High contrast tumor imaging with radio-labeled antibody Fab fragments tailored for optimized pharmacokinetics via PASylation

mAbs

Volumn 7, Issue 1, 2015, Pages 96-109

  Mendler, Claudia T ^a,b   Friedrich, Lars ^a   Laitinen, Iina ^b   Schlapschy, Martin ^a   Schwaiger, Markus ^b   Wester, Hans Jürgen ^a   Skerra, Arne ^a,c  

^a TECHNICAL UNIVERSITY OF MUNICH   (Germany)

^b TECHNICAL UNIVERSITY OF MUNICH   (Germany)

^c XL Protein GmbH   (Germany)

Author keywords

Antibody fragment; CD20; HER2; PEGylation; Plasma half life; Protein tracer

Indexed keywords

ALANINE; CD20 ANTIGEN; EPIDERMAL GROWTH FACTOR RECEPTOR 2; IMMUNOGLOBULIN F(AB) FRAGMENT; OFATUMUMAB; PROLINE; RECOMBINANT IMMUNOGLOBULIN F(AB) FRAGMENT; RECOMBINANT PROTEIN; RITUXIMAB; SERINE; TRASTUZUMAB; UNCLASSIFIED DRUG; CANCER ANTIBODY; ERBB2 PROTEIN, HUMAN; IODINE;

ANIMAL EXPERIMENT; ANIMAL MODEL; ANIMAL TISSUE; ANTIGEN BINDING; ARTICLE; BIOENGINEERING; CANCER IMAGING; CONTROLLED STUDY; CYTOFLUOROMETRY; DIAGNOSTIC IMAGING; DRUG DISTRIBUTION; DRUG HALF LIFE; ISOTOPE LABELING; MOUSE; NONHUMAN; PLASMA HALF LIFE; POSITRON EMISSION TOMOGRAPHY; RADIOACTIVITY; TUMOR XENOGRAFT; ANIMAL; CANCER TRANSPLANTATION; CHEMISTRY; FEMALE; GENETICS; HUMAN; METABOLISM; NEOPLASMS, EXPERIMENTAL; PATHOLOGY; TUMOR CELL LINE; XENOGRAFT;

ANIMALS; ANTIBODIES, NEOPLASM; ANTIGENS, CD20; CELL LINE, TUMOR; FEMALE; HETEROGRAFTS; HUMANS; IMMUNOGLOBULIN FAB FRAGMENTS; IODINE ISOTOPES; ISOTOPE LABELING; MICE; NEOPLASM TRANSPLANTATION; NEOPLASMS, EXPERIMENTAL; POSITRON-EMISSION TOMOGRAPHY; RECEPTOR, ERBB-2;

EID: 84921367864     PISSN: 19420862     EISSN: 19420870     Source Type: Journal    
DOI: 10.4161/19420862.2014.985522     Document Type: Article

References (70)

