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These comprise 6% of the total yeast genes encoding 173 unknown proteins and 208 proteins related to folding, glycosyla-tion⁄ modification, translocation, protein degradation, Keywords e

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stress in Arabidopsis thaliana

Shinya Kamauchi, Hiromi Nakatani, Chiharu Nakano and Reiko Urade

Graduate School of Agriculture, Kyoto University, Uji, Japan

A nascent polypeptide synthesized on the rough

endoplasmic reticulum (ER) is translocated and

folded with the assistance of molecular chaperones

and other folding factors such as glycosylation⁄

modi-fication enzymes and disulfide oxidoreductases within

the ER However, the folding of nascent

polypep-tides occasionally does not occur, resulting in the

accumulation of unfolded or misfolded proteins in

the ER (ER stress) To solve this problem, eukaryotic

cells sense ER stress and induce a set of genes called

unfolded protein response (UPR) genes In the

bud-ding yeast Saccharomyces cerevisiae, ER

transmem-brane protein kinase⁄ riboendonuclease Ire 1p is activated by ER stress [1,2], and nonconventionally splices mRNA of basic leucine zipper transcription factor Hac 1p [3–5] Hac 1p is translated from the spliced mRNA and induces the UPR genes, having a UPR cis-acting regulatory element [6–8] On DNA microarray analysis, 381 genes have been identified

as UPR ones induced by both tunicamycin (TM) and dithiothreitol [9] These comprise  6% of the total yeast genes encoding 173 unknown proteins and 208 proteins related to folding, glycosyla-tion⁄ modification, translocation, protein degradation,

Keywords

endoplasmic reticulum; fluid microarray;

gene expression; tunicamycin; unfolded

protein response

Correspondence

R Urade, Graduate School of Agriculture,

Kyoto University, Uji, Kyoto 611-0011, Japan

Fax: +81 774 38 3758

Tel: +81 774 38 3757

E-mail: urade@kais.kyoto-u.ac.jp

Database

The nucleotide sequence data for soybean

SEL-1L are available in the DDBJ ⁄

EMBL ⁄ GenBank databases under accession

number AB197676.

(Received 15 March 2005, revised 11 May

2005, accepted 16 May 2005)

doi:10.1111/j.1742-4658.2005.04770.x

Eukaryotic cells respond to the accumulation of unfolded proteins in the endoplasmic reticulum (ER) In this case, so-called unfolded protein response (UPR) genes are induced We determined the transcriptional expression of Arabidopsis thaliana UPR genes by fluid microarray analysis

of tunicamycin-treated plantlets Two hundred and fifteen up-regulated genes and 17 down-regulated ones were identified These genes were reana-lyzed with functional DNA microarrays, using DNA fragments cloned through fluid microarray analysis Finally, 36 up-regulated and two down-regulated genes were recognized as UPR genes Among them, the up-regu-lation of genes related to protein degradation (HRD1, SEL-1L⁄ HRD3 and DER1), regulation of translation (P58IPK), and apoptosis (BAX inhibitor-1) was reconfirmed by real-time reverse transcriptase-PCR The induction of SEL-1L protein in an Arabidopsis membrane fraction on tunicamycin-treat-ment was demonstrated Phosphorylation of initiation factor-2a, which was inhibited by P58IPK, was decreased in tunicamycin-treated plantlets How-ever, regulatory changes in translation caused by ER stress were not detec-ted in Arabidopsis Plant cells appeared to have a strategy for overcoming

ER stress through enhancement of protein folding activity, degradation of unfolded proteins, and regulation of apoptosis, but not regulation of trans-lation

Abbreviations

AARE, amino acid response element; ATF6, activating transcription factor 6; AZC, L -azetidine-2-carboxylic acid; BI-1, Bax inhibitor-1; eIF2a, initiation factor-2a; Endo H, endoglycosidase H; ER, endoplasmic reticulum; ERAD, ER-associated protein degradation; ERSE, ER stress response element; MS, Murashige and Skoog medium; PDI, protein disulfide isomerase; PKR, double stranded RNA-activated protein kinase; P-UPRE, plant-specific UPR element; RAMP4, ribosomal-associated membrane protein 4; TM, tunicamycin; UPR, unfolded protein response; UPRE, UPR cis-acting regulatory element; XBP-1, X-box binding factor.

