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Báo cáo khóa học: Large aggregating and small leucine-rich proteoglycans are degraded by different pathways and at different rates in tendon pot

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Detection of35S-labelled proteoglycan core proteins remaining in the matrix or released into the medium of tendon explant cultures by fluorography Tissue was dissected from a single meta

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Large aggregating and small leucine-rich proteoglycans are degraded

by different pathways and at different rates in tendon

Tom Samiric, Mirna Z Ilic and Christopher J Handley

School of Human Biosciences, La Trobe University, Melbourne, Victoria, Australia

This work investigated the kinetics of catabolism and the

catabolic fate of the newly synthesized35S-labelled

proteo-glycans present in explant cultures of tendon Tissue from

the proximal region of bovine deep flexor tendon was

incu-bated with [35S]sulfate for 6 h and then placed in explant

cultures for periods of up to 15 days The amount of

radi-olabel associated with proteoglycans and free [35S]sulfate lost

to the medium and retained in the matrix was determined for

each day in culture It was shown that the rate of catabolism

of radiolabelled small proteoglycans (decorin and biglycan)

was significantly slower (T½> 20 days) compared with the

radiolabelled large proteoglycans (aggrecan and versican)

that were rapidly lost from the tissue (T½ 2 days) Both

the small and large newly synthesized proteoglycans were

lost from the matrix with either intact or proteolytically

modified core proteins When explant cultures of tendon

were maintained either at 4C or in the presence of the lysosomotrophic

the cellular catabolic pathway for small proteoglycans was demonstrated indicating the involvement of cellular activity and lysosomes in the catabolism of small proteoglycans It was estimated from these studies that approximately 60% of the radiolabelled small proteoglycans that were lost from the tissue were degraded by the intracellular pathway present

in tendon cells This work shows that the pathways of catabolism for large aggregating and small leucine-rich proteoglycans are different in tendon and this may reflect the roles that these two populations of proteoglycans play

in the maintenance of the extracellular matrix of tendon Keywords: catabolism; proteoglycan; tendon

The extracellular matrix of tendon is composed of parallel

bundles of collagen, which endows the tissue with tensile

strength and its ability to transmit force generated by muscle

to bone Also present within the extracellular matrix of

tendon are two groups of proteoglycans that can be

distinguished on the basis of their size The small

leucine-rich proteoglycans make up approximately 80% of the total

proteoglycans present in the tendon with decorin being the

predominant species and biglycan being present at lower

levels [1–3] The remaining 20% of proteoglycans present in

tendon are the large aggregating proteoglycans, versican

and aggrecan, which are present in similar levels [1–3]

Tendon cells are responsible for the synthesis and

degradation of extracellular proteoglycans Studies

investi-gating the catabolism of the chemical pool of aggrecan and

versican by tendon in explant culture have revealed that this

process involves the proteolytic cleavage of the core proteins

of these proteoglycans by aggrecanase activity as well as

other proteinases [1–3] The catabolism of the chemical pool

of decorin and biglycan involves the loss of intact core

proteins from the tendon matrix as well as limited

proteo-lytic cleavage [1–3]

We have previously studied the kinetics of catabolism of newly synthesized proteoglycans in bovine collateral liga-ment [4] and demonstrated that the catabolism of newly synthesized 35S-labelled large proteoglycans was rapid (T½ 2 days) and involved proteolytic cleavage of the core protein On the other hand, 35S-labelled small proteoglycans were lost from the tissue at a slower rate (T½ 20 days) and were either lost from the tissue with an intact or partially degraded core protein, or were internalized

by the cells and completely degraded within the lysosomes of the cells [4] Indeed, it has been shown that the cellular uptake

of small proteoglycans is mediated by receptor proteins present in the plasma membranes of fibroblasts [5,6] This study was undertaken to determine the metabolic fate of newly synthesized 35S-labelled proteoglycans by tendon in order to elucidate the specific processes and pathways that are involved in the catabolism of newly synthesized proteoglycans present in a dense collagenous connective tissue and to compare the resulting radiolabelled catabolic products with those reported by us for the chemical pool present in the tissue [1]

Experimental procedures Materials

Dulbecco’s modified Eagle’s medium (DMEM), Eagle’s nonessential amino acids, penicillin and streptomycin were purchased from CSL (Melbourne, Victoria, Australia) Sephadex G-25 (as prepacked PD-10 columns) was from Pharmacia (Uppsala, Sweden) Aqueous solution of

Correspondence to C J Handley, School of Human Biosciences, La

Trobe University, 3086, Victoria, Australia Fax: +61 39479 5784,

Tel.: +61 39479 5800, E-mail: C.Handley@latrobe.edu.au

Abbreviation: GdnHCl, guanidine hydrochloride.