1. Nelson AL, Reichert JM. Development trends for therapeutic antibody fragments. Nat Biotechnol 2009; 27:331-337; PMID:19352366; http://dx.doi.org/ 10.1038/nbt0409-331
2. Reichert JM. Marketed therapeutic antibodies compendium. MAbs 2012; 4:413-415; PMID:22531442; http://dx.doi.org/10.4161/mabs.19931
3. Dimitrov DS, Marks JD. Therapeutic antibodies: current state and future trends-is a paradigm change coming soon? Methods Mol Biol 2009; 525:1-27; PMID:19252861; http://dx.doi.org/10.1007/978-1-59745-554-1-1
4. Witzig TE, Gordon LI, Cabanillas F, Czuczman MS, Emmanouilides C, Joyce R, Pohlman BL, Bartlett NL, Wiseman GA, Padre N, et al. Randomized controlled trial of yttrium-90-labeled ibritumomab tiuxetan radioimmunotherapy versus rituximab immunotherapy for patients with relapsed or refractory low-grade, follicular, or transformed B-cell non-Hodgkin's lymphoma. J Clin Oncol 2002; 20:2453-2463; PMID:12011122; http://dx.doi.org/10.1200/JCO.2002.11.076
5. Slamon DJ, Clark GM, Wong SG, Levin WJ, Ullrich A, McGuire WL. Human breast cancer: correlation of relapse and survival with amplification of the HER-2/ neu oncogene. Science 1987; 235:177-182; PMID:3798106; http://dx.doi.org/10.1126/ science.3798106
6. Scholl S, Beuzeboc P, Pouillart P. Targeting HER2 in other tumor types. Ann Oncol 2001; 12 Suppl 1:S81- S87; PMID:11521727; http://dx.doi.org/10.1093/ annonc/12.suppl-1.S81
7. Carter P, Presta L, Gorman CM, Ridgway JB, Henner D, Wong WL, Rowland AM, Kotts C, Carver ME, Shepard HM. Humanization of an anti-p185HER2 antibody for human cancer therapy. Proc Natl Acad Sci U S A 1992; 89:4285-4289; PMID:1350088; http://dx. doi.org/10.1073/pnas.89.10.4285
8. Baselga J. Clinical trials of Herceptin (trastuzumab). Eur J Cancer 2001; 37 Suppl 1:S18-S24; PMID:11167087; http://dx.doi.org/10.1016/S0959-8049(00)00404-4
9. Dirix LY, Rutten A, Huget P, Dirix M. Trastuzumab emtansine in breast cancer. Expert Opin Biol Ther 2013; 13:607-614; PMID:23477731; http://dx.doi. org/10.1517/14712598.2013.778238
10. Eisenberg R, Looney RJ. The therapeutic potential of anti-CD20: "What do B-cells do?". Clin Immunol 2005; 117:207-213; PMID:16169773; http://dx.doi. org/10.1016/j.clim.2005.08.006
11. Kosmas C, Stamatopoulos K, Stavroyianni N, Tsavaris N, Papadaki T. Anti-CD20-based therapy of B cell lymphoma: state of the art. Leukemia 2002; 16:2004- 2015; PMID:12357351; http://dx.doi.org/10.1038/sj.leu.2402639
12. Lemery SJ, Zhang J, Rothmann MD, Yang J, Earp J, Zhao H, McDougal A, Pilaro A, Chiang R, Gootenberg JE, et al. U.S. Food and Drug Administration approval: ofatumumab for the treatment of patients with chronic lymphocytic leukemia refractory to fludarabine and alemtuzumab. Clin Cancer Res 2010; 16:4331-4338; PMID:20601446; http://dx.doi.org/10.1158/1078-0432.CCR-10-0570
13. Hagenbeek A, Gadeberg O, Johnson P, Pedersen LM, Walewski J, Hellmann A, Link BK, Robak T, Wojtukiewicz M, Pfreundschuh M, et al. First clinical use of ofatumumab, a novel fully human anti-CD20 monoclonal antibody in relapsed or refractory follicular lymphoma: results of a phase 1/2 trial. Blood 2008; 111:5486-5495; PMID:18390837; http://dx.doi.org/10.1182/blood-2007-10-117671
14. Teeling JL, French RR, Cragg MS, van den Brakel J, Pluyter M, Huang H, Chan C, Parren PW, Hack CE, Dechant M, et al. Characterization of new human CD20 monoclonal antibodies with potent cytolytic activity against non-Hodgkin lymphomas. Blood 2004; 104:1793-1800; PMID:15172969; http://dx.doi.org/ 10.1182/blood-2004-01-0039
