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Tiêu đề Glycation of low-density lipoprotein results in the time-dependent accumulation of cholesteryl esters and apolipoprotein B-100 protein in primary human monocyte-derived macrophages
Tác giả Bronwyn E. Brown, Imran Rashid, David M. Van Reyk, Michael J. Davies
Trường học The Heart Research Institute
Chuyên ngành Biochemistry
Thể loại Journal article
Năm xuất bản 2007
Thành phố Sydney
Định dạng
Số trang 12
Dung lượng 222,06 KB

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This accumula-tion of cholesteryl esters and modified protein from glycated low-density lipoprotein may contribute to cellular dysfunction and the increased atherosclerosis observed in pe

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Glycation of low-density lipoprotein results in the

time-dependent accumulation of cholesteryl esters

and apolipoprotein B-100 protein in primary human

monocyte-derived macrophages

Bronwyn E Brown1, Imran Rashid1, David M van Reyk2and Michael J Davies1,3

1 Free Radical Group, The Heart Research Institute, Camperdown, Sydney, NSW, Australia

2 Department of Health Sciences, University of Technology Sydney, NSW, Australia

3 Faculty of Medicine, University of Sydney, NSW, Australia

Complications associated with diabetes are the major

cause of mortality and morbidity in people with this

disease These include microvascular complications that

induce damage to the retina, nephrons and peripheral nerves, and macrovascular disease that is associated with accelerated atherosclerosis (deposition of lipids in

Keywords

aldehydes; atherosclerosis; foam cells;

human monocyte-derived macrophages;

low-density lipoproteins

Correspondence

M J Davies, 114 Pyrmont Bridge Road,

Camperdown, Sydney, NSW 2050, Australia

Fax: +61 2 95655584

Tel: +61 2 82088900

E-mail: daviesm@hri.org.au

(Received 12 December 2006, accepted

15 January 2007)

doi:10.1111/j.1742-4658.2007.05699.x

Nonenzymatic covalent binding (glycation) of reactive aldehydes (from glu-cose or metabolic processes) to low-density lipoproteins has been previ-ously shown to result in lipid accumulation in a murine macrophage cell line The formation of such lipid-laden cells is a hallmark of atheroscler-osis In this study, we characterize lipid accumulation in primary human monocyte-derived macrophages, which are cells of immediate relevance to human atherosclerosis, on exposure to low-density lipoprotein glycated using methylglyoxal or glycolaldehyde The time course of cellular uptake

of low-density lipoprotein-derived lipids and protein has been character-ized, together with the subsequent turnover of the modified apolipoprotein B-100 (apoB) protein Cholesterol and cholesteryl ester accumulation occurs within 24 h of exposure to glycated low-density lipoprotein, and increases in a time-dependent manner Higher cellular cholesteryl ester lev-els were detected with glycolaldehyde-modified low-density lipoprotein than with methylglyoxal-modified low-density lipoprotein Uptake was signifi-cantly decreased by fucoidin (an inhibitor of scavenger receptor SR-A) and

a mAb to CD36 Human monocyte-derived macrophages endocytosed and degraded significantly more125I-labeled apoB from glycolaldehyde-modified than from methylglyoxal-modified, or control, low-density lipoprotein Dif-ferences in the endocytic and degradation rates resulted in net intracellular accumulation of modified apoB from glycolaldehyde-modified low-density lipoprotein Accumulation of lipid therefore parallels increased endocytosis and, to a lesser extent, degradation of apoB in human macrophages exposed to glycolaldehyde-modified low-density lipoprotein This accumula-tion of cholesteryl esters and modified protein from glycated low-density lipoprotein may contribute to cellular dysfunction and the increased atherosclerosis observed in people with diabetes, and other pathologies linked to exposure to reactive carbonyls

Abbreviations

AGE, advanced glycation end-products; apoB, apolipoprotein B-100; HBSS, Hank’s balanced salt solution; HMDM, human monocyte-derived macrophage; HSA, human serum albumin; LDL, low-density lipoprotein.

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the artery wall) in the coronary, peripheral and carotid

arteries [1] Factors that may contribute to this

acceler-ated atherosclerosis include chronic elevacceler-ated glucose

levels (hyperglycemia) and insulin resistance,

dyslipide-mias, and abnormalities of homeostasis [2]

Macrovas-cular disease has been reported to appear in people

with type 2 diabetes at, or near the time of, first

diag-nosis of diabetes, consistent with a shared underlying

pathogenesis [2] An early and persistent feature of the

atherosclerotic lesion is the presence of lipid-laden

(foam) cells in the intima of the artery wall, arising

from cholesterol and cholesteryl ester accumulation by

macrophage cells present in the artery wall [3]

Low-density lipoproteins (LDLs) are the likely source of this

lipid, with unregulated LDL uptake occurring via

receptors other than the native LDL receptor, including

CD36 and class A scavenger receptors [4,5] These

receptors recognize abnormal LDL species, including

those modified by oxidation, aggregation, chemical

modification and formation of immune complexes [4,6]

