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Tài liệu Báo cáo khoa học: Restricted localization of proline-rich membrane anchor (PRiMA) of globular form acetylcholinesterase at the neuromuscular junctions – contribution and expression from motor neurons doc

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Tiêu đề Restricted localization of proline-rich membrane anchor (PRiMA) of globular form acetylcholinesterase at the neuromuscular junctions – contribution and expression from motor neurons
Tác giả K. Wing Leung, Heidi Q. Xie, Vicky P. Chen, Mokka K. W. Mok, Glanice K. Y. Chu, Roy C. Y. Choi, Karl W. K. Tsim
Trường học The Hong Kong University of Science and Technology
Chuyên ngành Biology
Thể loại báo cáo khoa học
Năm xuất bản 2009
Thành phố Kowloon
Định dạng
Số trang 12
Dung lượng 910,13 KB

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During the development of rat muscles, the expression of PRiMA and AChET and the enzymatic activity increased dramatically; however, the proportion of G4AChE decreased.. In parallel, the

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(PRiMA) of globular form acetylcholinesterase at the

neuromuscular junctions – contribution and expression from motor neurons

K Wing Leung, Heidi Q Xie, Vicky P Chen, Mokka K W Mok, Glanice K Y Chu, Roy C Y Choi and Karl W K Tsim

Department of Biology and Center for Chinese Medicine, The Hong Kong University of Science and Technology, China

Acetylcholinesterase (AChE; EC 3.1.1.7) plays a

cru-cial role in terminating the synaptic transmission by

hydrolyzing the neurotransmitter acetylcholine at the

neuron-to-neuron synapses in the central nervous

sys-tem and at the neuromuscular junctions (NMJs) in the

peripheral nervous system AChE exists in different

molecular forms The formation of these molecular

forms depends on alternative splicing in the 3¢ region

of the primary transcript [1], which generates the

AChER (‘readthrough’), AChEH (‘hydrophobic’) and

AChET (‘tailed’) subunits, containing the same

cata-lytic domain but different carboxyl termini [1] In

mammals, the AChER variant produces a soluble monomer that is up-regulated in the brain during stress [2]; the AChEHvariant produces a glycosylphos-phatidylinositol-linked dimer and is expressed in blood cells; the AChET variant is the only subunit expressed

in the brain and muscle The AChET subunits form nonamphiphilic tetramers with a collagen tail as asym-metric AChE (A4, A8 and A12) in muscle In addition, the AChET variant produces monomers (G1), dimers (G2) and tetramers (G4) The amphiphilic tetramer (G4) is linked with a proline-rich membrane anchor (PRiMA) as a globular form of AChE (PRiMA-linked

Keywords

acetylcholinesterase; molecular form;

muscle fiber type; neuromuscular junction;

proline-rich membrane anchor

Correspondence

K W K Tsim, Department of Biology,

The Hong Kong University of Science and

Technology, Clear Water Bay Road,

Kowloon, Hong Kong SAR, China

Fax: +852 2358 1559

Tel: +852 2358 7332

E-mail: BOTSIM@UST.HK

(Received 21 November 2008, revised 11

March 2009, accepted 25 March 2009)

doi:10.1111/j.1742-4658.2009.07022.x

The expression and localization of the proline-rich membrane anchor (PRiMA), an anchoring protein of tetrameric globular form acetylcholines-terase (G4AChE), were studied at vertebrate neuromuscular junctions Both muscle and motor neuron contributed to this synaptic expression pattern During the development of rat muscles, the expression of PRiMA and AChET and the enzymatic activity increased dramatically; however, the proportion of G4AChE decreased G4AChE in muscle was recognized specifically by a PRiMA antibody, indicating the association of this enzyme with PRiMA Using western blot and ELISA, both PRiMA protein and PRiMA-linked G4AChE were found to be present in large amounts in fast-twitch muscle (e.g tibialis), but in relatively low abundance in slow-twitch muscle (e.g soleus) These results indicate that the expression level

of PRiMA-linked G4AChE depends on muscle fiber type In parallel, the expression of PRiMA, AChET and G4AChE also increased in the spinal cord during development Such expression in motor neurons contributed to the synaptic localization of G4 AChE After denervation, the expression of PRiMA, AChETand G4AChE decreased markedly in the spinal cord, and

in fast- and slow-twitch muscles

Abbreviations

AChE, acetylcholinesterase; AChR, acetylcholine receptor; BChE, butyrylcholinesterase; ChAT, choline acetyltransferase; GAPDH,

glyceraldehyde-3-phosphate dehydrogenase; GFAP, glial fibrillary acidic protein; NeuN, neuronal nuclei; NMJs, neuromuscular junctions; PRiMA, proline-rich membrane anchor; SNAP-25, synaptosomal-associated protein 25.