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vesicle trafficking⁄ transport, vacuolar protein sorting,

cell wall biogenesis, and lipid⁄ inositol metabolism

In comparison with those of yeast, the UPR genes

of mammalian cells are induced through a much more

complicated mechanism, which has been shown to be

triggered by at least three transcription factors, X-box

binding factor (XBP-1), activating transcription

fac-tor 6 (ATF6), and ATF4 [10] The mammalian paralog

of yeast Ire 1p is activated by ER stress and splices

the invalid mRNA into mature mRNA encoding

371-amino acid XBP-1 [11,12] XBP-1 translated from the

spliced mRNA is translocated to the nucleus [13],

where it binds to its target sequence in the regulatory

regions of the P58IPK, ERdj4, HEDJ, EDEM, protein

disulfide isomerase (PDI)-P5, ribosomal-associated

membrane protein 4 (RAMP4), DnaJ⁄ HSP40-like

genes, etc [14] ATF6 is an ER transmembrane protein

that senses ER stress through its luminal domain, and

then moves to Golgi bodies to be cleaved by site-1 and

site-2 proteases [15–17] The cleaved ATF6 cytoplasmic

domain is released from Golgi membranes into the

nucleus, where it induces, in the presence of nuclear

factor Y, ER chaperone genes including BIP, GRP94,

Calreticulin and ORP150, which have an ER stress

response element (ERSE) in their regulatory regions

[18,19] PERK is an interferone-induced double

stran-ded RNA-activated protein kinase (PKR)-related

pro-tein that senses ER stress through its luminal domain

and then phosphorylates initiation factor-2a (eIF2a),

resulting in inhibition of bulk protein translation

[20,21] and stimulation of translation of ATF4 [22]

ATF4 is a basic leucine zipper transcription factor that

induces the transcription of many amino acid synthetic

enzymes and amino acid transporters by binding to

the amino acid response element (AARE) in the

regu-latory regions of these genes [23] ATF4 has also been

shown to stimulate the transcription of CHOP, which

is important for apoptotic cell death [24]

In contrast to the UPR mechanism(s) in yeast and

animal cells, that of plant cells is not well understood

Putative plant paralogs of yeast Ire1p have been found

in Arabidopsis thaliana and Oryza sativa [25,26] Their

N-terminal luminal domains have each been shown to

function as a sensor for ER stress in yeast However,

neither target mRNAs of transcription factors for

plant Ire1p nor target genes induced by this system

have been identified On the other hand, the mRNAs

of BiP, calreticulin, calnexin and PDI have been shown

to be induced on treatment with TM and dithiothreitol

in Arabidopsis, Zea mays, Phaseolus vulgalis, Glycine

max and Nicotiana tabacum on northern analysis [27–

31] The 21 UPR genes up-regulated by the stress

induced by both TM and dithiothreitol have been

identified among 8297 genes of the  27 000 protein-coding genes of Arabidopsis with an Affimetrix Gene-Chips [32]

In this paper, we present a list of the UPR genes of Arabidopsis identified among all the protein-coding genes In order to increase the accuracy of the list, the genes selected on fluid microarray analysis were reana-lyzed by functional DNA microarray analysis In addi-tion to the genes related to protein folding and degradation, genes related to protein translation and apoptosis are also included in the list

Results

Fluid microarray analysis of gene expression

on TM-treatment

To identify UPR genes among all the genes expressed

in Arabidopsis, we adopted the fluid microarray method, by which target genes can be cloned from selected fluid microarray beads The fluid microarray beads and probes for array analysis were prepared using the mRNA from plantlets treated with or with-out TM for 6 h BiP mRNA, a representative UPR gene, in TM-treated plantlets, was shown to increase 5.7 times compared to the level in untreated plantlets

on real-time RT-PCR analysis For the control experi-ment, competitive hybridization and sorting of the beads with a cell sorter were performed on 4· 104 beads with a 1 : 1 mixture of the probes, which had been prepared from noninduced plantlets, and differen-tially labeled with Cy5 and fluorescein In the control experiment, almost all of the beads after the control hybridization were sorted in the diagonal line region, the fluorescence intensities for fluorescein and Cy5 being the same (Fig 1A) Based on the distribution of beads in this experiment, we set three gates to collect beads, i.e., for ones more heavily labeled with Cy5 (U1 and U2) and fluorescein (D) For differential gene expression analysis, probes from TM-treated plantlets were labeled with Cy5 Probes from nontreated plant-lets were labeled with fluorescein Then 4· 105 beads were hybridized with a 1 : 1 mixture of the two types

of probes For analysis of differential gene expression,

1473 and 1703 beads were collected in fractions U1 and U2 of the up-regulated genes, and 3550 beads in fraction D of the down-regulated genes (Figs 1B and 2A) The DNA fragments on beads in these fractions were amplified by PCR and then sequenced In the up-regulated fractions, 215 genes (Table S1) were found as clusters of clones, which were identified on more than two beads, and 412 as singlet clones, which were identified on single beads (Table S2) For the

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down-regulated fraction, 10% of the total beads were

analyzed to reveal 17 genes as clusters of clones

(Table 1) and 34 as singlet clones (Table S2)