Elevated glucose levels are strongly linked to the

incidence and severity of atherosclerosis [7,8] Of

par-ticular relevance is the potential role of glucose (or

species derived from glucose) in LDL modification

[9,10] Previous studies have identified multiple

poten-tial mechanisms of LDL modification, including

gly-cation and glycoxidation [9] Glygly-cation involves the

covalent adduction of an aldehyde (from glucose or

related species) to a reactive amine (e.g Lys and Arg

side chains, N-terminus [11–13]) or thiol (Cys) groups

on proteins [14], such as those of the single protein

molecule of LDL, apolipoprotein B-100 (apoB) The

initial Schiff base undergoes subsequent rearrangement

to yield Amadori products (e.g fructose-lysine)

Glyc-oxidation consists of two related processes) oxidation

of protein-bound sugars (from glycation), and

oxida-tion of free glucose and its products Both processes

can generate radicals that modify LDL, and hence

potentially contribute to the enhanced uptake of such

particles by macrophages [12,15–17]

The species formed by glycation and glycoxidation

undergo subsequent reactions to give a heterogeneous

and complex mixture of materials often called

advanced glycation end-products (AGEs) [9,12]

Eleva-ted levels of AGEs have been reporEleva-ted in people with

diabetes compared to controls [18], with some of these

materials (e.g Ne-carboxymethyl-lysines and Ne

-carboxy-ethyl-lysines and pentosidine) being known to

accumu-late with age on tissue proteins, and at an increased

rate in LDL and atherosclerotic lesions in people

with diabetes [16,19–21] Ne-carboxymethyl-lysine and

Ne-carboxyethyl-lysine can arise from reaction of Lys

residues with reactive aldehydes (glyoxal⁄

glycolalde-hyde and methylglyoxal, respectively) [22], providing strong evidence for the formation and subsequent reac-tions of these aldehydes in atherosclerotic lesions The plasma concentrations of these aldehydes are elevated

in people with diabetes [23,24], although the concentra-tions of these materials present in the artery wall, and

in atherosclerotic lesions, are unknown

The role of glycation and the two facets of glycoxida-tion in generating modified LDLs and lipid-laden (foam) cells, in vitro or in vivo, is incompletely under-stood Most studies have employed conditions under which both processes have occurred, or where the nat-ure and extent of modifications have not been quanti-fied adequately [15,25] It is therefore unclear as to whether glycation of LDL, in the absence of oxidation, results in foam cell formation in cell types of direct rele-vance to human atherosclerosis It is also not known whether the protein and lipid components of modified LDL accumulate in synchrony, or to similar levels, due

to differences in the rates of cellular proteolysis and lipolysis Furthermore, the cellular handling of the resulting glycated apoB has not been well characterized Modified proteins have been shown to have different susceptibilities to proteolysis than native proteins, with both enhanced and decreased rates having been charac-terized [26,27] The latter may result in the accumula-tion of modified proteins within cells, and subsequent perturbation of cellular metabolism [16,19–21]

Previously, we have characterized conditions that yield glycated, but nonoxidized, LDL [28], and have shown that such particles give rise to lipid accumula-tion in cultured mouse macrophage-like cells [29] In the current study, we have determined whether lipid accumulation also occurs in a more relevant cell type) human monocyte-derived macrophages (HMDMs))

on exposure to LDL glycated using methylglyoxal or glycolaldehyde The time course of cellular uptake of LDL-derived lipid and protein has been characterized,

as well as the subsequent turnover of the apoB protein

It is shown that both lipid and protein are taken up,

in a time-dependent manner, via scavenger receptor SR-A- and CD36-mediated processes, and that the uptake of lipid and protein occurs in synchrony Fur-thermore, it is shown that both lipid and modified pro-tein accumulate in cells, despite significant proteolytic degradation of the modified protein

Results

LDL characterization Glycated LDL particles were prepared using meth-ylglyoxal, glycolaldehyde and glucose, as described

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previously [28,29] This method results in minimal

oxidation of apoB, cholesterol, cholesteryl esters, or

a-tocopherol [28,29], and does not affect the relative

cholesterol, cholesteryl ester, phospholipid or

triglycer-ide composition of the particles (Table 1) In contrast,

significant time- and concentration-dependent

glyca-tion of apoB occurs with methylglyoxal or

glycolal-dehyde when compared to control or glucose-modified

particles, as indicated by particle charge, aggregation,

and amino acid modification [28,29] The relative

elec-trophoretic mobility of the particles used in the current

study was not significantly different to that reported

previously [29], irrespective of LDL iodination (data

not shown)