15. Milenic DE, Brady ED, Brechbiel MW. Antibody-targeted radiation cancer therapy. Nat Rev Drug Discov 2004; 3:488-499; PMID:15173838; http://dx.doi.org/ 10.1038/nrd1413
16. van Dongen GA, Poot AJ, Vugts DJ. PET imaging with radiolabeled antibodies and tyrosine kinase inhibitors: immuno-PET and TKI-PET. Tumour Biol 2012; 33:607-615; PMID:22270450; http://dx.doi.org/ 10.1007/s13277-012-0316-4
17. Dijkers EC, Oude Munnink TH, Kosterink JG, Brouwers AH, Jager PL, de Jong JR, van Dongen GA, Schroder CP, Lub-de Hooge MN, de Vries EG. Biodistribution of 89Zr-trastuzumab and PET imaging of HER2-positive lesions in patients with metastatic breast cancer. Clin Pharmacol Ther 2010; 87:586-592; PMID:20357763; http://dx.doi.org/10.1038/clpt.2010.12
18. Gaykema SB, Brouwers AH, Hovenga S, Lub-de Hooge MN, de Vries EG, Schroder CP. Zirconium- 89-trastuzumab positron emission tomography as a tool to solve a clinical dilemma in a patient with breast cancer. J Clin Oncol 2012; 30:e74-75; PMID:22203768; http://dx.doi.org/10.1200/JCO.2011.38.0204
19. Divgi CR, Pandit-Taskar N, Jungbluth AA, Reuter VE, Gonen M, Ruan S, Pierre C, Nagel A, Pryma DA, Humm J, et al. Preoperative characterisation of clearcell renal carcinoma using iodine-124-labelled antibody chimeric G250 (124I-cG250) and PET in patients with renal masses: a phase I trial. Lancet Oncol 2007; 8:304-310; PMID:17395103; http://dx.doi.org/10.1016/S1470-2045(07)70044-X
20. Lobo ED, Hansen RJ, Balthasar JP. Antibody pharmacokinetics and pharmacodynamics. J Pharm Sci 2004; 93:2645-2668; PMID:15389672; http://dx.doi.org/10.1002/jps.20178
21. Iyer AK, Khaled G, Fang J, Maeda H. Exploiting the enhanced permeability and retention effect for tumor targeting. Drug Discov Today 2006; 11:812-818; PMID:16935749; http://dx.doi.org/10.1016/j.drudis.2006.07.005
22. Wester HJ, Kessler H. Molecular targeting with peptides or peptide-polymer conjugates: just a question of size? J Nucl Med 2005; 46:1940-1945; PMID:16330555
23. Dreher MR, Liu W, Michelich CR, Dewhirst MW, Yuan F, Chilkoti A. Tumor vascular permeability, accumulation, and penetration of macromolecular drug carriers. J Natl Cancer Inst 2006; 98:335-344; PMID:16507830; http://dx.doi.org/10.1093/jnci/djj070
24. Wu AM, Senter PD. Arming antibodies: prospects and challenges for immunoconjugates. Nat Biotechnol 2005; 23:1137-1146; PMID:16151407; http://dx.doi.org/10.1038/nbt1141
25. Holliger P, Hudson PJ. Engineered antibody fragments and the rise of single domains. Nat Biotechnol 2005; 23:1126-1136; PMID:16151406; http://dx.doi.org/ 10.1038/nbt1142
26. Kenanova V, Wu AM. Tailoring antibodies for radionuclide delivery. Expert Opin Drug Deliv 2006; 3:53- 70; PMID:16370940; http://dx.doi.org/10.1517/17425247.3.1.53
27. Dennis MS, Jin H, Dugger D, Yang R, McFarland L, Ogasawara A, Williams S, Cole MJ, Ross S, Schwall R. Imaging tumors with an albumin-binding Fab, a novel tumor-targeting agent. Cancer Res 2007; 67:254-261; PMID:17210705; http://dx.doi.org/10.1158/0008-5472.CAN-06-2531
28. Thurber GM, Zajic SC, Wittrup KD. Theoretic criteria for antibody penetration into solid tumors and micrometastases. J Nucl Med 2007; 48:995-999; PMID:17504872; http://dx.doi.org/10.2967/jnumed.106.037069
29. Baker K, Qiao SW, Kuo T, Kobayashi K, Yoshida M, Lencer WI, Blumberg RS. Immune and non-immune functions of the (not so) neonatal Fc receptor, FcRn. Semin Immunopathol 2009; 31:223-236; PMID:19495758; http://dx.doi.org/10.1007/s00281- 009-0160-9
30. Chaudhury C, Mehnaz S, Robinson JM, Hayton WL, Pearl DK, Roopenian DC, Anderson CL. The major histocompatibility complex-related Fc receptor for IgG (FcRn) binds albumin and prolongs its lifespan. J Exp Med 2003; 197:315-322; PMID:12566415; http://dx.doi.org/10.1084/jem.20021829