Analysis with functional DNA microarrays

In order to increase the accuracy of the list of UPR

genes, we reanalyzed the genes selected on fluid

micro-array analysis with functional DNA micromicro-arrays The

functional DNA microarrays were prepared by

spot-ting PCR fragments from the 215 up-regulated cluster

genes (Table S1) and the 17 down-regulated cluster

genes (Table 1) cloned on fluid microarray analysis

Singlet genes were omitted from the functional DNA

microarray analysis, because the list of singlet genes

was predicted to contain missorted non-UPR genes

at a high frequency Functional DNA microarray

analyses were performed with mRNA preparations

from plantlets treated with or without TM,

dithio-threitol or l-azetidine-2-carboxylic acid (AZC) AZC

is a proline analog that is incorporated in nascent

polypeptides instead of proline and prevents the

fold-ing of the polypeptides [33] Induction of BiP mRNA

by dithiothreitol- or AZC-treatment (3 h or 17 h,

respectively) was confirmed to be 3.4 or 22-times

higher than that in untreated plantlets on real-time

RT-PCR analysis To identify the up-regulated UPR

genes, it was required that candidate UPR genes

show a mean fold variation of greater than 1.2-fold

with all the treatments with TM, dithiothreitol and

AZC In addition, from the list, we eliminated the

genes in which the degree of variation was lower

than the sum of the background variation and twice

the standard deviation The degree of background

variation was obtained by means of a self⁄ self hybridi-zation experiment with Cy5 or Cy3-labeled target DNA fragments prepared from nontreated plantlet mRNA Thus, the expression difference between selec-ted genes was regarded as being significant below a probability of error of 5% Thirty-six genes were con-firmed to be induced under the three different induct-ive conditions, because these genes satisfied this criterion (Fig 2B and Table 2) These genes com-prised 30 for which some functional information was available and six for which no information was avail-able Among them, 27 genes were putative paralogs that have been reported to be UPR genes in yeast and⁄ or mammalian cells The functional categories comprise protein folding (13 genes), translocation (six genes), ER-associated protein degradation (ERAD) (three genes; HRD1-like, SEL-1L⁄ HRD3-like, and DER1-like), protein glycosylation and modification (two genes), regulation of translation (P58IPK) [34], and vesicle trafficking (two genes) The induction of HRD1-like, SEL-1L⁄ HRD3-like, DER1-like, and P58IPK mRNA was confirmed by real-time RT-PCR analysis (Fig 3) In addition, we found that an anti-apoptosis protein, Bax inhibitor-1 (BI-1) [35,36], was also included in the list of up-regulated UPR genes Induction of this paralog by ER stress in organisms other than plants has not been reported The induc-tion of BI-1 mRNA by ER stress in Arabidopsis was confirmed by real-time RT-PCR analysis (Fig 3) Furthermore, the induction (1.5-fold variation) of Homo sapiens BI-1 by TM-treatment for 24 h was confirmed in Hep G2 cells, a cell line derived from a human hepatoma, by real-time RT-PCR (data not shown)

Fig 1 Competitive hybridization on fluid microarrays (A) Control hybridization: 4 · 10 4

beads were hybridized with a 1 : 1 mixture of differ-entially labeled probes from noninduced plantlets (B) Competitive hybridization: 4 · 10 5 beads were hybridized with a 1 : 1 mixture of cDNA probes prepared from induced (Cy5) and noninduced plantlets (fluorescein) as described under Experimental procedures After hybridization, beads that went to gates U1, U2 and D were collected and subjected to gene analysis as described under Experimental procedures.

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To identify the down-regulated UPR genes, we

required that candidate UPR genes show a mean fold

variation of lower than 0.8-fold with all the treatments

with TM, dithiothreitol and AZC Two genes encoding

vegetative storage proteins, Vsp1 and Vsp2 [37,38],

sat-isfied this criterion Vsp2-beads comprised 58% of the

beads collected and were analyzed at gate D

Putative cis-acting regulatory element

of UPR genes

In yeast, ER stress activates Ire1p, which triggers the nonconventional splicing of HAC1 mRNA [3–5] Hac1p produced from the spliced mRNA induces the transcription of UPR genes by binding to their UPR cis-acting regulatory element (UPRE), CAGCGTG [6–8] In mammals, four kinds of cis-acting regulatory elements, which respond to ER stress, are known Mammalian UPRE (TGACGTG-T⁄ G) has been shown to be the specific cis-acting regulatory element for XBP1 and is referred to as the XBP1 binding site [39,40] ERSE (CCAAT-N9-CCACG) has been found