Lipid accumulation in HMDMs

Lipid accumulation was quantified after exposure of

HMDMs (1· 106cells per well) at 37C, for up to

96 h, to LDL (0 or 100 lgÆmL)1) previously modified

by methylglyoxal (100 mm), glycolaldehyde (100 mm)

or glucose (100 mm ± 1 lm Cu2+), or control LDL

incubated with EDTA (50 lm) No change in cell

viab-ility or protein was detected in comparison to control

cells not exposed to LDL LDL chemically modified

by acetylation was employed as a positive control

Cells exposed to glucose (± Cu2+)-modified LDL did

not contain significantly elevated cellular cholesterol or

cholesteryl ester levels in comparison to control cells

incubated with LDL exposed to EDTA (data not

shown) No increase in cellular free cholesterol levels

was observed on exposure of HMDMs to

methylgly-oxal- or glycolaldehyde-modified LDL for 0–96 h in

comparison to incubation controls (LDL incubated

with EDTA; Fig 1A), although these values were

sig-nificantly higher than in cells exposed to no LDL No

significant difference was observed in free cholesterol

levels of HMDMs incubated with unmodified LDL,

compared to no LDL, except at the 96 h time point

(Fig 1A)

In contrast to the above, significant time-dependent accumulation of cholesteryl esters in HMDMs was observed on incubation with glycolaldehyde- or methyl-glyoxal-modified LDL (Fig 1B) Glycolaldehyde-modi-fied LDL induced the greatest accumulation, with this being significantly higher than for methylglyoxal-modi-fied LDL, or control LDL, at all time points Methyl-glyoxal-modified LDL induced significantly greater cholesterol ester accumulation than control LDL at the

48 h and 96 h time points, with the majority of this accumulation occurring over the first 24 h There was

no significant difference in cellular cholesterol ester content between cells incubated with unmodified LDL and cells not incubated with LDL, at all time points Glycolaldehyde-modified LDL induced a steady increase in the percentage of total cholesterol present

as esters over the 96 h period, reaching a value of

53 ± 7% (Fig 1C) Similar levels were detected with acetylated LDL (data not shown) Methylglyoxal-modified LDL also induced a significant increase in the percentage of cholesterol esters when compared to control LDL at all time points, with this reaching

23 ± 6% at 96 h There was no significant difference

in the percentage of cholesterol esters between HMDMs incubated with unmodified LDL and those not incubated with LDL, indicating an absolute requirement for LDL modification for significant lipid accumulation in these cells

Accumulation and turnover of apoB in HMDMs HMDMs were exposed to glycated 125I-labeled LDL, with the levels of cell surface, endocytosed, degraded and intracellular accumulated apoB being determined

by radioactive counting 125I-Labeled acetylated LDL was used as a positive control (data not shown), and gave similar results to those observed for glycol-aldehyde-modified LDL The extent of endocytosis, degradation and intracellular accumulation of apoB increased over time in HMDMs exposed to control

Table 1 Lipid composition (nmol lipidÆmg)1apo B) of native, control and glycated LDL LDL (1 mg proteinÆmL)1) was incubated with 50 l M EDTA (control LDL) or 100 m M modifying agent ± 1 l M Cu2+, in NaCl⁄ P i (pH 7.4), for 7 days at 37 C Values are means ± SEM from three experiments, each with triplicate samples None of the treatments resulted in significantly different values compared to the native LDL (P > 0.05).

Total cholesterol Free cholesterol Cholesteryl ester Triglyceride Phospholipid

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LDL (Fig 2A), methylglyoxal-modified LDL (Fig 2B), glycolaldehyde-modified LDL (Fig 2C) and LDL modified by glucose ± Cu2+(similar to control LDL; data not shown) However, the absolute amount of apoB endocytosed, degraded and accumulated was dependent upon the nature of the LDL modification; these were quantified at the 96 h time point (Fig 2D) The extent of protein endocytosis, degradation and intracellular accumulation of apoB was increased in HMDMs exposed to glycolaldehyde-modified LDL in comparison to those exposed to control LDL HMDMs exposed to methylglyoxal-modified LDL showed signifi-cantly increased endocytosis and degradation when compared to those exposed to control LDL, although this was less marked than with glycolaldehyde-modified LDL These parameters were not elevated for HMDMs exposed to glucose (± Cu2+)-modified LDL when compared to those exposed to control LDL In each case, amounts of cell surface (bound) apoB were min-imal, remained constant over time, and did not vary between conditions (Fig 2A–D)

The turnover of intracellular (accumulated) apoB was examined over a 24 h chase period using LDL-free medium following exposure of HMDMs to labeled gly-colaldehyde- and methylglyoxal-modified LDL, and control LDL, for 96 h The use of LDL-free medium during the chase period allows the turnover of preaccu-mulated protein to be studied in the absence of further cellular uptake In these studies, cell death was < 12%

as measured by the appearance of nondegraded apoB

in the medium In each case, a time-dependent decrease

in (previously nondegraded) intracellular apoB concen-trations was detected, and was matched by an increase

in the concentration of degraded apoB (i.e peptides) in the medium (Fig 3A–C) In all cases, only 20–30% of the apoB present at the start of the chase period was degraded The absolute concentration of apoB turned over decreased in the order glycolaldehyde-modi-fied > methylglyoxal-modiglycolaldehyde-modi-fied > control (P < 0.05) With a 24 h loading period with125I-labeled LDL prior

to a 24 h chase period, a greater turnover of intracellu-lar apoB was observed, with 35–55% of the

nondegrad-ed intracellular apoB being turnnondegrad-ed over (data not shown) The absolute concentration of apoB turned over was lower under these conditions, due to the lower initial accumulation of nondegraded intracellular apoB (data not shown)

