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17 b -Hydroxysteroid dehydrogenase type 11 is a major peroxisome proliferator-activated receptor a-regulated gene in mouse intestine Kiyoto Motojima Department of Biochemistry, Meiji Pha

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17 b -Hydroxysteroid dehydrogenase type 11 is a major peroxisome proliferator-activated receptor a-regulated gene in mouse intestine Kiyoto Motojima

Department of Biochemistry, Meiji Pharmaceutical University, Kiyose, Tokyo, Japan

In order to study the role of peroxisome

proliferator-acti-vated receptor a in mouse intestine, its agonist-induced

proteins were identified by peptide mass fingerprinting

fol-lowed by Northern blot analysis using their cDNAs One of

the most remarkably induced proteins was identified as

17b-hydroxysterol dehydrogenase type 11 Its very rapid

induction by various agonists was most efficient in intestine

and then in liver These findings together with recently

reported results showing the enzyme family’s wide substrate

spectrum, including not only glucocorticoids and sex ster-oids but also bile acids, fatty acids and branched chain amino acids, suggest new roles for both peroxisome proliferator-activated receptor a and 17b-hydroxysterol dehydrogenase type 11 in lipid metabolism and/or detoxification in the intestine

Keywords: PPAR; intestine; hydroxysteroid dehydrogenase; lipid metabolism

Peroxisome proliferator-activated receptors [PPARa, b(d),

and c] are members of the nuclear hormone receptor

superfamily and function as ligand-dependent transcription

factors, playing crucial roles in several processes including

energy metabolism, cellular differentiation, and

inflamma-tion [1,2] It is now well accepted that PPARa is particularly

important in lipid catabolism in the liver by upregulating

the expression of a variety of genes that encode proteins

involved in fatty acid transport [3], a-oxidation and

lipoprotein metabolism [4,5] However, it is important to

point out that these studies have been mostly carried out

using rodent models and strong synthetic PPARa agonists

PPARa was originally cloned from a mouse cDNA

library to explain a rodent-specific response called

per-oxisome proliferation to a variety of synthetic compounds

[6] The amount of PPARa in the mouse liver is 10 times

higher than that in human liver, and fibrates, hypolipidemic

drugs and PPARa agonists do not cause peroxisome

proliferation and a large induction of proteins involved in

lipid metabolism in human liver [7,8] Thus there is a

possibility that our knowledge on the role of PPARa in lipid

metabolism is biased against its extra-hepatic functions

In this study, I examined the PPARa agonist-induced

proteins in the intestine, another important organ for lipid

metabolism expressing a fairly large amount of PPARa in

mouse and human, to obtain new insight into the roles of

PPARa A major change in the intestine at the protein level,

namely a rapid induction of 17b-hydroxycholestrol

dehy-drogenase type 11 (17b-HSD-11) by PPARa ligand, was identified

Materials and methods Animals and treatment Normal male C57BL and PPARa-null mice [9] were kept under a 12-h light–dark cycle and provided with food and water ad libitum Mice were fed either a control diet or

a diet containing a drug at the concentration (%, w/w) and for the number of days or weeks indicated in the figure legends All animal procedures were approved by the Meiji Pharmaceutical University Committee for Ethics of Experi-mentation and Animal Care

Preparation of postnuclear fractions and SDS/PAGE analysis

The livers and intestinal mucosa from wild (C57BL) or PPARa-null mice fed a control or a diet containing Wy14 643 {[4-chloro-6-(2,3-xylidino)-2-pyrimidinyl-thio]acetic acid} purchased from Tokyo-Kasei, Tokyo, Japan) for

5 days were homogenized in five volumes of sucrose buffer [0.25M sucrose, 1 mM EDTA, 0.1% (v/v) ethanol, the protease inhibitor mixture (Wako, Tokyo, Japan), pH 7.4]

by Potter–Elvehjem homogenizer [10] The homogenates

were centrifuged for 13 min at 2000 g and the supernatant,

postnuclear fraction was obtained Total proteins in the intestinal postnuclear fraction of wild-type mice fed a diet containing 0.05% Wy14 643 were separated by SDS/PAGE (12% gel) as described previously [10]

Identification of Wy14643-induced proteins The proteins separated by SDS/PAGE were electric-ally transferred to a nylon membrane (Immobilon, Millipore, MA, USA) and stained with Coomassie blue The proteins of interest were excised from the membrane,

Correspondence toDepartment of Biochemistry, Meiji Pharmaceutical

University, 2-522-1 Noshio, Kiyose, Tokyo 204–8588, Japan.