to be recognized by both ATF6 and XBP1 in vitro [41] ERSEII (ATTGG-N-CCACG) has also been demonstrated to be a target of ATF6 [42] Binding of ATF6 to these cis-acting regulatory elements occurs in collaboration with general transcription factor nuclear factor-Y [43,44] AARE (C⁄ EBT-ATF) (TT-G⁄ T-CATCA), which was discovered in the CHOP pro-moter, is recognized by ATF4, translation of which is accelerated by ER stress [24] In plants, a plant-specific UPR element (P-UPRE) (ATTGGTCCACGTCATC), which contains two mammalian UPR cis-acting regula-tory elements such as ERSEII and XBP1 binding sequences, was found in the 5¢ upstream regions of the BiPand calnexin genes [45] Furthermore, complement-ary sequences to the mammalian ERSE and XBP1 binding sequences have been found in the 5¢ upstream regions of several genes that are induced by TM- or dithiothreitol-treatment [32,45] Therefore, we searched for P-UPRE, the XBP1 binding sequence, ERSE, AARE, or complementary sequences in the 5¢ upstream regions (up to 1000 nucleotides) of the UPR genes Sin-gle or plural putative cis-acting regulatory elements were found in the 5¢ upstream regions of 28 of the 36 up-regulated genes (Fig 2C and Table 3) No cis-acting regulatory element sequence was found in the 5¢ upstream regions of the two down-regulated genes

Increase in putative SEL-1L due to ER stress

in Arabidopsis

In yeast and mammalian cells, the HRD1⁄ HRD3 (SEL-1L) ubiquitination system coupled to protein degradation by 26S proteasomes is known to be induced to remove unfolded proteins under ER stress [9,46] Plant paralogs of these genes have not been identified yet In this study, the transcriptional induc-tion of genes homologous to mammalian HRD1 and SEL-1L [47–49] was observed (Fig 3) Then, HRD1-and SEL-1L-like cDNAs were cloned with mRNA of

Fig 2 Overview of the fluid microarray and functional microarray

analyses (A) Gene selection by fluid microarray analysis Gates,

U1, U2 and D were set as shown in Fig 1B Singlet, a gene

identi-fied on a single bead Cluster, a gene identiidenti-fied on more than two

beads (B) Analysis with functional DNA microarrays The genes

selected in (A) were analyzed Two hundred and thirty-two genes

(215 up-regulated cluster and 17 down-regulated cluster genes)

were spotted on functional DNA microarrays The functional DNA

microarray analysis was carried out with target DNA fragments

pre-pared from the mRNA of control plantlets or plantlets treated with

tunicamycin (TM), dithiothreitol (DTT) or L -azetidine-2-carboxylic acid

(AZC) as described under Experimental procedures The numbers

are the numbers of genes that showed an expression difference

between control plantlets and plantlets treated with TM, DTT or

AZC The numbers in the ‘Overlap’ row are the numbers of

overlap-ping up-regulated genes or down-regulated genes upon treatments

with the three reagents (C) Venn diagram of the numbers of

over-lapping and nonoverover-lapping putative UPR cis-acting regulatory

ele-ments of the 36 up-regulated genes selected in (B) The numbers

in parentheses are the numbers of genes that have a cis-acting

reg-ulatory element Bold letters are the numbers of overlapping genes.

ERSE, CCAAT-N9-(A ⁄ C)CACG; XbpI, TGACGTG(G ⁄ T); P-UPRE,

ATTGG(T ⁄ G)CCACGTCAT; AARE, TT(G ⁄ T)CATCA.

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Arabidopsis plantlets by RT-PCR Their nucleotide

sequences coincided with those presented in the

data-base of ‘The Arabidopsis Information Resource’

(http://www.arabidopsis.org/) The putative amino acid

sequence of an HRD1-like protein contained an

N-ter-minal signal sequence and five membrane-spanning

regions (data not shown) The recombinant luminal

domain of the HRD1-like protein was expressed in

Escherichia coliand purified Unfortunately,

autoubiq-uitination activity was not detected for the

recombin-ant HRD1-like protein On the other hand, the

putative amino acid sequence of Arabidopsis SEL-1L

(At SEL-1L) contained an N-terminal signal sequence

(Met1–Glu20), two N-glycosylation consensus

seq-uences, and a membrane-spanning region (Phe623–

Arg643) near the C-terminus (data not shown) The

amino acid sequence of a soybean paralog of SEL-1L,

which was deduced from the nucleotide sequence of

cDNA cloned from young leaves by RT-PCR, was

clo-sely similar to Arabidopsis ones (data not shown)

Anti-(At SEL-1L) serum was prepared with the

recom-binant luminal domain (Phe21–Val622) of At SEL-1L,

which was expressed in E coli and isolated The

anti-serum only immunoreacted with a 74 kDa protein of

control plantlets on western blotting analysis (Fig 4A)