31. Stehle G, Sinn H, Wunder A, Schrenk HH, Stewart JC, Hartung G, Maier-Borst W, Heene DL. Plasma protein (albumin) catabolism by the tumor itself - implications for tumor metabolism and the genesis of cachexia. Crit Rev Oncol Hematol 1997; 26:77-100; PMID:9298326; http://dx.doi.org/10.1016/S1040-8428(97)00015-2
32. Merlot AM, Kalinowski DS, Richardson DR. Unraveling the mysteries of serum albumin-more than just a serum protein. Front Physiol 2014; 5:299; PMID:25161624; http://dx.doi.org/10.3389/fphys.2014.00299
33. Pasut G, Veronese FM. State of the art in PEGylation: the great versatility achieved after forty years of research. J Control Release 2012; 161:461-472; PMID:22094104; http://dx.doi.org/10.1016/j.jconrel.2011.10.037
34. Zahnd C, Kawe M, Stumpp MT, de Pasquale C, Tamaskovic R, Nagy-Davidescu G, Dreier B, Schibli R, Binz HK, Waibel R, et al. Efficient tumor targeting with high-affinity designed ankyrin repeat proteins: effects of affinity and molecular size. Cancer Res 2010; 70:1595-1605; PMID:20124480; http://dx.doi.org/ 10.1158/0008-5472.CAN-09-2724
35. Kubetzko S, Balic E, Waibel R, Zangemeister-Wittke U, Plückthun A. PEGylation and multimerization of the anti-p185HER-2 single chain Fv fragment 4D5. Effects on tumor targeting. J Biol Chem 2006; 281:35186-35201; PMID:16963450; http://dx.doi.org/10.1074/jbc.M604127200
36. Schlapschy M, Binder U, Börger C, Theobald I, Wachinger K, Kisling S, Haller D, Skerra A. PASylation: a biological alternative to PEGylation for extending the plasma half-life of pharmaceutically active proteins. Protein Eng Des Sel 2013; 26:489-501; PMID:23754528; http://dx.doi.org/10.1093/protein/ gzt023
37. Binder U, Skerra A. Half-life extension of therapeutic proteins via genetic fusion to recombinant PEG mimetics. In: Kontermann R, ed. Therapeutic Proteins - Strategies to Modulate Their Plasma Half-lives. Weinheim, Germany: Wiley-VCH, 2012:63-80.
38. Du J, Yang H, Guo Y, Ding J. Structure of the Fab fragment of therapeutic antibody Ofatumumab provides insights into the recognition mechanismwith CD20. Mol Immunol 2009; 46:2419-2423; PMID:19427037; http://dx.doi.org/10.1016/j.molimm.2009.04.009
39. McKeage K, Perry CM. Trastuzumab: a review of its use in the treatment of metastatic breast cancer overexpressing HER2. Drugs 2002; 62:209-243; PMID:11790161; http://dx.doi.org/10.2165/00003495-200262010-00008
40. Schlapschy M, Theobald I, Mack H, Schottelius M, Wester HJ, Skerra A. Fusion of a recombinant antibody fragment with a homo-amino-acid polymer: effects on biophysical properties and prolonged plasma half-life. Protein Eng Des Sel 2007; 20:273-284; PMID:17595342; http://dx.doi.org/10.1093/protein/gzm020
41. Gerstner RB, Carter P, Lowman HB. Sequence plasticity in the antigen-binding site of a therapeutic anti- HER2 antibody. J Mol Biol 2002; 321:851-862; PMID:12206766; http://dx.doi.org/10.1016/S0022-2836(02)00677-0
42. Schiweck W, Skerra A. Fermenter production of an artificial Fab fragment, rationally designed for the antigen cystatin, and its optimized crystallization through constant domain shuffling. Proteins 1995; 23:561-565; PMID:8749852; http://dx.doi.org/10.1002/prot.340230411
43. Kraulis PJ, Jonasson P, Nygren PA˚, Uhlén M, Jendeberg L, Nilsson B, Kördel J. The serum albumin- binding domain of streptococcal protein G is a three-helical bundle: a heteronuclear NMR study. FEBS Lett 1996; 378:190-194; PMID:8549831; http://dx.doi.org/10.1016/0014-5793(95)01452-7