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G4AChE) in brain and muscle [3–5] Two PRiMA

isoforms (PRiMA I and PRiMA II) are generated

from the PRiMA gene by alternative splicing

PRi-MA I contains a longer C-terminal cytoplasmic

domain than does PRiMA II [6]

Although asymmetric AChE is the predominant

species at NMJs and its appearance in muscle

coin-cides with the establishment of neuromuscular contacts

during development and regeneration [7,8], G4AChE

also exists in muscles Several studies have revealed

that the level of G4AChE is controlled by the

dynamic activity of skeletal muscles The

transcrip-tional regulation of PRiMA is down-regulated during

myogenic differentiation and under the influence of

innervation [9] In line with the transcriptional

expres-sion of PRiMA, the proportion of G4AChE decreases

during myogenic differentiation and innervation [1,9]

In mammals, fast-twitch muscles contain a large

amount of G4AChE, whereas slow-twitch muscles

contain a much smaller amount [10]

The expression of different AChE forms at NMJs

raises the question of whether the synaptic enzyme is

produced by muscle, nerve or both under different

physiological states Both asymmetric and globular

forms of AChE are known to be produced by muscle

cells [11,12], and the presynaptic motor nerve terminals

synthesize and secrete AChE at NMJs [13,14] The

pre-dominant form of AChE expressed by motor neurons

in chick spinal cord is G4AChE [15]

In this article, we analyze the expression and

locali-zation of the PRiMA I-linked G4form of AChE in rat

muscles and motor neurons We prepared an antibody

against the cytoplasmic domain of PRiMA I, which allowed us to show that PRiMA-linked G4AChE is localized at NMJs in both presynaptic nerve terminals and postsynaptic muscle fiber It is expressed by motor neurons in the rat spinal cord: this expression increased during development, but decreased after denervation These data show that both presynaptic motor neuron and postsynaptic muscle fiber contribute

to the synaptic expression of PRiMA-linked G4AChE and illustrate its temporal and spatial expression at NMJs

Results

Regulation of G4AChE and PRiMA during muscle development

A rabbit polyclonal antibody against the C-terminus

of PRiMA I was generated To validate the PRiMA antibody, a full-length mouse PRiMA cDNA (corre-sponding to PRiMA I unless specified) and a C-termi-nal truncated mutant (PRiMADC-term) cDNA, both tagged with a FLAG epitope, were transfected into HEK293T cells In western blot analysis, a FLAG antibody recognized both PRiMA and PRiMADC-term with protein bands of approximately 20 and 16 kDa, respectively: these protein bands corresponded to the predicted size of the recombinant proteins (Fig 1A) The PRiMA antibody, however, recognized only the full-length PRiMA, but not the truncated PRiMADC-term construct In addition, the recognition was fully blocked by pre-incubation of the PRiMA

Fig 1 The specificity of the PRiMA antibody (A) Protein samples (40 lg) of HEK293T cells expressing FLAG-PRiMA or FLAG-PRiMADC-term were analyzed by 12% SDS–PAGE Both PRiMA and FLAG antibodies (Ab) were used to label the PRiMA proteins In the blocking experiment, excess amounts of recombinant PRiMA antigen (Ag) (from residues 114 to 153) at 5 lgÆmL)1were pre-incubated with the PRiMA antibody (0.5 lgÆmL)1) for 4 h at 4 C before it was used for western blotting (B) Transfected HEK293T cells were stained with PRiMA or FLAG antibody

as described in Materials and methods Bar, 10 lm.

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antibody with the antigen, i.e the PRiMA I

C-terminal peptide (Fig 1A) In the

immunocytofluo-rescent staining of transfected fibroblasts, the PRiMA

antibody also recognized FLAG-tagged

PRiMA-expressing cells (Fig 1B) In contrast, FLAG-tagged

PRiMADC-term-expressing cells were not recognized by

the antibody As a positive control, FLAG antibody

was used; it recognized both full-length and truncated

PRiMA in protein detection and immunostaining

(Fig 1A,B) Such recognition could not be blocked by

pre-incubation with PRiMA antigen These results

clearly indicate the specificity of the PRiMA antibody

in recognizing the cytoplasmic domain of PRiMA I

According to Perrier et al [6], two splicing variants

of PRiMA mRNAs are generated from the PRiMA

gene to produce different proteins (PRiMA I and

PRiMA II; Fig 2A) PRiMA I mRNA, which

posses-ses exons 4 and 5, produces a 40-residue-long

intra-cellular cytoplasmic tail, whereas PRiMA II mRNA, which possesses exons 4, 4b and 5, encodes a shorter intracellular motif These two PRiMA isoforms may