Enzymes: chondroitinase ABC from Proteus vulgaris (EC 4.2.2.4);

keratanase from Pseudomonas sp (EC 3.2.1.103).

(Received 16 June 2004, revised 21 July 2004, accepted 27 July 2004)

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[35S]sulfate (carrier free) was from DuPont New England

Nuclear (Boston, MA, USA) Keratanase (from

Pseudo-monassp.; EC 3.2.1.103) was obtained from Sigma Chemical

Co (St Louis, MO, USA) and chondroitinase ABC

(protease free; from Proteus vulgaris; EC 4.2.2.4) from ICN

Biochemicals (Costa Mesa, CA, USA) Adult bovine

meta-carpophalangeal joints were obtained from a local abattoir

Tendon explant cultures

Deep flexor tendon proximal to the bifurcation was dissected

from a single metacarpophalangeal joint of a one-to-two year

old steer The tendon was then chopped into small pieces and

incubated in sulfate-free medium (1 g tissue per 10 mL

medium) containing 200 lCiÆmL)1[35S]sulfate at 37C for

6 h The sulfate-free medium contained 0.13M sodium

chloride, 4.74 mM potassium chloride, 2.54 mM calcium

chloride, 1.9 mM magnesium chloride, 10 mM glucose,

1.0 mM L-glutamine, 1.19 mMpotassium dihydrogen

phos-phate, 0.02 gÆmL)1 Phenol Red and was buffered with

25 mMHEPES adjusted to pH 7.4 with sodium hydroxide

[7] Sulfate-free medium was used in order to increase the

incorporation of [35S]sulfate into proteoglycans as it has

previously been reported that the rate of incorporation of

[35S]sulfate into proteoglycans by tendon is considerably less

than other connective tissues such as articular cartilage, and

this necessitated the use of high specific radioactivity

[35S]sulfate [8] It was also shown that the rate of

incorpor-ation of [35S]sulfate into proteoglycans was linear over the

6 h incubation period After washing the tissue extensively in

DMEM to remove most of the unincorporated radioisotope,

duplicate samples containing 100 ± 20 mg of tissue were

distributed into individual sterile preweighed plastic vials

containing 4 mL of DMEM DMEM contains sufficient

chemical levels of sulfate (0.8Mmagnesium sulfate) so that

the specific radioactivity of radiolabelled sulfate present in or

produced by the explant cultures will be considerably

reduced, thereby decreasing the level of re-use of [35S]sulfate

by the cells of the cultures

The culture medium was collected and replaced daily with

4 mL of fresh DMEM The collected medium was stored at

)20 C in the presence of proteinase inhibitors [9] At the

end of the culture period, the tissue was extracted with 4M

guanidine hydrochloride (GdnHCl) in the presence of

proteinase inhibitors at 4C for 72 h, followed by 0.5M

NaOH at 21C for 24 h

Determination of the percentage of35S-labelled

proteoglycans remaining in the matrix of tendon

explant cultures

To determine the percentage of35S-labelled proteoglycans

remaining in the matrix of tendon cultures on each day after

incubation with [35S]sulfate, 0.5 mL aliquots of the medium

fractions, GdnHCl and NaOH extracts were applied to

columns of Sephadex G-25 (PD-10 columns) equilibrated

and eluted with 4M GdnHCl, 0.1M Na2SO4, 0.05M

sodium acetate, 0.1% (v/v) Triton X-100, pH 6.1 The

35S-labelled material that eluted in the excluded volume of

the column was attributable to35S-labelled macromolecules

in the medium that were originally derived from

proteo-glycans present in tendon matrix The35S-labelled material

which eluted in the total volume was shown to represent free [35S]sulfate The rate of loss of35S-labelled proteoglycans from the matrix of explant cultures was calculated from the amount of35S-labelled macromolecules in the medium on each day of culture and that remained in the matrix at the end of the culture period From these data the percentage of