44. Bandtlow C, Schiweck W, Tai HH, Schwab ME, Skerra A. The Escherichia coli -derived Fab fragment of the IgM/k antibody IN-1 recognizes and neutralizes myelin-associated inhibitors of neurite growth. Eur J Biochem 1996; 241:468-475; PMID:8917444; http://dx.doi.org/10.1111/j.1432-1033.1996.00468.x
45. Holmes WE, Sliwkowski MX, Akita RW, Henzel WJ, Lee J, Park JW, Yansura D, Abadi N, Raab H, Lewis GD, et al. Identification of heregulin, a specific activator of p185erbB2. Science 1992; 256:1205-1210; PMID:1350381; http://dx.doi.org/10.1126/science. 256.5060.1205
46. Rudolph C, Steinemann D, Von Neuhoff N, Gadzicki D, Ripperger T, Drexler HG, Mrasek K, Liehr T, Claussen U, Emura M, et al. Molecular cytogenetic characterization of the mantle cell lymphoma cell line GRANTA-519. Cancer Genet Cytogenet 2004; 153:144-150; PMID:15350304; http://dx.doi.org/10.1016/j.cancergencyto.2004.01.006
47. De Lorenzo C, Tedesco A, Terrazzano G, Cozzolino R, Laccetti P, Piccoli R, D'Alessio G. A human, compact, fully functional anti-ErbB2 antibody as a novel antitumour agent. Br J Cancer 2004; 91:1200-1204; PMID:15305184
48. Uchiyama S, Suzuki Y, Otake K, Yokoyama M, Ohta M, Aikawa S, Komatsu M, Sawada T, Kagami Y, Morishima Y, et al. Development of novel humanized anti- CD20 antibodies based on affinity constant and epitope. Cancer Sci 2010; 101:201-209; PMID:19930155; http://dx.doi.org/10.1111/j.1349-7006.2009.01392.x
49. Fraker PJ, Speck JC, Jr. Protein and cell membrane iodinations with a sparingly soluble chloroamide, 1,3,4,6-tetrachloro-3a,6a-diphenylglycoluril. Biochem Biophys Res Commun 1978; 80:849-857; PMID:637870; http://dx.doi.org/10.1016/0006-291X(78)91322-0
50. Reiners C, Schneider R. Potassium iodide (KI) to block the thyroid from exposure to I-131: current questions and answers to be discussed. Radiat Environ Biophys 2013; 52:189-193; PMID:23475155; http://dx.doi. org/10.1007/s00411-013-0462-0
51. Wyffels L, De Bruyne S, Blanckaert P, Lambert DM, De Vos F. Radiosynthesis, in vitro and in vivo evaluation of 123I-labeled anandamide analogues for mapping brain FAAH. Bioorg Med Chem 2009; 17:49-56; PMID:19054678; http://dx.doi.org/10.1016/j.bmc.2008.11.019
52. Burvenich IJ, Schoonooghe S, Blanckaert P, Bacher K, Vervoort L, Coene E, Mertens N, De Vos F, Slegers G. Biodistribution and planar gamma camera imaging of 123I- and 131I-labeled F(ab0 )2 and Fab fragments of monoclonal antibody 14C5 in nude mice bearing an A549 lung tumor. Nucl Med Biol 2007; 34:257-265; PMID:17383575; http://dx.doi.org/10.1016/j.nucmedbio.2006.12.006
53. Dias CR, Jeger S, Osso JA, Jr, Müller C, De Pasquale C, Hohn A, Waibel R, Schibli R. Radiolabeling of rituximab with (188)Re and (99m)Tc using the tricarbonyl technology. Nucl Med Biol 2011; 38:19-28; PMID:21220126; http://dx.doi.org/10.1016/j.nucmedbio.2010.05.010
54. Goldenberg DM, Juweid M, Dunn RM, Sharkey RM. Cancer imaging with radiolabeled antibodies: new advances with technetium-99m-labeled monoclonal antibody Fab' fragments, especially CEA-Scan and prospects for therapy. J Nucl Med Technol 1997; 25:18-23; quiz 34; PMID:9239599
55. Gratz S, Schipper ML, Dörner J, Höffken H, Becker W, Kaiser JW, Béhé M, Behr TM. LeukoScan for imaging infection in different clinical settings: a retrospective evaluation and extended review of the literature. Clin Nucl Med 2003; 28:267-276; PMID:12642703
56. Lamonica D, Czuczman M, Nabi H, Klippenstein D, Grossman Z. Radioimmunoscintigraphy (RIS) with bectumomab (Tc99m labeled IMMU-LL2, Lymphoscan) in the assessment of recurrent non-Hodgkin's lymphoma (NHL). Cancer Biother Radiopharm 2002; 17:689-697; PMID:12537673; http://dx.doi.org/10.1089/108497802320970307