Tel./Fax: +81 424 958474; E-mail: motojima@my-pharm.ac.jp

Abbreviations: FABP, fatty acid binding protein; HSD,

hydroxy-steroid dehydrogenase; PMF, peptide mass fingerprinting; PPAR,

peroxisome proliferator-activated receptor.

(Received 20 July 2004, revised 24 August 2004,

accepted 31 August 2004)

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carboxymethylated and digested with endoproteinase

Lys-C The resultant peptides were subsequently analyzed

by MALDI-TOF mass spectrometry The spectra were used

to identify the proteins, using theMS-FIT search program

[11] Each protein band contained two or more proteins

and the protein mass fingerprinting alone could not identify

the proteins of interest without ambiguity

RNA preparation and Northern blotting

Total RNA was prepared from the mouse tissues and

cultured cells by the acid guanidinium isothiocyanate/

phenol/chloroform extraction method [12] Northern

blot-ting analysis was carried out essentially as described

previously using Express Hyb hybridization solution

(Clon-tech, CA, USA) [13] The cDNAs used for probes were

described previously [3,14] or obtained by the cloning of

PCR products of cDNA synthesized from poly(A+) RNA

isolated from the liver of Wy14,543-fed mice The

synthe-ticoligonucleotides used to amplify the respective cDNA

sequences were 5¢- GGGAATTCGTTTAGGACCGGGA

ACGAGAGC-3¢ and 5¢-CCCTCGAGCGAAATCCCTG

CAAGCACCTGT-3¢ for 17b-HSD-11 (corresponding to

nucleotide numbers 62–860 of the published sequence with

additional nucleotides for restriction enzyme digestion

underlined; GenBank accession number AK049355);

5¢-GGGAATTCGACGGGCGTGTGGTGTTGGTCA-3¢ and 5¢-GGCTCGAGGAAGTGGCTTATACAGCTC

CAA-3¢ for 17b-HSD-4 (corresponding to nucleotide

num-bers 43–1273 of the published sequence with additional

nucleotides underlined; GenBank accession number

NM008292) The PCR products were digested with EcoRI

and XhoI, cloned into a plasmid vector, and sequenced for

identification

Cell culture and DNA transfection

Fao cells (a subclone of rat hepatoma HIIE cells) were

cultured in Ham’s F-12 medium, and CV-1 cells (monkey

kidney-derived cells) were cultured in minimal essential

medium under the conditions described previously [13]

A PPARa ligand Wy14 643 was added to the medium at

a final concentration of 50 lM (Fao cells) or 100 lM

(CV-1 cells) A 1.8 kb DNA fragment containing possible enhancer sequences in the 17b-HSD-11 gene promoter was amplified by PCR using the mouse genomic DNA and the oligonucleotide primers The entire fragment and digested enhancer truncated fragment were cloned into the enhancer vector pGL3 (Promega, WI, USA) Transfection was performed in 24-well plates with SuperFect (Qiagen, CA, USA) using the Dual Luciferase assay system (Promega) according to the manufacturer’s protocol [13]

Results and Discussion SDS/PAGE analysis of the proteins whose expression levels were regulated by PPARa and its ligand

To detect the protein bands whose expression levels were markedly altered by administration of a PPARa ligand, postnuclear fractions of the liver and intestine were prepared from mice fed a PPARa ligand for 5 days The result of one-dimensional SDS/PAGE analysis of these proteins from wild (C57BL) or PPARa-null mice fed a control or Wy14,643-containing diet is shown in Fig 1 As already reported [14,15], several proteins including peroxisomal enzymes were largely induced in the liver of wild mice by feeding Wy14 643 and it was difficult to assign uncharacterized new protein bands on one-dimensional gels In contrast, the number of affected protein bands was limited in the intestine of wild mice and we chose three protein bands as uniquely increased

in the intestine by Wy14 643 in a PPARa-dependent manner These include proteins having molecular masses of 32, 78 and