Investigation of the nature of the receptors responsible for uptake of glycated LDL HMDMs were exposed to methylglyoxal- or glycol-aldehyde-modified LDL in the absence or presence of

Fig 1 Cellular free cholesterol (A), total cholesteryl esters (B) and

percentage cholesteryl esters of total cholesterol (sum of free

cho-lesterol plus total cholesteryl esters) (C) present in HMDMs after

exposure to no LDL (circles), incubation control LDL (LDL + EDTA;

triangles), methylglyoxal-modified LDL (squares), or

glycolaldehyde-modified LDL (diamonds) HMDMs (1.0 · 10 6

cells per well) were exposed to 100 lgÆmL)1modified LDL (1 mg proteinÆmL)1,

incuba-ted with 100 m M modifying agent or 50 l M EDTA, in NaCl ⁄ P i ,

pH 7.4, for 7 days at 37 C) for up to 96 h in medium containing

10% lipoprotein-deficient serum (with fresh medium and LDL

added at 48 h) before extraction and analysis by HPLC with UV

detection Values are means ± SEM from three or more

experi-ments, each with triplicate samples *, # and + indicate statistically

elevated values (P < 0.05) compared to the control cells (no LDL),

LDL plus EDTA-treated cells, and methylglyoxal-modified

LDL-treated cells, respectively, at each time point.

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mAb to CD36, fucoidin or AGE–human serum albu-min (HSA) for 48 h, and changes in total cellular cho-lesteryl esters were determined using HPLC Exposure

of cells to methylglyoxal-modified LDL (Fig 4A) or glycolaldehyde-modified LDL (Fig 4B) and the mAb

to CD36 or fucoidin resulted in significantly decreased cellular cholesteryl ester accumulation in comparison

to cells exposed only to modified LDL Cells exposed

to modified LDL in the presence of AGE–HSA had lower cholesteryl ester levels, but this decrease was not significantly different in comparison to cells exposed to modified LDL alone

Fig 3 Turnover of accumulated apoB in HMDMs after exposure to

50 lgÆmL)1incubation control [ 125 I]LDL (A) or 50 lgÆmL)1[ 125 I]LDL modified by methylglyoxal (B) or glycolaldehyde (C) for 96 h The preparation and cellular exposure to [ 125 I]LDL were performed as described in Fig 1, after iodination of the LDL, and were followed

by cell washing and exposure to LDL-free chase medium (DMEM containing 1 mgÆmL)1 BSA in place of serum) At the appropriate chase times, cells were lysed and processed to determine nonde-graded intracellular apoB (triangles), denonde-graded intracellular apoB (open circles), and degraded extracellular apoB (squares) Values are means ± SEM from three experiments, each with triplicate samples Note different axis scales * and # indicate statisti-cally elevated values (P < 0.05) compared to 0 h chase time for nondegraded intracellular apoB and extracellular degraded apoB, respectively.

Fig 2 Time course of endocytosis (open circles), surface binding

(triangles), degradation (diamonds) and intracellular accumulation

(squares) of apoB from incubation control [125I]LDL (A) and

[ 125 I]LDL modified by methylglyoxal (B) or glycolaldehyde (C) in

HMDMs (D) compares the data obtained at the 96 h time point on

the cellular handling of apoB in HMDMs exposed to 50 lgÆmL)1

incubation control [ 125 I]LDL (white) or 50 lgÆmL)1[ 125 I]LDL

modi-fied by methylglyoxal (black), glycolaldehyde (horizontal stripes) or

glucose in the absence (dots) or presence (vertical stripes) of Cu2+.

HMDMs (1.0 · 10 6 cells per well) were exposed to 50 lgÆmL)1

modified [ 125 I]LDL for up to 96 h (with fresh medium and [ 125 I]LDL

added at 48 h) before analyses The preparation and cellular

expo-sure to [ 125 I]LDL were performed as described in Fig 1, after

iodi-nation of the LDL Endocytosed material is the sum of degraded

and intracellular measurements Values are means ± SEM from

three experiments, each with triplicate samples Note different axis

scales *, # and + (A–C) indicate statistically elevated values

(P < 0.05) compared to the 0 h time point for apoB endocytosis,

degradation and intracellular accumulation, respectively Columns

(D) with different letters above them are significantly different by

one-way ANOVA (P < 0.05) for that apoB measurement.

