in ankylosing spondylitis. J. Rheumatol. 2012, 39:327-333.
127. Thiébaut A.C., Rotival M., Gauthier E., Lenoir G.M., Boutron-Ruault M.C., Joulin V., Clavel-Chapelon F., Chajès V. Correlation between serum phospholipid fatty acids and dietary intakes assessed a few years earlier. Nutr. Cancer 2009, 61:500-509.
128. Childs C.E., Romeu-Nadal M., Burdge G.C., Calder P.C. The polyunsaturated fatty acid composition of hepatic and plasma lipids differ by both sex and dietary fat intake in rats. J. Nutr. 2010, 140:245-250.
129. Bastos-Amador P., Royo F., Gonzalez E., Conde-Vancells J., Palomo-Diez L., Borras F.E., Falcon-Perez J.M. Proteomic analysis of microvesicles from plasma of healthy donors reveals high individual variability. J. Proteomics 2012, 75:3574-3584.
130. Dasenaki M.E., Thomaidis N.S. Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LC-ESI-MS/MS approach based on advanced mass spectrometric techniques. Anal. Chim. Acta 2010, 672:93-102.
131. Dejaegher B., Capron X., Smeyers-Verbeke J., Vander Heyden Y. Randomization tests to identify significant effects in experimental design for robustness testing. Anal. Chim. Acta 2006, 564:184-200.
132. Plackett R.L., Burman J.P. The design of optimum multifactorial experiments. Biometrica 1946, 33(4):305-325.
133. Vander Heyden Y., Luypaert K., Hartmann C., Massart D.L., Hoogmartens J., De Beer J. Ruggedness tests on the high-performance liquid chromatography assay of the United States Pharmacopeia XXII for tetracycline hydrochloride. A comparison of experimental designs and statistical interpretations. Anal. Chim. Acta 1995, 312:245-262.
134. Vander Heyden Y., Hartmann C., Massart D.L., Hollands A.M.J., Nuyten P., Schoenmakers P. Ruggedness testing of a size-exclusion chromatographic assay for low-molecular-mass polymers. J. Chromatogr. A 1996, 756(1):89-106.
135. Dejaegher B., Vander Heyden Y. Ruggedness and robustness testing. J. Chromatogr. A 2007, 1158:138-157.
136. Benetti C., Piro R., Binato G., Angeletti R., Biancotto G. Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry (LC-MS/MS). Food Addit. Contam. 2006, 23(11):1099-1108.
137. Jedziniak P., Szprengier-Juszkiewicz T., Olejnik M. Determination of benzimidazoles and levamisole residues in milk by liquid chromatography-mass spectrometry: screening method development and validation. J. Chromatogr. A 2009, 1216:8165-8172.
138. Zeleny R., Harbeck S., Schimmel H. Validation of a liquid chromatography-tandem mass spectrometry method for the identification and quantification of 5-nitroimidazole drugs and their corresponding hydroxy metabolites in lyophilised pork meat. J. Chromatogr. A 2009, 1216:249-256.
139. Gasparini M., Curatolo M., Assini W., Bozzoni E., Tognoli N., Dusi G. Confirmatory method for the determination of nandrolone and trenbolone in urine samples using immunoaffinity cleanup and liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 2009, 1216:8059-8066.
140. Lopes C.C.G.O., Salgado H.R.N. Development of a validated stability-indicating LC assay and stress degradation studies of linezolid in tablets. Chromatographia 2009, 69:S129-S135.
141. Kaul N., Agrawal H., Paradkar A.R., Mahadik K.R. The ICH guidance in practice: stress degradation studies on indinavir sulphate and development of a validated specific stability-indicating HPTLC assay method. Il Farmaco 2004, 59:729-738.
142. Junior L.B., Uchoa F.T., Guterres S.S., Costa T.D. Development and validation of LC-MS/MS method for the simultaneous determination of quinine and doxycycline in pharmaceutical formulations. J. Liq. Chromatogr. Relat. Technol. 2009, 1:2699-2711.
143. Yardimci C., Özalti{dotless}n N. Method development and validation for the simultaneous determirnation of rosiglitazone and metformin in pharmaceutical preparations by capillary zone electrophoresis. Anal. Chim. Acta 2005, 549:88-95.
144. Thomas S., Shandilya S., Bharati A., Paul S.K., Agarwal A., Mathela C.S. Identification, characterization and quantification of new impurities by LC-ESI/MS/MS and LC-UV methods in rivastigmine tartrate active pharmaceutical ingredient. J. Pharm. Biomed. Anal. 2012, 57:39-51.
145. von Holst C., Müller A., Björklund E., Anklam E. In-house validation of a simplified method for the determination of PCBs in food and feedingstuffs. Eur. Food Res. Technol. 2001, 213:154-160.
146. Épshtein N.A. Validation of HPLC techniques for pharmaceutical analysis. Pharm. Chem. J. 2004, 38:212-228.
147. Mirza T., Tan H.S.I. Determination of captopril in pharmaceutical tablets by anion-exchange HPLC using indirect photometric detection; a study in systematic method development. J. Pharm. Biomed. Anal. 2001, 25(1):39-52.
148. Szekely G., Henriques B., Gil M., Alvarez C. Experimental design for the optimization and robustness testing of a liquid chromatography tandem mass spectrometry method for the trace analysis of the potentially genotoxic 1,3-diisopropylurea. Drug Test. Anal. 2014, 6:898-908.
149. Calbiani F., Careri M., Elviri L., Mangia A., Zagnoni I. Validation of an ion-pair liquid chromatography-electrospray-tandem mass spectrometry method for the determination of heterocyclic aromatic amines in meat-based infant foods. Food Addit. Contam. 2007, 24(8):833-841.
150. Currie L.A. Limits for qualitative detection and quantitative determination. Anal. Chem. 1968, 40:586-593.
151. Evard H., Kruve A., Leito I. LoD determination in LC/MS/MS: choosing the appropriate methodology and comparability of the results. J. Chromatogr. A 2015, submitted for publication.
152. Fonollosa J., Vergara A., Huerta R., Marco S. Estimation of the limit of detection using information theory measures. Anal. Chim. Acta 2014, 810:1-9.
153. Huber W. Basic calculations about the limit of detection and its optimal determination. Accred. Qual. Assur. 2003, 8:213-217.
154. Lindegardh N., Hanpithakpong W., Wattanagoon Y., Singhasivanon P., White N.J., Day N.P.J. Development and validation of a liquid chromatographic-tandem mass spectrometric method for determination of oseltamivir and its metabolite oseltamivir carboxylate in plasma, saliva and urine. J. Chromatogr. B 2007, 859:74-78.
155. Currie L.A. Nomenclature in evaluation of analytical methods including detection and quantification capabilities. Pure Appl. Chem. 1995, 67:1699-1723.
156. Directive 2000/60/EC of the European Parliament and of the Council establishing a framework for Community action in the field of water policy, CELEX-EUR. Off. J. L 327 (2000) 1-72.
157. ISO 11843-6:2013 Capability of detection - Part 6: Methodology for the determination of the critical value and the minimum detectable value in Poisson distributed measurements by normal approximations.
158. Szilagyi S., de la Calle B. Development and validation of an analytical method for the determination of semicarbazide in fresh egg and in egg powder based on the use of liquid chromatography tandem mass spectrometry. Anal. Chim. Acta 2006, 572:113-120.
159. Rokka M., Peltonen K. Simultaneous determination of four coccidiostats in eggs and broiler meat: validation of an LC-MS/MS method. Food Addit. Contam. 2006, 23:470-478.