80 kDa as shown by arrows in Fig 1B

Peptide mass fingerprinting (PMF) analysis

of the PPARa-regulated proteins in the intestine Among the three proteins bands, I further selected P32 and P78 for PMF analysis, because they seemed to be expressed

Fig 1 Effects of Wy14 643 on protein expression in the liver and intestine of control and PPARa-null mice Wild-type (+/+) and PPARa-null mice (–/–) were fed either a control (–) diet or one containing 0.05% Wy14 643 (+) for 5 days The proteins in postnuclear fractions from the liver and intestine were analyzed by SDS/PAGE (10%, w/v) followed by staining with Coomassie brilliant blue (A) The portions (indicated by boxes) of the gel containing the induced proteins (indicated by arrows) in the intestine are shown enlarged (B).

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more in the intestine than in the liver and isolated from

other major protein bands on the one-dimensional gel After

enzymatic digestion using endoproteinase Lys-C and

ana-lysis of the resulting peptides by MALDI-TOF mass

spectrometry, the masses of 12 among 29 peptides derived

from P32 were consistent with those calculated from

the peptide sequences from 17b-HSD-11 (gi|16716597|

ref|NP_444492.1|), and the masses of 12 peptides matched

those from annexin IV (gi|7304889|ref|NP_038499.1|) The

masses of 18 among 79 peptides derived from P80 were

consistent with those calculated from the peptide sequences

from 17b-HSD-4 (gi|1706397|sp.|P51660|) The peptides

from P80 also contained 32 peptides from Ezrin

(gi|32363497|sp.|P26040|) and 18 peptides from P450

oxidoreductase (gi|6679421|ref|NP_032924.1|)

Among these proteins, 17b-HSD-4 is known as a

peroxisomal enzyme and induction of several peroxisomal

enzymes in the liver has been extensively studied [16,17]

17b-HSD-4 is not a major protein in the liver, but it could be

identified as a distinct protein band on the one dimensional

gel of all the proteins in the post nuclear fraction probably

because of the absence of abundant liver-specific proteins in

the intestine Furthermore, the increase of 17b-HSD-4

caused by the PPARa ligand in the liver as protein amount

was not remarkable when compared with that of mRNA,

and Corton et al suggested the possibility of

post-trans-lational regulation of the protein levels in the liver [16]

It was noteworthy that two types of 17b-HSDs were identified as the most remarkably increased proteins in the intestine by PPARa ligand in total protein mixture of the postnuclear fraction of the mouse intestine 17b-HSD-4 is a multifunctional protein involved in not only inactivation of estradiol but also successive steps of a-oxidation of long-and branched-chain fatty acids in peroxisomes In contrast, 17b-HSD-11 is a new member of the 17b-HSD family [18] Mouse 17b-HSD-11 was found from a large set of full-length cDNAs by sequence homology and functional annotation [19] and human 17b-HSD-11 was identified in expressed sequence tag databases with conserved domains

of the family members [20] and therefore its function has not been fully characterized yet [18] 17b-HSD-11 has no peroxisomal targeting signal at the C-terminus but a possible hydrophobic signal sequence at the N-terminus The N-terminal sequence was expected to be cleavable by signal peptidase (SignalP, http://www.cbs.dtu.dk) but the exact N-terminal sequence was detected during PMF analysis of P32 protein as shown in Table 1 Thus 17b-HSD-11 should be a membrane protein and our preliminary data using green fluorescence protein linked

to the C-terminus of the protein suggested association with the endoplasmic reticulum In contrast, Chai et al [20] recently reported that the myc-tagged human 17b-HSD-11

at the N-terminus localized in the cytoplasm The tagged myc sequence should have abolished the function of the

Table 1 Summary of PMF analysis of P32 and P80 The residue numbers for P32 are from the peptide sequence of 17b-HSD-11 and those for P80 are from that of 17b-HSD-4.