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The present study has shown that incubation of

pri-mary HMDMs with glycated, but nonoxidized, LDL

can give rise to time-dependent lipid loading, with this

lipid accumulation occurring in parallel with the

endo-cytosis and degradation of the protein (apoB)

compo-nent of the LDL This uptake of glycated LDL occurs

primarily via scavenger receptor SR-A and CD36

endocytosis, as demonstrated by receptor-blocking

experiments The rates of uptake of both the lipid and

protein components are not matched by the rate of

cel-lular metabolism of these species, resulting in the

accu-mulation of both unmodified cholesteryl esters and

glycated apoB in the cells The rate of removal of the

latter species is slow, with only 20–30% of the glycated

protein being degraded over a 24 h chase period

In contrast to the rapid and extensive lipid

accumu-lation induced by LDL modified by glycolaldehyde or

methylglyoxal, incubation of HMDMs with LDL modified by glucose, or glucose plus Cu2+(with a con-centration of Cu2+ similar to that detected in advan-ced atherosclerotic lesions [30]), did not result in significant cellular sterol accumulation This is in con-trast to the results of a previous study, in which a two-fold increase in cholesteryl ester synthesis was observed

in HMDMs exposed to glucose-modified LDL [25]

No characterization data were presented for the LDL used in this previous study, so this discrepancy may arise from the nature of the modified LDL used, with oxidation being a potential confounding factor Uptake of oxidized LDL has been previously shown to result in foam cell formation [17] The lack of choleste-ryl ester accumulation resulting from LDL being incu-bated with glucose, in the presence or absence of

Cu2+, is consistent with our previous studies using murine macrophage-like cells [29]

Exposure of LDL to 100 mm glycolaldehyde has been shown previously to result in extensive modifica-tion of the Lys residues present on the apoB protein [29] Such modification has been reported to result in recognition by macrophage scavenger receptors [15,29,31] The cellular accumulation of cholesteryl esters (approximately 50% of total sterol levels) observed in the present study is consistent with that reported with cultured murine macrophage-like cells [29] The proportion of total cholesterol present as cholesterol esters in these HMDMs is of a similar mag-nitude to that detected in human atherosclerotic lesions [32]

It has been reported that LDL modified by 10 mm methylglyoxal for 3 days is recognized by macrophage scavenger receptors, but results in decreased intracellu-lar cholesteryl ester synthesis in comparison to controls [33] This is in contrast to the situation with cultured murine cells, where exposure to LDL modified with methylglyoxal for 14 days (with approximately 80% of Lys residues modified) resulted in significant choleste-ryl ester accumulation, with approximately 25% of the total cellular sterol being present as esters [29] In the present study, HMDMs exposed to LDL modified by methylglyoxal for 7 days accumulated significant levels

of cholesteryl ester within 24 h, with approximately 25% of total sterols being present as cholesteryl esters

by 96 h Thus, modification of LDL by methylglyoxal appears to result in macrophage scavenger receptor recognition, and significant cholesteryl ester accumula-tion, in human macrophages It has been reported that LDL isolated from people with diabetes can stimulate cholesteryl ester synthesis in HMDMs, although the level of modification reported (approximately 5% of Lys residues [34]) is lower than that used in the current

Fig 4 Cholesteryl ester changes in HMDMs exposed to

100 lgÆmL)1LDL modified by methylglyoxal (A) or glycolaldehyde

(B) for 48 h in the absence (control) or presence of mAb to CD36

(2 lgÆmL)1), fucoidin (200 lgÆmL)1), or AGE–HSA (200 lgÆmL)1).

Modified LDL was prepared and incubated with cells as described

in Fig 1 Values are means ± SEM from three experiments, each

with triplicate samples *Significantly decreased (P < 0.05) cellular

cholesteryl esters levels compared to cells incubated with the

modified LDL in the absence of any receptor inhibitors.

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study However, direct comparison between these two

