LC–MS/MS application for urine free pyridinoline and free deoxypyridinoline: Urine markers of collagen and bone degradation

Tang, Jonathan; Dutton, John; Piec, Isabelle; Green, Darrell; Fisher, Emily; Washbourne, Christopher; Fraser, William D.

doi:10.1016/j.clinms.2016.08.001

Cited by 15 publications

(14 citation statements)

References 33 publications

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“…A complete 24-h urine collection was conducted at the beginning and end of the intervention, and aliquots were stored at −80°C until analysis. Free pyridinium cross-links in urine were measured by liquid chromatography–tandem mass spectrometry (LC-MS/MS), as described elsewhere ( 12 ). In brief, the LC-MS/MS method quantified free pyridinoline (fPYD) and free deoxypyridinoline (fDPD) simultaneously from a single-sample analysis.…”

Section: Methodsmentioning

confidence: 99%

A Mediterranean-like dietary pattern with vitamin D3 (10 µg/d) supplements reduced the rate of bone loss in older Europeans with osteoporosis at baseline: results of a 1-y randomized controlled trial

Jennings

Cashman

Gillings

et al. 2018

The American Journal of Clinical Nutrition

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BackgroundThe Mediterranean diet (MD) is widely recommended for the prevention of chronic disease, but evidence for a beneficial effect on bone health is lacking.ObjectiveThe aim of this study was to examine the effect of a Mediterranean-like dietary pattern [NU-AGE (New Dietary Strategies Addressing the Specific Needs of the Elderly Population for Healthy Aging in Europe)] on indexes of inflammation with a number of secondary endpoints, including bone mineral density (BMD) and biomarkers of bone and collagen degradation in a 1-y multicenter randomized controlled trial (RCT; NU-AGE) in elderly Europeans.DesignAn RCT was undertaken across 5 European centers. Subjects in the intervention group consumed the NU-AGE diet for 1 y by receiving individually tailored dietary advice, coupled with supplies of foods including whole-grain pasta, olive oil, and a vitamin D3 supplement (10 µg/d). Participants in the control group were provided with leaflets on healthy eating available in their country.ResultsA total of 1294 participants (mean ± SD age: 70.9 ±4.0 y; 44% male) were recruited to the study and 1142 completed the 1-y trial. The Mediterranean-like dietary pattern had no effect on BMD (site-specific or whole-body); the inclusion of compliance to the intervention in the statistical model did not change the findings. There was also no effect of the intervention on the urinary biomarkers free pyridinoline or free deoxypyridinoline. Serum 25-hydroxyvitamin D significantly increased and parathyroid hormone decreased (P < 0.001) in the MD compared with the control group. Subgroup analysis of individuals with osteoporosis at baseline (site-specific BMD T-score ≤ −2.5 SDs) showed that the MD attenuated the expected decline in femoral neck BMD (n = 24 and 30 in MD and control groups, respectively; P = 0.04) but had no effect on lumbar spine or whole-body BMD.ConclusionsA 1-y intervention of the Mediterranean-like diet together with vitamin D3 supplements (10 µg/d) had no effect on BMD in the normal age-related range, but it significantly reduced the rate of loss of bone at the femoral neck in individuals with osteoporosis. The NU-AGE trial is registered at clinicaltrials.gov as NCT01754012.

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Section: Methodsmentioning

confidence: 99%

A Mediterranean-like dietary pattern with vitamin D3 (10 µg/d) supplements reduced the rate of bone loss in older Europeans with osteoporosis at baseline: results of a 1-y randomized controlled trial

Jennings

Cashman

Gillings

et al. 2018

The American Journal of Clinical Nutrition

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“…Analysis for urinary fPYD and fDPD were conducted following the method described by Tang et al [ 15 ]. Human urine pyridinium cross-links calibrator was used from Immundiagnostik (Bensheim, Germany).…”