With TM-treatment, the 74 kDa protein gradually

decreased and a 70 kDa band began to appear at 4 h

after the treatment During the next 24 h, the 70 kDa

band significantly increased The size of the 74 kDa

band decreased to 70 kDa on endoglycosidase H (Endo H) digestion On the other hand, the 70 kDa band was insensitive to Endo H (Fig 4B) From these results, the 70 kDa protein was thought to be a non-glycosylated form of At SEL-1L On cell fractionation,

At SEL-1L was assumed to be a membrane protein, as judging from the existence of a putative membrane spanning region (Fig 4C) The 70 kDa band of plant-lets treated with TM for 24 or 48 h was denser than the 74 kDa band of the control plantlets (Fig 4B) Thus, it was suggested that At SEL-1L polypeptides were synthesized from the At SEL-1L mRNA induced

by ER stress, but that N-glycosylation of newly syn-thesized At SEL-1L molecules was inhibited by TM

ER stress and phosphorylation of eIF2a

In this study, we found that the mRNA of P58IPKwas induced by ER stress (Table 2 and Fig 3) P58IPKwas first identified as an inhibitor of interferon-induced PKR in mammalian cells [50] The PKR family responds to different stress signals and attenuates translation by phosphorylating the specific serine resi-due of eIF2a [51] to protect cells from the stress P58IPK inhibits PKR-mediated translational arrest by inactivating the kinase by binding to the domain of PKR family members In mammals, ER stress also causes translational arrest through phosphorylation

of eIF2a by PKR-like ER kinase, PERK [20,52]

Table 1 Genes recovered at gate D and functional DNA microarray analysis of them Tunicamycin (TM), dithiothreitol (DTT) and L -azetidine-2-carboxylic acid (AZC) values are means for six experiments Control ratio obtained on competitive hybridization with Cy5- and Cy3-labeled control mRNA; values are means for six experiments SD, standard deviation; n.d., not determined.

AGI gene Description

Fluid microbead array (number of beads)

Functional DNA microarray (fold variation)

At3g04120 Glyceraldehyde-3-phosphate dehydrogenase C subunit 0 0 2 0.68 0.99 0.98 1.01 (0.03)

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Table 2 Genes up-regulated by ER stress Tunicamycin (TM), dithiothreitol (DTT) and L -azetidine-2-carboxylic acid (AZC) values are means for six experiments Control ratio obtained on competitive hybridization with Cy5- and Cy3-labeled control mRNA; values are means for six experiments SD, standard deviation.

AGI gene Description

Fluid microbead array (number of beads) Functional DNA microarray (fold variation)

PROTEIN FOLDING

GLYCOSYLATION ⁄ MODIFICATION

At2g02810 UDP-glucose ⁄ UDP-galactose

transporter a,b

At2g41490 UDP-GlcNac:dolichol phosphate

N-acetyl-glucosamine-1-phosphate

transferase a

TRANSLOCATION

PROTEIN DEGRADATION

TRANSLATION

VESICLE TRAFFICKING

ANTI-APOPTOSIS

UNCLASSIFIED

At5g09410 Similar to anther ethylene-up-regulated

calmodulin-binding protein ER1

UNKNOWN

a Gene identified by Martı`nez and Chrispeels [32] b Genes identified by Noh et al [54].

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Mammalian P58IPKhas been shown to be induced at a

later phase of ER stress [53] Deletion of P58IPK has

been reported to result in an increase in

phosphory-lated eIF2a Hence P58IPK is thought to function as a

feedback regulator for translational regulation in the

later phase of ER stress The phosphorylated Ser51 of

eIF2a in plantlets was examined during ER stress by

western blot analysis (Fig 5A) The level of

phosphor-ylated eIF2a (Ser51) in the plantlets treated with TM

was lower than that in untreated plantlets The

phos-phorylated eIF2a increased again on removal of TM

from the medium after 6 h of treatment However, the

protein synthesis in plantlets, which was assayed as the

incorporation of [35S]-labeled Met and Cys into

nas-cent proteins, was not affected by TM-treatment

(Fig 5B)