35S-labelled proteoglycans remaining in the matrix was plotted as a function of time in culture [10]

Separation of35S-labelled proteoglycans remaining in the matrix of tendon explant cultures by size exclusion chromatography

Aliquots (1 mL) of the GdnHCl extracts obtained from tissue after predetermined times in culture were applied to a column of Sepharose CL-4B (1.3· 87.0 cm) equilibrated and eluted with 4MGdnHCl, 50 mMsodium acetate buffer, 0.1% (v/v) Triton X-100 pH 5.8 Fractions of 1 mL were collected at a flow rate of 6 mLÆh)1 and assayed for

35S-radioactivity From these data the percentage of

35S-labelled large and small proteoglycan species remaining

in the matrix at different times in culture was determined [10]

Detection of35S-labelled proteoglycan core proteins remaining in the matrix or released into the medium

of tendon explant cultures by fluorography Tissue was dissected from a single metacarpophalangeal joint and incubated with [35S]sulfate for 6 h as described above The tissue was maintained in DMEM alone for up to

10 days The culture medium was collected and replaced daily After predetermined times in culture, the tissue was extracted with 4M GdnHCl as described above Proteo-glycans were isolated from tissue extracts and medium samples by ion-exchange chromatography on Q-Sepharose

as described previously [1]

The samples were then dialysed against distilled H2O containing proteinase inhibitors, lyophilized, and dissolved

in 1 mL of 0.1M Tris/0.1M sodium acetate pH 7.0 containing proteinase inhibitors [10] The dried samples were then digested with chondroitinase ABC (0.0375 U) and keratanase (0.075 U) at 37C for 24 h in the presence

of proteinase inhibitors [11] Samples were subjected to electrophoresis on a 4–15% gradient polyacrylamide/SDS slab gel The gel was then fixed in a solution of 30% (v/v) methanol and 10% (v/v) acetic acid for 30 min, soaked in Amplify for 30 min, dried and exposed to X-ray film at )20 C for approximately 40 days

Intracellular degradation of35S-labelled small proteoglycans

In order to determine the rate of intracellular degradation of

35S-labelled small proteoglycans, bovine tendon from a single metacarpophalangeal joint was incubated with [35S]sulfate for 6 h as described above and then maintained

in DMEM alone for 5 days to allow time for loss of the

35S-labelled large proteoglycans from the tissue cultures For the subsequent days (days 6–15) the tissue was maintained in culture under the conditions described below The rate of intracellular proteoglycan catabolism by tendon explants was determined from the amount of radiolabelled

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sulfate appearing in the medium on each day For this,