Observed m/z Theoretical MH+ Delta Residues Peptide sequence Modification P32

766.45 766.47 )0.02 283–288 K)HRINVK

898.5 898.47 0.03 289–296 K)FDAVVGYK

1000.6 1000.58 0.02 63–70 K)LVLWDINK

1692.9 1692.87 0.03 140–153 K)TFEVNVLAHFWTTK

2527.6 2527.58 0.02 3–24 K)YLLDLILLLPLLIVFSIESLVK

2577.26 2577.24 0.02 83–105 K)LGAQAHPFVVDCSQREEIYSAAK

2630.44 2630.43 0.01 33–58 K)SVAGEIVLITGAGHGIGRLTAYEFAK

2951.45 2951.48 )0.03 162–189 K)NNHGHIVTVASAAGHTVVPFLLAYCSSK

2984.54 2984.5 0.04 228–254 K)NPSTNLGPTLEPEEVVEHLMHGILTEK 0Met–ox P80

873.54 873.52 0.02 636–643 K)SVGREVVK

1001.61 1001.61 0 636–644 K)SVGREVVKK

1229.67 1229.64 0.03 579–588 K)EGNRIHFQTK

1315.73 1315.68 0.05 645–655 K)ANAVFEWHITK

152.7 1352.63 0.07 69–81 K)AVANYDVEAGEK

1597.98 1597.97 0.01 247–259 K)LRWERTLGAIVRK

1728.92 1728.97 )0.05 169–184 K)LGILGLCNTLAIEGRK

1985.99 1985.94 0.05 384–402 K)SMMNGGLAEVPGLSFNFAK 1Met–ox

2820.47 2820.4 0.07 302–330 K)VDSEGISPNRTSHAAPAATSGFVGAVGHK

2969.45 2969.42 )0.03 141–168 K)QNYGRILMTSSASGIYGNFGQANYSAAK 0Met–ox

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N-terminal leader sequence Table 1 summarizes

assign-ment of the peptide masses to 17b-HSD-11 and 17b-HSD-4

Northern blot analysis of 17b-HSD-11 mRNA

To confirm that intestinal expression of 17b-HSD-11 is

regulated by PPARa and Wy14,643, we analyzed the effect

of the drug on the levels of 17b-HSD-11 and 17b-HSD-4

mRNAs in the liver and intestine of wild-type or

PPARa-null mice (Fig 2) Two types 17b-HSD mRNAs were

largely induced in both the liver and intestine in a

PPARa-and ligPPARa-and-dependent manner Their inductions were more

outstanding than those of two typical PPARa-target gene

transcripts, liver-type fatty acid binding protein (L-FABP)

and intestine-type fatty acid binding protein (I-FABP)

mRNAs [3,21] When compared to each other, some

preference of 17b-HSD-11 for intestine and of 17b-HSD-4

for liver was observed Thus it was confirmed that

17b-HSD-11 is a new protein whose expression is regulated by

PPARa and its ligand in the intestine

17b-HSD-11 mRNA was efficiently induced by various

types of PPARa activators in addition to a potent

Wy14 643 (Fig 3) The time course of the induction was

very rapid not only in the liver but also in intestine (Fig 4)

and the rapid induction of the mRNA by Wy14 643 was

reproduced in the cultured hepatoma Fao cells (Fig 5)

Almost a maximal level of induction was achieved in both

tissues within a day, making a sharp contrast to the cases of

typical PPARa-target genes so far studied [3,13,21]

Tran-scription of the peroxisomal hydratase-dehydrogenase

(HD) and L-FABP genes is activated by PPARa within a

few hours and the mRNAs reach their maximal levels in a

day in the liver but not in intestine [13] The levels of their

mRNAs in intestine slowly increase during a few days of

feeding a diet containing Wy14 643 This slow time course

of induction is also the case for the intestine-specific

PPARa-target gene I-FABP [21] Thus the induction of

two 17b-HSD mRNAs by a PPAR ligand in the intestine is

much more efficient than that of typical PPARa-target genes

Promoter structure of the17b-HSD-11 gene and transcriptional regulation

All the above data strongly suggest that expression of the 17b-HSD-11 gene is directly regulated by PPARa and its ligand So the genome database was searched for the