Discussion

In this study, we tried to make a list of the UPR genes

in Arabidopsis In total, 215 up-regulated and 17

down-regulated cluster genes were cloned from mRNA

of Arabidopsis plantlets treated with TM on fluid

microarray analysis A functional DNA array was

pre-pared by using the cloned gene fragments, and then

used for analysis Among the 215 up-regulated cluster

genes, only 63 showed statistically positive signals on

functional DNA array analysis, showing differences in

the expression of target mRNA of the plantlets treated

with or without TM Because the fluid microarray

beads included a large number with highly expressed housekeeping genes, some of them might be missorted

at the gates, which would expand the list of genes Of the beads collected at gates U1 and D on fluid micro-array analysis, 89 and 87% were regarded as up-regu-lated and down-reguup-regu-lated genes on functional DNA microarray analysis, respectively On the other hand, 38% of the beads collected at gate U2 were regarded

as up-regulated genes on functional DNA microarray analysis This suggests that the discrepancy between the values obtained in the two analyses is mainly due

to the beads missorted at gate U2 However, of the rest, the 50 genes that showed no up-regulated signal for the plantlets treated with TM showed an up-regula-ted signal in the plantlets treaup-regula-ted with dithiothreitol and⁄ or AZC In addition, 23 of the genes that showed

no difference in expression on DNA microarray analy-sis between plantlets treated and untreated with TM had putative UPR cis-acting regulatory elements in their upstream regions Furthermore, 27 of the 63 genes were eliminated on functional DNA microarray analysis from the list by setting some criteria There-fore, the remaining 36 genes, which satisfied these criteria, were considered to be reliable up-regulated UPR genes Among these 36 genes, 12 coincided with up-regulated UPR genes previously identified on ana-lysis with an Affimetrix GeneChips loaded with 8297 Arabidopsis probe sets [32,54] Two down-regulated genes, Vsp1 and Vsp2, which satisfied all the criteria, are known to be for temporary nitrogen-storage pro-teins [38], and are subject to regulation by sugars, light, phosphates, nitrogen, wounding, auxins, jasmo-nates and oxidative-stress [55] The down-regulation of Vsp1 and Vsp2 may result in an increase in the intra-cellular amino acid pool, which may play an important role in the recovery from ER stress In mammalian cells, ER stress affects cellular amino acid metabolism via the PERK⁄ ATF4-mediated signaling pathway, which induces some amino acid synthesis- and trans-port-related genes [23] No putative UPR cis-acting regulatory element was found in the 5¢ upstream regions of Arabidopsis Vsp1 and Vsp2 Therefore, it is not clear whether these genes are directly regulated by the UPR system or down-regulated by a metabolic dis-order caused by ER stress

Thirteen genes, which encode six protein families responsible for protein folding, are included in the UPRgene list Among them, BiP (three genes),

calnex-in(two genes), calreticulin (two genes), and AtHSP

90-7 (one gene) have been shown to be induced by ER stress on northern blotting [25,54] Four genes enco-ding PDI families are also included in the list PDI and its family members are characterized by the

pres-Fig 3 Confirmation of transcriptional induction of six genes by

real-time RT-PCR analysis The amounts of actin, BiP, HRD1,

SEL-1L, DER1, p58 IPK and BI-1 mRNAs in total RNA from Arabidopsis

plantlets treated with TM (black bars), DTT (hatched bars), or AZC

(white bars) for 2 h were determined by real-time RT-PCR as

des-cribed under Experimental procedures The value for each mRNA

was standardized to the value for actin mRNA in the corresponding

total RNA preparation Fold expression change was calculated as

the ratio of mRNA in the plantlets treated and untreated with a

stress reagent Each value represents the mean for two

experi-ments.

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Table 3 Putative cis-acting regulatory elements of genes up-regulated by ER stress Position designated from the 5¢ terminus of the ATG initiation codon Lowercase letters in sequences correspond to N9 in ERSE-like sequence CCAAT-N9-(A/C) CACG.

AGI gene Description

cis-Acting regulatory element

ERSE-like CGTGTctgcttgtgATTGG(220–202)

Xbp1 binding-like TGACGTGG(240–233)

Xbp1 binding-like CCACGTCA(253–246)

Xbp1 binding-like TGACGTGT(131–124)

ERSE-like CCAATtacaattgtACACG(134–116) At2g02810 Similar to UDP-glucose ⁄ UDP-galactose transporter –

At2g41490 UDP-GlcNac:dolichol phosphate

Xbp1 binding-like TGACGTGT(322–315)

ERSE-like CGTGTaataatataATTGG(146–128)

ERSE-like CGTGTttaattatcATTGG(304–286)

Xbp1 binding-like TGACGTGG(477–470) Xbp1 binding-like ACACGTCA(609–602) At4g21730 Similar to NEM-sensitive fusion protein –

At5g09410 Similar to anther ethylene-up-regulated

Xbp1 binding-like TGACGTGG(396–389)

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ence of one or two thioredoxin homologous motifs per

molecule Yeast and mammalian PDIs are known as

multifunctional folding catalysts and molecular

chaper-ones, which catalyze the formation and rearrangement

of disulfide bonds between correct pairs of cysteine

residues in nascent polypeptide chains in the ER [56]