57. Flanagan RJ, Jones AL. Fab antibody fragments: some applications in clinical toxicology. Drug Saf 2004; 27:1115-1133; PMID:15554746; http://dx.doi.org/ 10.2165/00002018-200427140-00004
58. Schmidt MM, Wittrup KD. A modeling analysis of the effects of molecular size and binding affinity on tumor targeting. Mol Cancer Ther 2009; 8:2861-2871; PMID:19825804; http://dx.doi.org/10.1158/1535-7163.MCT-09-0195
59. Wittrup KD, Thurber GM, Schmidt MM, Rhoden JJ. Practical theoretic guidance for the design of tumor-targeting agents. Methods Enzymol 2012; 503:255-268; PMID:22230572; http://dx.doi.org/10.1016/B978-0-12-396962-0.00010-0
60. Delgado C, Pedley RB, Herraez A, Boden R, Boden JA, Keep PA, Chester KA, Fisher D, Begent RH, Francis GE. Enhanced tumour specificity of an anti-carcinoembrionic antigen Fab' fragment by poly(ethylene glycol) (PEG) modification. Br J Cancer 1996; 73:175-182; PMID:8546903; http://dx.doi.org/10.1038/bjc.1996.32
61. Tolmachev V, Wallberg H, Andersson K, Wennborg A, Lundqvist H, Orlova A. The influence of Bz-DOTA and CHX-A″ -DTPA on the biodistribution of ABD-fused anti-HER2 Affibody molecules: implications for 114mIn-mediated targeting therapy. Eur J Nucl Med Mol Imaging 2009; 36:1460-1468; PMID:19430786; http://dx.doi.org/10.1007/s00259-009-1134-9
62. Smith-Jones PM, Solit DB, Akhurst T, Afroze F, Rosen N, Larson SM. Imaging the pharmacodynamics of HER2 degradation in response to Hsp90 inhibitors. Nat Biotechnol 2004; 22:701-706; PMID:15133471; http://dx.doi.org/10.1038/nbt968
63. Olafsen T, Betting D, Kenanova VE, Salazar FB, Clarke P, Said J, Raubitschek AA, Timmerman JM, Wu AM. Recombinant anti-CD20 antibody fragments for small-animal PET imaging of B-cell lymphomas. J Nucl Med 2009; 50:1500-1508; PMID:19690034; http://dx.doi.org/10.2967/jnumed.108.060426
64. Olafsen T, Sirk SJ, Betting DJ, Kenanova VE, Bauer KB, Ladno W, Raubitschek AA, Timmerman JM, Wu AM. ImmunoPET imaging of B-cell lymphoma using 124I-anti-CD20 scFv dimers (diabodies). Protein Eng Des Sel 2010; 23:243-249; PMID:20053640; http://dx.doi.org/10.1093/protein/gzp081
65. Boswell CA, Marik J, Elowson MJ, Reyes NA, Ulufatu S, Bumbaca D, Yip V, Mundo EE, Majidy N, Van Hoy M, et al. Enhanced tumor retention of a radiohalogen label for site-specific modification of antibodies. J Med Chem 2013; 56:9418-9426; PMID:24131491; http://dx.doi.org/10.1021/jm401365h
66. König T, Skerra A. Use of an albumin-binding domain for the selective immobilisation of recombinant capture antibody fragments on ELISA plates. J Immunol Methods 1998; 218:73-83; PMID:9819124; http://dx.doi.org/10.1016/S0022-1759(98)00112-4
67. Skerra A. A general vector, pASK84, for cloning, bacterial production, and single-step purification of antibody Fab fragments. Gene 1994; 141:79-84; PMID:8163179; http://dx.doi.org/10.1016/0378-1119(94)90131-7
68. Skerra A. Use of the tetracycline promoter for the tightly regulated production of a murine antibody fragment in Escherichia coli. Gene 1994; 151:131-135; PMID:7828861; http://dx.doi.org/10.1016/0378-1119(94)90643-2
69. Schmidt TG, Skerra A. The Strep-tag system for one-step purification and high-affinity detection or capturing of proteins. Nat Protoc 2007; 2:1528-1535; PMID:17571060; http://dx.doi.org/10.1038/nprot.2007.209
70. Gill SC, von Hippel PH. Calculation of protein extinction coefficients from amino acid sequence data. Anal Biochem 1989; 182:319-326; PMID:2610349; http://dx.doi.org/10.1016/0003-2697(89)90602-7