aliquots of the culture medium were applied to Sephadex

G-25 (PD-10) columns and the amount of [35S]sulfate

determined from the amount of35S-radioactivity in the total

volume of the columns The rate of release of35S-labelled

proteoglycans into the culture medium in these experiments

was determined by the35S-radioactivity that eluted in the

excluded volume on Sephadex G-25 columns The

percent-age of35S-labelled proteoglycans remaining in the matrix

was determined as described above

Treatment of data

Previous work has shown that there is variation between

animals in the absolute rates of metabolism of

macro-molecular components of the extracelullar matrix of

synovial connective tissues Because the amount of tissue

was limiting, this only enabled points to be repeated in

duplicate Therefore, individual experiments were repeated

at least three times using tissue from different animals

Results

Determination of the loss of35S-labelled proteoglycans

from the extracellular matrix of tendon explant cultures

Explants of bovine tendon were incubated with [35S]sulfate

for 6 h and then maintained in culture in DMEM for up to

10 days Medium fractions were collected daily and the

tissue extracted at the end of the culture period with 4M

GdnHCl followed by 0.5M NaOH as described above

Approximately 75% of 35S-labelled proteoglycans were

extracted from the tendon matrix with GdnHCl (data not

shown) The medium fractions and the GdnHCl and NaOH

extracts were analyzed by size exclusion chromatography on

Sephadex G-25 as described above All the radiolabelled

material appearing in the total volume of the columns was

shown to be free [35S]sulfate because it was all precipitated

by barium acetate (data not shown) Figure 1 shows the rate

at which 35S-labelled proteoglycans and free [35S]sulfate

appeared in medium samples on each day in culture During

the first two days of culture the appearance of free

[35S]sulfate in the culture medium was attributable to

unincorporated [35S]sulfate following incubation of the

tissue with [35S]sulfate on day 0 Over the subsequent days

(days 3–10), both the free [35S]sulfate and 35S-labelled

proteoglycans appeared in the culture medium at a similar

rate Any re-use of free [35S]sulfate during the first two days

of explant culture would be minimal as the specific

radioactivity of the radiolabelled sulfate would be markedly

reduced by the sulfate content of DMEM Figure 2A shows

that there was a faster rate of loss of35S-labelled

proteo-glycans from the matrix in the first four days of culture and

approximately 60% of35S-labelled proteoglycans remained

in the matrix after 10 days in culture

Kinetics of loss of large and small35S-labelled

proteoglycans from the extracellular matrix of tendon

explant cultures

The amount of 35S-radiolabel associated with large and

small proteoglycans remaining in the matrix of tendon

explants described in Fig 2A was determined from tissue extracts on days 0, 2, 4, 6, 8 and 10 These extracts were subjected to gel filtration on a column of Sepharose CL-4B eluted under dissociative conditions (Fig 3) It is evident that there are two35S-labelled proteoglycan peaks,

a minor peak (Kav 0.05) representing the large prote-oglycans and a major peak (Kav 0.5) representing the small proteoglycans The proportion of 35S-radioactivity associated with the large proteoglycans decreased from 16.6% on day 0 (the day of incubation with [35S]sulfate)

to 2.1% on day 10, whereas that for the small proteo-glycans showed an apparent increase from 83.4% on day

0 to 97.9% by day 10 This indicates that there is a preferential loss of the newly synthesized35S-labelled large proteoglycans from the extracellular matrix of tendon Although 40% of the35S-labelled proteoglycans was lost from the extracellular matrix of tendon over the 10 day culture period, the hydrodynamic size of each35S-labelled proteoglycan species extracted from the matrix of the tissue immediately after incubation of the tissue with [35S]sulfate and at various time points in culture remained constant The presence of unincorporated [35S]sulfate early

in the culture period (days 0 and 2) is indicated in the elution profiles in the total volume of the column

The percentage of 35S-labelled large and small proteo-glycans remaining in the matrix at various times after incubation with [35S]sulfate was determined by multiplying the percentage of each proteoglycan species present in the tissue extracts on days 0, 2, 4, 6, 8 and 10 of the culture period (Fig 3) by the percentage of 35S-labelled proteoglycans remaining in the matrix on the corresponding day of culture (Fig 2A) This was then expressed as the percentage of the amount of each proteoglycan species present in the tissue on day 0 (Fig 3; top) in order to determine the kinetics of loss of the large and small

Fig 1 Rate of appearance of35S-labelled proteoglycans and [35 S]sul-fate into the culture medium of explant cultures of tendon The proximal region of bovine deep flexor tendon was incubated with [ 35 S]sulfate as described in Experimental procedures, and cultured in DMEM alone for 10 days The rate of appearance of 35 S-labelled proteoglycans (d) and [ 35 S]sulfate (s) into the culture medium from bovine tendon explant cultures was determined by analysis of medium samples from each day of culture period on columns of Sephadex G-25 The error bars represent the range of duplicate samples.

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35S-labelled proteoglycans in tendon Figure 2B shows that

the loss of 35S-labelled small proteoglycans from the

extracellular matrix was much slower (T½> 20 days)