Mammalian PDI functions not only as a catalytic

enzyme but also as a subunit of microsome

triacylglyc-erol transfer protein [57] and prolylhydroxylase [58]

Mammalian PDI family ER-60⁄ ERp57, which also

exhibits protein oxidoreductase activity, interacts and

cooperates with calnexin or calreticulin for oxidative

folding of N-glycosylated proteins [59–61] The genes

of these PDI families are UPR genes [41] In the

Ara-bidopsisgenome, 13 genes encoding putative

PDI-rela-ted proteins, i.e At1g04980 (NP 171990), At1g07960

(NP172274), At1g15020 (NP 172955), At1g35620 (NP

564462), At1g21750 (NP 173594), At1g52260

(NP 175636), At1g77510 (NP 177875), At2g01270 (NP

565258), At2g32920 (NP 180851), At2g47470

(NP182269), At3g54960 (NP 191056), At3g16110 (NP

188232), and At5g60640 (NP 568926), were found

Identification and characterization of these PDI family

proteins were not carried out However, they were

sup-posed to play important roles in protein folding, as

four PDI-related genes among the above 13 genes were

confirmed to be induced by ER stress A gene enco-ding cyclophilin family protein ATCYP20-1 was identi-fied as a UPR gene Twenty-nine genes encoding cyclophilin family members were found in the Arabi-dopsis genome [62] Among them, five gene products are assumed to be targeted to the ER lumen with N-terminal signal peptides Among them, ATCYP20-1 has the amino acid sequence RFWH, which is an essential sequence for peptidyl prolyl cis, trans iso-merase activity Hence, it is suggested that ATCYP20-1 may participate in the folding of proteins in the ER The genes of six translocation-related proteins were found to be induced In mammalian cells and yeast, translocon subunit proteins are thought to be induced

to enhance retrotranslocation of unfolded proteins from the ER to the cytosol [63] The retrotranslocated proteins are degraded by 26S proteasomes Recently,

in tobacco, a GFP-fusion protein containing the P region of calreticulin, which is a model of a misfolded

A

B

C

Fig 4 Increase in At SEL-1L in the membranes of Arabidopsis

plantlets on TM-treatment (A) Plantlets were incubated in the

pres-ence (lanes 7–12) or abspres-ence of TM (lanes 1–6) for the indicated

times Proteins were extracted and then subjected to SDS ⁄ PAGE.

At SEL-1L was stained by western blotting with antiserum as

des-cribed under Experimental procedures (B) Plantlets were incubated

in the presence (lanes 3 and 4) or absence of TM (lanes 1 and 2)

for 48 h Proteins were extracted, digested with (lanes 2 and 4) or

without (lanes 1 and 3) Endo H, and then subjected to SDS ⁄ PAGE.

At SEL-1L was stained by western blotting with antiserum as

des-cribed under Experimental procedures (C) The total (lane 1),

super-natant (lane 2), and membrane (lane 3) fractions obtained from the

plantlets treated with TM for 48 h on centrifugation at 100 000 g

were subjected to SDS ⁄ PAGE, and At SEL-1L was stained by

western blotting with antiserum as described under Experimental

procedures.

A

B

Fig 5 Effect of TM-treatment on phosphorylation of eIF2a Plant-lets were incubated in the medium with TM for 6 h (lane 2), 7 h (lane 3), or 9 h (lane 4), or without TM for 9 h (lane 1) as described under Experimental procedures In other experiments, plantlets were incubated in the medium with TM for 6 h and then incubated

in the medium without TM for an additional 1 h (lane 5) or 2 h (lane 6) (A) After the incubation, the proteins were extracted from the plantlets and subjected to SDS ⁄ PAGE Phosphorylated Ser51 of eIF2a was determined by western blot analysis as described under Experimental procedures (B) After the incubation, proteins of the plantlets were metabolically labeled with [ 35 S]Met and [ 35 S]Cys for

20 min at 25 C Then, the proteins were extracted and subjected

to SDS ⁄ PAGE Labeled proteins were determined by fluorography

as described under Experimental procedures.