Fig 2 Influence of PPARa and Wy14 643

on the expression levels of 17b-HSD-11 and 17b-HSD-4 mRNAs Wild-type (+/+) and PPARa-null mice (–/–) were fed either a con-trol (–) diet or one containing 0.05% (w/v) Wy14 643 for 5 days Total RNA from indi-vidual livers and intestines (5 lg) was analyzed

by Northern blotting using cDNAs for 17b-HSD-11, 17b-HSD-4, 17b-HSD-10, liver-type fatty acid binding protein (L-FABP), intes-tine-type fatty acid binding protein (I-FABP) and ribosomal S14 protein (S14, loading control).

Fig 3 PPARa activator specificity for 17b-HSD-11 mRNA induction

in the liver Wild-type mice were fed either a control diet or one containing 0.05% (w/v) Wy14,643, 0.5% (w/v) clofibrate, 2% (w/v) di(2-ethylhexyl)adipate (DEHA), or 2% (w/v) di(2-ethylhexyl)phtha-late (DEHP) for 5 days Total RNA isodi(2-ethylhexyl)phtha-lated from individual livers was subjected to Northern blot analysis using the cDNA probes for 17b-HSD-11, L-FABP, a2u-globulin (a2u), and apolipoprotein E (apoE, loading control).

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promoter sequence and PPAR binding site The mouse

17b-HSD-11 gene is located in cytoband E4 on

chromo-some 5 and the sequence has been published (accession

number, AL714024) Searching for a typical PPRE by

TRANSSEARCH program (http://www.cbrc.jp/research/db/

TFSEARCHJ.html) in the region between 3 kb upstream

and 2 kb downstream of the estimated transcriptional

start site from the 5¢ end of the reported cDNA [19]

showed no significantly similar motif The cloned

pro-moter sequence up to)1800 bp from the transcriptional

start site did not respond to a PPARa ligand Wy14 643

in the reporter gene assay (data not shown) Although an

essential role of PPARa in the ligand-dependent

tran-scriptional activation of the 17b-HSD-11 gene in the

intestine became clear, whether another region of the

gene is necessary or an unknown mechanism is operating

for the activation could not be clarified by the

conven-tional methods used in this study The molecular

mechanism of the unusual induction of the 17b-HSD-11

gene in the intestine is clearly important and we are

trying to solve this problem in our laboratory hoping to

uncover a new role of PPARa in this organ

Possible roles of 17b-HSD-11 in the intestine Mouse 17b-HSD-11 may reside not in the extracellular space as previously predicted but in the cell probably on the membrane as noted above Supporting this prospect, Chai

et al [20] recently reported that human normal liver parenchymal cells and epithelium of the endomerium and small intestine, as well as steroidogenic cells, were immuno-histochemically stained by anti-human 17b-HSD-11 Ig They also suggested that 17b-HSD-11 was localized to cytoplasm in the cell, but it should be associated with the endoplasmic reticulum (see above)

17b-HSD-11 belongs to the short-chain dehydrogenase/ reductase superfamily (SDR family member 8) and also has a protein domain of glucose/ribitol dehydrogenase (Mouse Genome Informatics, http://www.informatics jax.org) Recent studies on the specificities of several types of 17b-HSDs have revealed their wide substrate spectrum, including not only glucocorticoids and sex steroids but also bile acids, fatty acids and branched chain amino acids [18,22] Thus 17b-HSDs in the epithelium of the intestine may metabolize potentially toxic compounds included in the diet to protect the organism, as suggested by Chai et al [20] More work is required to address the in vivo function of 17b-HSD-11 and physiological significance of its rapid and marked induction by PPARa ligands in the intestine

Acknowledgements

The author thanks Dr A Iwamatsu (Central Laboratories for Key Technology, Kirin Brewery Co Ltd, Yokohama, Japan) for PMF analysis.

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