sets of data is not possible, as the extent of other

mod-ifications present on these in vivo-modified particles is

not known We have suggested that it may be the

nat-ure of the products arising from glycation, rather than

purely the loss of the parent amino acid, which is the

key factor in terms of receptor recognition [29] There

are no data available on the extent of Lys (and other

amino acid) modification, arising from glycation, in

LDL isolated from human atherosclerotic lesions, so it

is not possible to judge the extent, or type, of amino

acid modification on LDL to which macrophage cells

might be exposed in vivo Further studies are required

to fully elucidate this point

The increased rates of endocytosis and

intracellu-lar degradation of methylglyoxal- and

glycolaldehyde-modified apoB protein from LDL, in HMDMs, is

consistent with particle recognition by macrophage

scavenger [15,29,31,33], or other receptors [35] These

data are in agreement with previous, more limited,

stud-ies with glycolaldehyde-modified LDL [15,31] The

cel-lular uptake and turnover of apoB in macrophages

exposed to methylglyoxal-modified LDL has not been

examined previously, although increased endocytosis

and degradation of apoB modified by other aldehydes

(e.g 4-hydroxynonenal, malondialdehyde) has been

reported [36] The pattern of uptake and degradation of

apoB from the various types of modified LDL examined

here mirrors cholesterol ester accumulation, with

glycol-aldehyde inducing the largest changes, glucose (with or

without Cu2+) the least, and methylglyoxal showing

intermediate behavior Previous studies have reported

both decreased [15] and increased [25] degradation of

apoB from glucose-modified LDL when compared to

native LDL; however, the nature and extent of

modifi-cation (or oxidation) of these particles are not known

Interestingly, apoB from glycolaldehyde-modified

LDL accumulated in HMDMs over time

Accumula-tion of modified proteins has been previously

implica-ted in diseases such as atherosclerosis and diabetes

[16,19–21], and reported to have a variety of cellular

effects It has been shown that moderately oxidized

proteins are more sensitive to proteolysis [37], and are

endocytosed more quickly than native proteins, which

in turn are more rapidly removed than heavily

oxid-ized proteins [27,37] Previous studies have shown that

some proteins that contain AGEs (e.g

pyrraline-modi-fied albumin) accumulate in macrophages because of

decreased cellular degradation rates and a reduced

sus-ceptibility of this glycated protein to lysosomal

proteo-lytic enzymes [38] Thus, glycation alone appears to be

sufficient to inhibit lysosomal degradation of modified

proteins Interestingly, apoB from oxidized LDL has

been shown to accumulate in secondary lysosomes in macrophages because of inefficient degradation [39], although the extent of (labeled) apoB turnover in the chase period (i.e after the cessation of loading) observed in the current study with glycated LDL is much lower than that observed previously for some forms of oxidized LDL (e.g that generated on expo-sure to 10 lm Cu2+ for 4 h [36]), consistent with poor cellular handling of the glycated apoB protein This may be partly explained by the resistance of the modi-fied apoB to degradation by lysosomal cathepsins [40]

In addition we have also shown that glycated⁄ glycoxi-dized proteins can inhibit thiol-dependent lysosomal cathpesins [41], as well as other intracellular enzymes, including lactate dehydrogenase, glyceraldehyde-3-phosphate dehydrogenase, and glutathione reductase [42] The inhibition of the thiol-dependent lysosomal cathepsins by glycated proteins may be of particular importance in apoB turnover

The accumulation of glycated apoB within HMDMs may be related to that of the cholesteryl esters observed under identical conditions, as a result of an interdependence of proteolysis and lipolysis Jessup

et al have postulated, on the basis of studies with oxidized LDL, that failure of macrophages to degrade oxidized apoB may protect LDL cholesteryl esters in the core of the particle from lysosomal esterases, or that impaired lipolysis of LDL lipids may block pro-teolysis of apoB [36] This may arise as a result of the failure of hydrophobic regions of apoB, which have been reported to be recognition signals for proteolysis,

to become exposed [43,44] The accumulation of such AGE-modified proteins may have significant cellular and atherogenic effects, and requires further study SR-A and CD36 have previously been reported to account for 75–90% of the uptake and degradation of acetylated or oxidized LDL [45] Glycated⁄ glycoxi-dized LDL has also been previously reported to

be recognized by macrophage scavenger receptors, although data on which specific scavenger receptors were involved have not been reported [15,31,33]; the current data are consistent with SR-A and CD36 being key species Greater than 60% modification of parent apoB Lys residues has been reported to result in macro-phage scavenger receptor recognition for both glycated and acetylated LDL [31,46] Lys data previously repor-ted by our group [28,29] show that that greater than 60% Lys modification is observed for methylglyoxal-and glycolaldehyde-modified LDL under the condi-tions used in these studies, consistent with this previous conclusion To investigate the types of recep-tor responsible for the uptake of glycated LDL observed in the current study, cells were incubated

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with LDL glycated using glycolaldehyde or

methylgly-oxal, and either a mAb to CD36 [47], the SR-A

inhib-itor fucoidin, or AGE–HSA, which is known to bind

to RAGE [48] The inhibition of uptake observed with

the mAb to CD36 or fucoidin indicates that SR-A and

CD36 are responsible for most of the observed uptake

Inhibition of RAGE by AGE–HSA did not decrease

uptake significantly Although RAGE is not an

endo-cytotic receptor, binding of AGE ligands to RAGE

has been shown to activate signaling pathways [49]

that potentially could have affected LDL uptake

The aldehyde concentrations utilized in this study

are higher than those reported for plasma from both

healthy controls and people with diabetes [23,24,50,51]

These plasma values (up to 0.5 mm [51]) are, however,

potentially misleading, as they represent only the

(small) fraction of these highly reactive species that has

not undergone reaction with plasma proteins, a process

that is known to be extremely rapid and efficient [52]