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protein in the ER, was shown to be retrotranslocated

to the cytosol, ubiquitinated, and then degraded [64]

The induction of translocon subunits by ER stress in

Arabidopsis suggests that an ERAD system similar to

those of yeast or mammalian cells may remove

mis-folded proteins produced in the ER of plant cells This

is supported by our finding that the genes encoding

putative plant DER1, HRD1 and SEL-1L⁄ HRD3 were

also induced by ER stress DER1 is a hydrophobic

protein that is localized to the ER In yeast, deletion

of DER1 prevents degradation of unfolded proteins,

suggesting that the function of DER1 may be

specific-ally required for ERAD [65] Yeast HRD1 is an

ER-membrane-anchored ubiquitin ligase, which is required

for the degradation and ubiquitination of several

ERAD substrates, and is associated with relevant

ubiquitin-conjugating enzymes [46] At HRD1, which

has the same nucleotide sequence as that registered in

‘The Arabidopsis Information Resource’, was cloned

by RT-PCR with mRNA from Arabidopsis Six

trans-membrane regions and a RING-H2 domain of

Arabi-dopsis HRD1 (At HRD1) showed high sequence

homology with those of yeast and human HRD1s

Unfortunately, it is unclear whether or not At HRD1

functions as an ubiquitin ligase, as the cytosolic

domain of At HRD1, which was expressed in E coli

and isolated, showed no self-ubiquitination activity

with an in vitro assay system involving commercial

human E1 and yeast E2 (UbCH5c) Yeast HRD3 is an

ER-resident glycoprotein with a single span near the

C-terminus, which stabilizes HRD1 and regulates the

cytosolic HRD1 RING-H2 domain through

interac-tion with the HRD1 transmembrane domain [66] We

showed that At SEL-1L was a membrane-anchored

glycoprotein and that it increased under ER stress In

order to clarify the details of the mechanism of plant

ERAD, functional characterization of these proteins

must be performed

In mammalian cells, ER stress responses are

com-posed of three steps, i.e., enhancement of the refolding

and degradation of unfolded proteins, attenuation of

translation [20,21], and apoptosis [24] ER stress has

not been found to cause attenuation of translation in

plants In this study, we found that the P58IPK gene

was up-regulated by ER stress Mammalian P58IPK is

induced at a later phase of ER stress and inhibits

PKR-mediated translational arrest by binding to the

kinase domain of the PKR family [53] However, bulk

protein translation of Arabidopsis was not affected by

ER stress, even though the phosphorylation of eIF2a

(Ser51) was partially inhibited by ER stress The

phos-phorylation of eIF2a (Ser51) increases the translational

efficiency of yeast GCN4 mRNA and mammalian

ATF4 mRNA, which have four and two upstream open reading frames in the 5¢ noncoding portion, respectively [67,68] Induction of Arabidopsis P58IPK followed by a decrease in the phosphorylation of eIF2a (Ser51) may increase the translational efficiency for unidentified gene(s)

It is unclear whether apoptosis may function as a UPR in plants, although inhibition of ER-type IIA

Ca2+-pumps has been reported to induce ER stress and apoptosis in soybean cells [69] In this study, we identified apoptosis-related gene BI-1 as a UPR gene BI-1 is an evolutionarily conserved integral membrane protein localized in the ER [35,36] In mammalian cells, BI-1 affords protection from apoptosis induced

by ER stress by inhibiting BAX activation and translo-cation to mitochondria, by preserving the mitochond-rial membrane potential, and by suppressing caspase activation [70] BAX and Bcl2, and their relatives were not found in plants However, in rice and barley, BI-1 has been shown to suppress fungal elicitor-induced apoptosis [71,72]

Experimental procedures

Plant materials and treatments Sterile seeds of Arabidopsis thaliana (Columbia) were germi-nated in 0.5· Murashige and Skoog medium [73] containing 1% (w⁄ v) sucrose (MS), and cultured for two weeks To prepare a cDNA tagged library and probes for transcrip-tome analysis with fluid microarrays or functional DNA microarrays, whole plantlets were treated by immersing

their roots in MS containing 5 lgÆmL)1TM, 1 mm dithio-threitol or 50 mm AZC for the indicated times For the control experiment, plantlets were treated with MS without stress reagents For relative quantification of mRNA by real-time RT-PCR, and pulse-labeling experiments with [35S]Met and [35S]Cys, the upper parts of plants were cut off from their roots and immersed in MS with a stress rea-gent

Real-time RT-PCR analysis Total RNA was isolated with an RNeasy Plant Mini kit (Qiagen, Valencia, CA) from plant tissues treated with or without TM for 6 h Relative quantification of mRNA was carried out by the real-time RT-PCR method with an ABI PRISM 7000 Sequence Detection System (Applied Biosys-tems, Foster City, CA) Forward primers, 5¢-AAGTCGT TGCACCTCCTGAGA-3¢, 5¢-TCAAGGACGCTGTTGT CACTGT-3¢, 5¢-ACACGGCAAATAACGTTCATCTCTA-3¢, 5¢-GGACTGCTTTCATCTGGCTTGT-3¢, 5¢-TCTCT GTTGGGTTTATCTCTTTGGTT-3¢, 5¢-TGATGGAAGA AGCAGTGGATGA-3¢ and 5¢-CGTAGAAGAGTGGTA

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