Section: Methodsmentioning

confidence: 99%

Elevated urinary excretion of free pyridinoline in Friesian horses suggests a breed-specific increase in collagen degradation

et al. 2018

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BackgroundFriesian horses are known for their high inbreeding rate resulting in several genetic diseases such as hydrocephaly and dwarfism. This last decade, several studies focused on two other presumed hereditary traits in Friesian horses: megaoesophagus and aortic rupture. The pathogenesis of these diseases remains obscure but an important role of collagen has been hypothesized. The purpose of this study was to examine possible breed-related differences in collagen catabolism. Urinary specimens from Friesian (n = 17, median age 10 years old) and Warmblood horses (n = 17, median age 10 years old) were assessed for mature collagen cross-links, i.e. pyridinoline (PYD) (=hydroxylysylpyridinoline/HP) and deoxypyridinoline (DPD) (lysylpyridinoline /LP).Solid-phase extraction was performed, followed by reversed-phase ion-paired liquid chromatography prior to tandem mass spectrometry (MS/MS) detection.ResultsMean urinary concentrations of free PYD, expressed as fPYD/creatinine ratio, were significantly higher in Friesian horses compared to Warmblood horses (28.5 ± 5.2 versus 22.2 ± 9.6 nmol/mmol, p = 0.02) while mean fDPD/creatinine ratios were similar in both horse breeds (3.0 ± 0.7 versus 4.6 ± 3.7 nmol/mmol, p = 0.09).ConclusionsSince DPD is considered a specific bone degradation marker and PYD is more widely distributed in connective tissues, the significant elevation in the mean PYD/DPD ratio in Friesian versus Warmblood horses (9.6 ± 1.6 versus 5.7 ± 1.8, p < 0.0001) suggests a soft tissue origin for the increased fPYD levels. Considering that a previous study found no differences in total collagen content between Friesian and Warmblood horses for tendon and aortic tissue, this indicates a higher rate of collagen degradation. The latter might, at least in part, explain the predisposition of Friesians to connective tissue disorders.

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“…Furthermore, a more sensitive method for PYR and DPYD quantitation was obtained using RP LC‐MS. However, an ion‐pairing agent is essential for PYR and DPYR column retention .…”

Section: Introductionmentioning

confidence: 99%

“…Using the above methods, both free and collagen‐bound PYR and DPYR were measured in urine samples which are biomarkers for several bone diseases . A thorough search of the literature reveals that all the existing RP‐HPLC and LC‐MS methods require strong ion pairing agents to be added to the mobile phase to solve the poor column retention of the hydrophilic PYR and DPYR compounds . The two most common ion pairing agents are heptafluorobutyric acid and 1‐octanesulfonic acid, however, both are known to suppress the ESI resulting in significant loss of sensitivity .…”

Section: Introductionmentioning

confidence: 99%

Rapid analysis of pyridinoline and deoxypyridinoline in biological samples by liquid chromatography with mass spectrometry and a silica hydride column

Naffa

Watanabe

Zhang

et al. 2019

J of Separation Science

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Pyridinoline and deoxypyridinoline crosslinks are biomarkers found in urine for collagen degradation in bone turnover. For the first time, a rapid, sensitive, and ionpairing free method is described for the analysis of pyridinoline and deoxypyridinoline using ultra-high performance liquid chromatography with Cogent Diamond Hydride column and detection by Q Exactive hybrid quadrupole-orbitrap high resolution accurate mass spectrometry. The separation was achieved using both isocratic and gradient conditions and run time <5 min under isocratic conditions of 20% acetonitrile in water containing 0.1% formic acid. Pyridoxine was used as an internal standard and relative standard deviation of the retention times of both pyridinoline and deoxypyridinoline were <1%. The limit of detection was 0.082 ± 0.023 μM for pyridinoline and 0.118 ± 0.052 μM for deoxypyridinoline. The limit of quantitation was 0.245 ± 0.070 μM for pyridinoline and 0.354 ± 0.157 μM for deoxypyridinoline. The method was validated by the detection and quantitation of both pyridinoline and deoxypyridinoline in skin and urine samples. K E Y W O R D Sdeoxypyridinoline, mass spectrometry, pyridinoline, silica hydride column, urine analysis 1482

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LC–MS/MS application for urine free pyridinoline and free deoxypyridinoline: Urine markers of collagen and bone degradation

Cited by 15 publications

References 33 publications

A Mediterranean-like dietary pattern with vitamin D3 (10 µg/d) supplements reduced the rate of bone loss in older Europeans with osteoporosis at baseline: results of a 1-y randomized controlled trial

A Mediterranean-like dietary pattern with vitamin D3 (10 µg/d) supplements reduced the rate of bone loss in older Europeans with osteoporosis at baseline: results of a 1-y randomized controlled trial

Elevated urinary excretion of free pyridinoline in Friesian horses suggests a breed-specific increase in collagen degradation

Rapid analysis of pyridinoline and deoxypyridinoline in biological samples by liquid chromatography with mass spectrometry and a silica hydride column

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