The true flux of these compounds is therefore likely to

be considerably higher Irrespective of this, it is clear

that the levels of these aldehydes are elevated in people

with diabetes [24] Furthermore, the levels of these

aldehydes may be substantially greater in the artery

wall than in plasma, as a result of cell-mediated

forma-tion of these species, with the major route to such

aldehydes being via the intracellular decomposition of

triose phosphates [53], the concentrations of which are

markedly elevated in hyperglycemia [54] It has also

been shown that the heme enzyme myeloperoxidase,

which is present at elevated levels at sites of

inflamma-tion (such as atherosclerotic lesions [55]) as a result of

the influx and activation of neutrophils and

mono-cytes, can oxidize free amino acids to reactive

alde-hydes, including methylglyoxal [56] Both these

processes might therefore be expected to give higher

levels of reactive aldehydes within tissues, and

partic-ularly at sites of inflammation, than would be present

in plasma Subendothelial entrapment of LDL [57–59]

may also result in more extensive LDL modification

than observed in the circulation, as a result of longer

exposure times

Overall, these studies have established that LDL

gly-cation, in the absence of significant oxidation, is

suffi-cient to induce lipid loading in primary human

macrophages, primarily via the scavenger receptors

SR-A and CD36 The accumulation of lipid in these

macrophages is accompanied by increased endocytosis

and degradation of apoB, with the difference in the

rates of the latter two processes resulting in

accumula-tion of modified apoB in HMDMs exposed to

glycolal-dehyde-modified LDL Thus, alglycolal-dehyde-modified LDL

may contribute to the increased atherosclerosis and

accumulation of glycated proteins observed in people with diabetes

Experimental procedures

Materials

Reagents were obtained from the following sources Sigma-Aldrich (Castle Hill, NSW, Australia): methylglyoxal, glycolaldehyde, fatty acid-free BSA, HSA, fucoidin, tryp-sin [type I, Na-benzoyl-l-arginine ethyl esters,  10 000 unitsÆ(mg protein))1], EDTA, Hank’s balanced salt solution (HBSS), PenStrep (100 unitsÆmL)1 penicillin, 0.1 mgÆmL)1 streptomycin), and Dulbecco’s NaCl⁄ Pi, (pH 7.4) BDH (Merck, Kilsyth, VIC, Australia): glucose Bio-Rad (Regents Park, NSW, Australia): Chelex-100 resin ICN (Seven Hills, NSW, Australia): CuSO4 Amersham Biosciences (Castle Hill, NSW, Australia): PD10 columns and Na125I (‡ 15 CiÆmg)1iodide) JRH Biosciences (CSL, North Ryde, NSW, Australia): RPMI-1640 medium Trace Scientific (Mel-bourne, VC, Australia): glutamine Australian Red Cross, Clarence St Blood Bank: human serum Axis-Shield (Oslo, Norway): Lymphoprep BD Biosciences-Pharmingen (San Diego, CA, USA): purified mouse anti-(human CD36) mAb All other chemicals were of analytical grade, and all solvents were of HPLC grade

Solutions were prepared with nanopure water (Milli Q system, Millipore-Waters, Lane Cove, NSW, Australia) treated with washed Chelex-100 resin to remove trace trans-ition metal ions, with the exception of tissue culture rea-gents, for which Baxter (Old Toongabbie, NSW, Australia) sterile, endotoxin-free, water, NaCl⁄ Pior HBSS were used

LDL modification

LDL was isolated as reported previously from multiple healthy male and female donors (four males, five females, aged 22–42 years) [29] 125I-Labeling of LDL was per-formed, prior to other modification, using iodine mono-chloride [36,60] Specific activity (typically 50–100 c.p.m.Æng)1 apoB protein) was determined by c-counting (Cobra II; Packard, Downers Grove, IL, USA) Acetylation

of LDL was performed as reported previously [29] Modifi-cation of LDL was performed as described previously [28] Briefly, sterile LDL (1 mg proteinÆmL)1) was incubated with 100 mm glycolaldehyde, methylglyoxal or glucose (± 1 lm CuSO4) in Chelex-treated NaCl⁄ Pi at 37C for

7 days Incubation controls contained 50 lm EDTA in place of glucose or aldehyde Excess reagents were removed

by elution of the LDL through PD10 columns before use Modification was confirmed by changes in relative elec-trophoretic mobility [29] LDL lipid composition (total cho-lesterol, free chocho-lesterol, triglycerides and phospholipids) was determined using a Roche Diagnostics⁄ Hitachi 902

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autoanalyzer (Roche Diagnostics GmbH, Mannheim,

Ger-many) [61,62] Cholesteryl ester concentrations were

calcu-lated as the difference between total and free cholesterol

concentrations

Isolation and culture of HMDMs

Monocytes were isolated by countercurrent elutriation

[63,64], using HBSS (with phenol red and 0.01% EDTA,

but without Ca2+ and Mg2+) White cell concentrates

were diluted 1 : 2 in HBSS, and 30 mL samples were

underlaid with 15 mL of Lymphoprep and centrifuged

using a Beckman (Palo Alto, CA, USA) GS–6KR

centri-fuge with a GH3Æ8 rotor (2060 g, 40 min, 22C)