compared to the 35S-labelled large proteoglycans (T½

2 days) It is evident from Fig 2B that over 85% of large

proteoglycans were lost from the tissue within the first six

days after incubation of the tissue with [35S]sulfate, whilst

only 20% of small proteoglycans were lost over this time

period

Characterization of35S-labelled proteoglycans remaining

in the matrix and released into the medium of tendon

explant cultures by fluorography

To analyze the 35S-labelled proteoglycan core proteins

isolated from either the tissue or released into the culture

medium, tendon was incubated with [35S]sulfate for 6 h

prior to being maintained in culture in DMEM for up to

10 days Radiolabelled proteoglycans present in the matrix

Fig 2 Percentage of 35S-labelled proteoglycans remaining in the

extracellular matrix of tendon explants cultures (A) The proximal

region of bovine deep flexor tendon was incubated with [35S]sulfate

and maintained in DMEM for 10 days The percentage of35S-labelled

proteoglycans remaining in the matrix of tendon cultures on each day

after incubation with [ 35 S]sulfate was determined as described in

Experimental procedures The error bar represents the range of

duplicate samples (B) The percentage of 35 S-labelled large

proteogly-cans (d) and 35 S-labelled small proteoglycans (s) remaining in the

tissue at each time after incubation of bovine tendon with [35S]sulfate

was determined as described in Results The error bars represent the

range of duplicate samples.

Fig 3 Elution profiles on Sepharose CL-4B of the 35S-labelled pro-teoglycans remaining in the matrix of tendon cultures maintained in DMEM On the days indicated, tissue samples from the experiment described in Fig 2 were extracted with 4 M GdnHCl and aliquots of the 35 S-labelled proteoglycans were applied to a column of Sepharose CL-4B eluted with a buffer containing 4 M GdnHCl In each profile, the amount of 35 S-labelled proteoglycans extracted from the tissue on each day is expressed as a percentage of the 35 S-labelled proteoglycans extracted on day 0 The values in parentheses refer to the relative percentage of large and small proteoglycan species present

of extraction.

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and culture medium were digested with chondroitinase

ABC and keratanase, which results in the removal of most

of the glycosaminoglycan chains but leaves 35

S-radio-labelled glycosaminoglycan stubs associated with the core

protein The partially deglycosylated core proteins were

then subjected to electrophoresis on a 4–15% gradient

polyacrylamide/SDS large gel followed by fluorography as

described in Experimental procedures Figure 4 (lane i)

shows that three distinct high molecular mass bands above

300 kDa were present in tendon matrix immediately after

incubation with [35S]sulfate Based on our previous work it

is likely that these bands represent intact core protein of

aggrecan and V0 and/or V1 splice-variants of versican [1]

With time in culture, a distinct band at  300 kDa

(indicated by asterisk) appeared, and remained in the

matrix over the culture period of 10 days (lanes ii and iii)

The precise identity of this band is not known but it is likely

to be a product of the proteolytic processing of the core

protein of aggrecan or versican A series of weak bands

ranging between 80 to above 250 kDa were also present and

these are likely to represent degradation products of the

large proteoglycans that are retained in the matrix The majority of radiolabelled material present in the matrix of fresh tendon was associated with the band ranging between

37 and 45 kDa This band corresponds to the decorin core protein; also present are small levels of biglycan core protein [1] A number of bands were also observed at 33 kDa and below, which we have shown to be degradation products of decorin [1]

A diffuse band at 50 kDa, which is likely to represent intact fibromodulin or degradation products of large proteoglycans, was also evident [10] It was apparent that the decorin core protein of 43 kDa (lane i) present in tissue immediately after incubation with [35S]sulfate, decreased in size with time in culture (lanes ii and iii) indicating extracellular processing of decorin core protein It is possible that newly synthesized decorin contains an intact amino-terminal propeptide which is removed with time in culture

by the action of proteinases present in the extracellular matrix of the tissue [12,13] Further proteolytic processing

of decorin core protein was shown by the presence of additional distinct bands at 25 kDa and below (lanes ii and iii) These observations indicate that degradation of core proteins of newly synthesized small proteoglycans occurs and that fragments are retained within the matrix Figure 4 (lanes iv and v) shows the proteoglycan core proteins released into the medium of explant cultures after 3 and 6 days in culture, respectively A number of distinct bands of over 250 kDa and a series of bands ranging between 75 and 160 kDa are present in the medium and we have previously shown that they represent catabolic prod-ucts of aggrecan and versican [1] It must be pointed out that the amount of35S-radioactivity associated with these high molecular mass peptides is directly attributable to the high density of sulfate groups associated with these large proteoglycans

