Single-column high-performance liquid chromatographic-fluorescence detection of immature, mature, and senescent cross-links of collagen

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Saito, Mitsuru¹; Marumo, Keishi¹; Fujii, Katsuyuki¹; Ishioka, Noriaki²

Single-column high-performance liquid chromatographic-fluorescence detection of immature, mature, and senescent cross-links of collagen

Anal Ciochem. November 1, 1997;253(1):26-32

©1997 Academic Press.

Affiliations

¹Department of Orthopaedic Surgery, Jikei University School of Medicine, 3-25-8 Nishi-Shinbashi, Minato-ku, Tokyo, 105, Japan

²Division of Molecular Cell Biology, Institute of DNA Medicine, Jikei University School of Medicine, 3-25-8 Nishi-Shinbashi, Minato-ku, Tokyo, 105, Japan
Abstract

A high-performance liquid chromatographic-fluorescence detection method of reducible (immature) and nonreducible (mature and senescent) cross-links of collagen was established without the use of a radioisotope and preliminary fractionation step. This method used a gradient elution procedure of sodium citrate buffer containing 7% ethanol. The reducible cross-links (dihydroxylysinonorleucine, hydroxylysinonorleucine, and lysinonorleucine) and nonreducible cross-link (histidinohydroxylysinonorleucine) were detected by O-phthalaldehyde derivatization with the postcolumn method, whereas other nonreducible cross-links (pyridinoline, deoxypyridinoline, and pentosidine) were detected by natural fluorescence. The linear ranges of contents of the O-phthalaldehyde derivative cross-links and the natural fluorescent nonreducible cross-links were 20-600, 5-500 (pyridinoline, deoxypyridinoline), and 0.2-20 pmol (pentosidine), respectively. Tissue containing 1-2 mg dry wt of collagen was adequate for duplicate analyses of the reducible and nonreducible cross-links. An equivalent of 0.25 mg of hydrolyzed collagen could be analyzed by this HPLC system. Using this system, age-related changes in the cross-links of collagen from human connective tissues were also investigated.
Links

DOI: 10.1006/abio.1997.2350

PubMed: 9356137

WoS: A1997YH04400005
History

Received: 1997-05-28

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2006	Saito M, Fujii K, Soshi S, Tanaka T. Reductions in degree of mineralization and enzymatic collagen cross-links and increases in glycation-induced pentosidine in the femoral neck cortex in cases of femoral neck fracture. Osteoporos Int. July 2006;17(7):986-995.
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2008	Saito M, Mori S, Mashiba T, Komatsubara S, Marumo K. Collagen maturity, glycation induced-pentosidine, and mineralization are increased following 3-year treatment with incadronate in dogs. Osteoporos Int. September 2008;19(9):1343-1354.
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2020	Arakawa S, Suzuki R, Kurosaka D, Ikeda R, Hayashi H, Kayama T, Ohno R-i, Nagai R, Marumo K, Saito M. Mass spectrometric quantitation of AGEs and enzymatic crosslinks in human cancellous bone. Sci Rep. 2020;10:18774.
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