Periph-eral mononuclear cells were isolated from the interface,

washed, and resuspended in 30 mL The cells were then

loaded into a Beckman Avanti J–20XPI centrifuge

equipped with a JE 5.0 elutriation rotor (770 g, flow rate

9 mLÆmin)1) The flow rate was increased by 1 mLÆmin)1

every 10 min, and the monocyte cell fractions collected

with flow rates of 15, 16, 17, 18 and, finally, 40 mLÆmin)1

were collected and combined The presence of monocytes

was confirmed by cytospinning and staining (Diff Quik,

Narrabeen, NSW, Australia) Cells were diluted (1.0· 106

cellsÆmL)1 in RPMI-1640, no serum), added to 12-well

plates (1 mL per well; Costar, Corning, NY, USA), and

left to adhere for 1–2 h Cells were then washed, and

RPMI medium [containing 10% heat-inactivated human

serum, 4 mm glutamine and 1% (v⁄ v) PenStrep] was

added; this was followed by incubation (5% CO2, 37C)

for 9–11 days, with the medium being changed every

3 days, to give matured HMDMs

Cellular cholesterol and cholesteryl ester analysis

HMDMs were exposed to 0 or 100 lgÆmL)1modified LDL

for 0–96 h in medium containing 10% lipoprotein-deficient

serum (prepared as reported previously [29]) Fresh LDL

and medium were added at 48 h Cell medium samples were

collected at the stated times, and the cells were washed and

lysed in water Cell viability was determined by assaying

lactate dehydrogenase release [29] Cellular cholesterol and

cholesteryl ester content was quantified using HPLC, as

described previously [29]

Cellular apoB accumulation and turnover

HMDMs were incubated with modified [125I]LDL (50 lg

proteinÆmL)1) as described above Cell medium (0.5 mL)

and cells (after being washed twice with cold NaCl⁄ Pi)

were sampled at the indicated times For turnover studies,

the [125I]LDL-containing medium was removed after the

accumulation phase The cells were then washed with

warm NaCl⁄ Pi, and medium containing 1 mgÆmL)1 BSA

was added; this was followed by incubation for 0–24 h

At the indicated times, medium (0.5 mL) was collected, and the cells were washed with cold NaCl⁄ Pi For both the accumulation and turnover studies, after the medium was collected, trypsin (1 mL, 0.01% w⁄ v) was added to the wells (60 min, 4C) to remove surface-bound ligand [36] This medium was retained to quantify cell surface-bound apoB Triton X-100 (1 mL, 0.1% v⁄ v) was then added (30 min, 4C) Of the resulting lysate, 0.5 mL was used to measure total intracellular radioactivity BSA (0.1 mL, 30 mgÆmL)1) and trichloroacetic acid (1 mL,

3 m) were added to the remaining lysate, and medium samples; this was followed by incubation (20 min, 4C) and centrifugation using a Sorvall (Sorvall Instruments, Newtown, CT, USA) RT600B centrifuge and a H1000B rotor (10 min, 1500 g, 4C) to precipitate proteins The supernatant (1 mL) was added to AgNO3 (0.25 mL, 0.7 m) and respun to precipitate free iodide One milliliter

of the iodide-free, trichloroacetic acid-soluble, supernatant from the medium or lysate was counted to quantify extra-cellular and intraextra-cellular degraded apoB, respectively [36] The medium and cell protein pellets were washed (3· 5%

w⁄ v trichloroacetic acid), and then counted to determine extracellular and intracellular nondegraded apoB, respect-ively

Receptor blocking

HMDMs were exposed to 0 or 100 lgÆmL)1 control or modified LDL for 48 h in medium containing 10% lipopro-tein-deficient serum with 200 lgÆmL)1 fucoidin [48],

2 lgÆmL)1 mAb to CD36 [47], or 200 lgÆmL)1 AGE–HSA [48] AGE–HSA was prepared by incubation of

20 mgÆmL)1 HSA with 1 m glucose for 4 weeks at 37C, followed by dialysis to remove unreacted glucose [65] At the end of 48 h, cell medium samples were collected, and the cells were washed and lysed in water Cell viability was determined by assaying lactate dehydrogenase release, and cellular cholesterol and cholesteryl ester content was quanti-fied by HPLC, as described above

Protein assay

Protein concentrations were quantified using the bicinchoni-nic acid assay (Pierce, Rockford, IL, USA) with 60 min of incubation at 60C, using BSA as a standard

Data analysis

Data are expressed as mean ± SEM from three or more separate experiments with triplicate samples One-way or two-way analysis of variance (anova) was used with Bon-ferroni’s post hoc analysis, with P < 0.05 taken as signifi-cant

Trang 10

This work was supported by grants from the Diabetes

Australia Research Trust and the Australian Research

Council B E Brown and I Rashid gratefully

acknow-ledge receipt of Australian Postgraduate Awards

administered through the University of Sydney The

authors thank Professor Roger T Dean and Associate

Professor Wendy Jessup for helpful discussions, and

Mr Pat Pisansarakit for the isolation of HMDMs

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