Intracellular catabolism of35S-labelled small proteoglycans by tendon explant cultures Because it was shown that [35S]sulfate appeared in the culture medium throughout the culture period (Fig 1), experiments were performed to determine if this was due to intracellular degradation of 35S-labelled small proteogly-cans Bovine deep flexor tendon was maintained in culture

in DMEM for 5 days after incubation with [35S]sulfate to allow for the loss of the majority of the radiolabelled large proteoglycans (Fig 2B) Cultures were then maintained in DMEM at 37C or 4 C for a subsequent 10 days to determine the effect of reduced cellular activity on the appearance of free [35S]sulfate in the medium In some cultures, the temperature was switched at the mid-point of the culture period to determine whether the effect of low temperature on the generation of free [35S]sulfate was reversible Figure 5A shows that in cultures maintained at

37C, there was a continuous rate of formation of free [35S]sulfate in the culture medium The rate of generation of [35S]sulfate in the medium was reduced by over 90% in cultures maintained at 4C, suggesting that metabolically active cells were required for this process This reduction was also demonstrated when cultures were switched from

37C to 4 C on day 10 of the culture period, whereas in cultures that were initially maintained at 4C, there was an

Fig 4 Analysis of35S-labelled proteoglycan core proteins present in the

matrix or medium of explant cultures of tendon Newly synthesized

35

S-labelled proteoglycans remaining in the matrix or released into the

medium of tendon explant cultures after 10 days in culture were

iso-lated as described in Experimental procedures and digested with

chondroitinase ABC and keratanase, prior to electrophoresis on a

4–15% polyacrylamide/SDS large gel The gel was subjected to

fluo-rography as described in Experimental procedures Lanes show

pep-tides present in (i) fresh tendon tissue, (ii) tissue after 6 days in culture,

(iii) tissue after 10 days in culture, (iv) days 1–3 pooled medium, and

(v) days 4–6 pooled medium Approximate molecular mass of

observed peptides are given.

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apparent increase in the rate of [35S]sulfate appearance

when these cultures were switched to 37C, demonstrating

that this effect was reversible In contrast to the rate of

formation of [35S]sulfate, Fig 5B shows that there was an

increase by 40% of35S-labelled proteoglycans appearing in

the culture medium of tendon explants maintained at 4C

The percentage of35S-labelled proteoglycans remaining in

the matrix of cultures maintained at 37C (calculated from

both the release of 35S-labelled proteoglycans and the

appearance of [35S]sulfate with time in culture) was

approximately 80% by the end of the culture period on

day 15 as shown in Fig 5C However, the loss of

35S-labelled proteoglycans was reduced in cultures

main-tained at 4C, where about 95% of 35S-labelled

proteo-glycans remained in the matrix by the end of the culture

period on day 15

The work described above suggests that small

proteo-glycans are taken up by the cells and digested intracellularly

To demonstrate that the lysosomal system is involved in the

appearance of free [35S]sulfate in the culture medium,

tendon cultures were maintained in DMEM containing

10 mMammonium chloride following 5 days in culture in

DMEM alone Ammonium chloride is a lysosomotropic

amine and acts by raising the intralysosomal pH which

inhibits the activity of lysosomal enzymes, and is known to

be an effective reversible inhibitor of lysosomal function at

low concentration [14] Figure 6A shows that in cultures

maintained in DMEM containing 10 mM ammonium

chloride, the rate of [35S]sulfate appearing in the medium

was suppressed by approximately 78% compared with

control cultures This suppression was further demonstrated

when cultures were switched on day 10 from DMEM alone

to DMEM containing 10 mMammonium chloride When

cultures were switched on day 10 from DMEM containing

10 mMammonium chloride to DMEM alone, the rate of

[35S]sulfate appearance was restored, demonstrating that

this effect was reversible The rate of release of35S-labelled

proteoglycans into the culture medium was increased by

approximately 107% in cultures maintained in the presence

of ammonium chloride (Fig 6B) The percentage of

35S-labelled proteoglycans remaining in the matrix in

DMEM alone was approximately 80% by the end of the

culture period on day 15 as shown in Fig 6C However, the

loss of35S-labelled proteoglycans was reduced in cultures

maintained in the presence of ammonium chloride, where

about 85% of35S-labelled proteoglycans remained in the

matrix by the end of the culture period on day 15

Discussion

This study showed that the loss of the large aggregating

proteoglycans (aggrecan and V0 and/or V1 splice-variants

of versican) that make up approximately 17% of the

35S-labelled pool of newly synthesized proteoglycans was

rapid, with a half-life of about 2 days (Fig 4) These

findings are consistent with studies using other joint

connective tissues such as articular cartilage [15] and

collateral ligament [10] In the case of articular cartilage, it

has been shown that the majority of newly synthesized

aggrecan remains closely associated with the chondrocytes

[16,17] However, the majority of the chemical pool of

aggrecan resides in the interterritorial matrix and it is this

Fig 5 Effect of reduced temperature on the rate of formation of [ 35 S]sulfate and release of 35 S-labelled proteoglycans from tendon explant cultures Explant cultures of deep flexor tendon were incubated with [ 35 S]sulfate as described in Experimental procedures and then maintained in DMEM for 5 days prior to analysis Tissue was sub-sequently cultured for a further 10 days in DMEM at 37 C (d), DMEM at 4 C (s), DMEM at 37 C which was switched to 4 C on day 10 (,), or DMEM at 4 C which was switched to 37 C on day 10 (.) The culture medium was collected daily and analyzed for the presence of [ 35 S]sulfate and 35 S-labelled proteoglycans From this data, (A) the rate of appearance of [35S]sulfate, (B) the rate of release of

35

S-labelled proteoglycans, and (C) the percentage of 35S-labelled proteoglycans remaining in the matrix were determined, as described in Experimental procedures The error bars represent the range of duplicate samples over the remaining 10 days.

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population that is responsible for the biomechanical prop-erties of cartilage Work has shown that this population of aggrecan turns over very slowly, with a half-life in excess of 3.5 years [18] If this is applied to the present study, it is likely that newly synthesized aggrecan and versican may be closely associated with tendon cells where the turnover is mediated

by proteolytic enzymes originating from tendon cells Indeed, we have shown that the catabolism of aggrecan in tendon appears to be exclusively attributed to aggrecanase proteinases whereas the catabolism of versican may involve aggrecanase as well as other proteinases [1] It is likely that these enzymes are responsible for the rapid turnover of the newly synthesized pool of large proteoglycans, as the resulting radiolabelled core protein fragments are of similar size to those previously reported by our laboratory for the chemical pools of large aggregating proteoglycans present

in tendon [1] Furthermore, it has been reported that the aggrecanase proteinases ADAMTS-4 and ADAMTS-5 are expressed in bovine tendon cells [2], but at different stages of development of the animal We have observed the expres-sion of both ADAMTS-4 and ADAMTS-5 in bovine tendon cells from mature cattle (T Samiric, M.Z Ilic & C.J Handley, unpublished data)

In contrast to the rapid rate of loss of newly synthesized large proteoglycans, the newly synthesized small proteo-glycans were lost slowly from the matrix of tendon cultures with a half-life of greater than 20 days, which is consistent with findings from earlier studies in explant cultures of tendon [19], articular cartilage [15] and ligament [4,10] This slow loss of newly synthesized small proteoglycans may be indicative of their association with other matrix molecules, particularly Type I collagen fibres [20], and it is possible that the turnover of this group of proteoglycans may be coordinated with the turnover of other matrix macromolecules However, some of the radiolabelled decorin undergoes proteolytic cleavage and these products are either retained within the matrix or lost to the culture medium in a similar manner to that observed for the chemical pool [1]

Approximately 60% of the35S-labelled decorin that was lost from the matrix was taken up by the tendon cells and degraded within the lysosomal system This was shown by the generation of free [35S]sulfate by tendon explant cultures throughout the culture period This finding is supported by similar studies using ligament explant cultures [4] The cellular uptake and subsequent degradation of decorin has been observed in a variety of cells of mesenchymal origin [4,21] It has been shown that the leucine-rich repeat region

of decorin binds to specific receptors present in the plasma membrane and endosomes of skin fibroblasts, osteosarcoma cells and chondrocytes [5,22] Upon entering the cell by endocytosis, decorin is subsequently transported to the lysosomes Previous work has shown that at least two intracellular pathways are involved in the catabolism of endogenously radiolabelled proteoglycans associated with the cell surface in rat ovarian granulosa cells [23] One pathway leads to a rapid and complete intralysosomal degradation resulting in the release of [35S]sulfate In the second pathway, the rate of degradation is slower and commences with extensive proteolysis, generating glycos-aminoglycan chains bound to peptides before final hydro-lysis takes place [23]

Fig 6 Effect of ammonium chloride on the rate of formation of

[35S]sulfate and release of 35S-labelled proteoglycans from tendon

explant cultures Explant cultures of deep flexor tendon were incubated

with [ 35 S]sulfate as described in Experimental procedures and then

maintained in DMEM for 5 days prior to analysis Tissue was

sub-sequently cultured for a further 10 days in DMEM alone (d), DMEM

containing 10 m M ammonium chloride (s), DMEM alone which was

switched to DMEM containing 10 m M ammonium chloride on day 10

(,), or DMEM containing 10 m M ammonium chloride which was

switched to DMEM alone on day 10 (.) The culture medium was

collected daily and analyzed for the presence of [35S]sulfate and

35 S-labelled proteoglycans From this data, (A) the rate of appearance

of [ 35 S]sulfate, (B) the rate of release of 35 S-labelled proteoglycans, and

(C) the percentage of 35S-labelled proteoglycans remaining in the

matrix were determined, as described in Experimental procedures The

error bars represent the range of duplicate samples over the remaining

10 days.

Trang 8

This study indicates that the intracellular degradation of

decorin requires metabolically active cells including a

functional lysosomal system because this process was

inhibited at 4C and in the presence of ammonium chloride

(Figs 5 and 6) In addition, when these treatments were

applied to tendon explant cultures there was an inhibition of

the intracellular degradation of decorin and a simultaneous

increase in the appearance of35S-labelled of decorin in the

medium throughout the culture period (Figs 5 and 6), albeit

to different degrees This enhanced loss of decorin by the

pathway that results in the loss of decorin from the

extracellular matrix has also been observed in ligament

explant cultures [4] It has previously been reported that

decorin is only taken up by cells if it is not bound to other

extracellular matrix molecules [24] However, little is known

about the nature of interactions of newly synthesized

decorin with other extracellular components and its

distri-bution within the matrix of fibrous connective tissues It is

possible that a proportion of newly synthesized decorin

remains located close to the cell and may be loosely

associated with the cell membrane and/or extracellular

matrix This pool of decorin is likely to be subjected to

intracellular degradation The inhibition of the cellular

uptake of newly synthesized decorin appears to result in

more of this pool of decorin being lost from the tissue into

the culture medium This may involve displacement of

newly synthesized decorin that is further away from the cell

and subsequent release to the medium, thus reducing

the accumulation of this proteoglycan within the

extra-cellular matrix of tendon The low level of loss of

radio-labelled decorin suggests that a significant proportion of

the newly synthesized decorin is retained in the

extra-cellular matrix in strong interactions with other extraextra-cellular

matrix macromolecules where the core protein of this

proteoglycan can undergo proteolytic processing (Fig 4;

lanes ii and iii)

The work presented in this paper supports previous

observations which show that the catabolism of large and

small proteoglycans follow distinct separate pathways

Furthermore, it is evident that in both tendon and ligament

[4] the processes involved in the catabolism of proteoglycans

are similar and this is not unexpected considering the

similarity in the structure and organization of these two

dense connective tissues In both tissues the intracellular

degradation pathway plays a significant role in the

catabo-lism of newly synthesized small proteoglycans In the case of

tendon this pathway represents about 60% of the

radio-labelled pool of small proteoglycans and in the case of

ligament represents 30% of this pool [4] This raises the

question of whether this pathway is also involved in the

catabolism of the chemical pool of small proteoglycans that

are present in the extracellular matrix of these tissues

Furthermore, the contribution of this intracellular pathway

of catabolism of small proteoglycans needs to be taken into

account in studies investigating the catabolism of small

proteoglycans in dense connective tissues in pathological

conditions

6

Acknowledgements

We wish to thank the Arthritis Foundation of Australia and the

Faculty of Health Sciences, La Trobe University for support.

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