be distinguished by RT-PCR using primers flanking exons 4 and 5 In rat muscles, PRiMA I was found to

be present, whereas PRiMA II was barely detectable (Fig 2B) For precise quantification, we used real-time PCR with the same set of primers In agreement with the absence of PRiMA II in muscle, all the amplified products revealed by real-time PCR corresponded to PRiMA I The mRNA level of PRiMA I was up-regu-lated gradually in the early postnatal stages and dra-matically in the adult stage (Fig 2B) Meanwhile, the level of AChET mRNA increased gradually from the early postnatal stage to the adult Using PRiMA anti-body, the PRiMA protein was detected in the muscles

of embryonic rats; its level increased after postnatal day 10 to the adult (Fig 2C) As reported previously,

Fig 2 Developmental profiles of PRiMA, AChETand G4AChE in skeletal muscles (A) Splice variants of PRiMA mRNAs (PRiMA I and II) are illustrated PRiMA II contains an additional exon 4b Arrows show the location of primers used for qualitative and real-time PCR analyses (B) Total RNAs were extracted from rat leg muscles at different developmental stages to perform RT-PCR for PRiMA I (145 bp) PRiMA II (302 bp) and AChET(671 bp) Adult rat brain served as a positive control One representative result is shown (top) The bottom panel shows the results of real-time PCR analysis of the mRNA expression of PRiMA I and AChE T (C) Samples of extracts from the lower leg muscles

of rat (birth to adult stage) containing 40 lg of protein were loaded per lane for western blotting (top) The levels of PRiMA and AChET proteins were determined GAPDH served as a loading control The bottom panel shows the quantified data of protein bands AChE activity was determined by the Ellman assay (D) Samples of extracts from rat leg muscles containing equal amounts of AChE activity were loaded

on sucrose density gradients AChE activity was plotted as a function of the S value, estimated from the position of the sedimentation mark-ers Enzymatic activities are expressed in arbitrary units, and representative sedimentation profiles are shown (E) The specific activity of

G 4 AChE was quantified at different developmental stages Samples of muscle extracts at different developmental stages containing 600 lg

of protein were loaded on sucrose density gradients The peak area corresponding to G 4 AChE activity was determined The results are expressed as the ratio to the value obtained at E21 (basal), and are shown as means ± standard error of the mean (SEM), n = 4.

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AChETprotein and AChE enzymatic activity increased

during muscle development (Fig 2C) With regard to

the AChE molecular form, the AChE G1and G4forms

were predominant in embryonic muscles (Fig 2D) In

mature muscles, the relative proportion of the G1 and

G4 forms was reduced and the asymmetric form of

AChE (A12) was increased (Fig 2D) In order to

quan-tify the relative amount of PRiMA-linked G4AChE in

developing muscle, protein extracts at different

develop-mental stages were analyzed by sedimentation in sucrose

density gradients The proportion of G4AChE was

determined from the peak area, relative to the area of

the entire sedimentation profile, and its activity was

given by the product of this proportion with the total

AChE activity The amount of G4AChE in muscle

increased twofold from birth to adult (Fig 2E)

PRiMA-linked G4AChE therefore increased during

muscle development

Expression of PRiMA-linked G4AChE in

fast-twitch and slow-twitch muscles

In order to investigate the expression level of PRiMA

and PRiMA-linked G4AChE in different muscle fiber

types, fast-twitch (tibialis) and slow-twitch (soleus)

muscles from adult rats were collected and analyzed In

western blotting, PRiMA protein was detected in both

tissues, but its level was about threefold lower in the

soleus than in the tibialis (Fig 3A) The relative

abun-dance of PRiMA-linked G4AChE was determined by

ELISA using our PRiMA antibody Equal amounts of

AChE activity were loaded onto an ELISA plate

pre-coated with serial dilutions of PRiMA antibody The

retained AChE enzymatic activity, corresponding to

PRiMA-linked G4AChE, was measured after washing

We found larger amounts (over twofold) of

PRiMA-linked G4AChE in the tibialis than in the soleus

(Fig 3B) The higher expression of G4AChE in the

tibialis was further confirmed by sucrose density

gradi-ent analysis The PRiMA antibody was able to deplete

the G4 form of AChE in the tibialis, but this was not

obvious in the soleus (Fig 3C) In all cases, the brain

enzyme was used as a control

We analyzed the localization of PRiMA in sections

of tibialis and soleus muscle by

immunohistofluores-cence NMJs were visualized by labeling the

post-synaptic acetylcholine receptor (AChR) with

a-bungarotoxin (shown in red or pseudo-blue) and the

presynaptic nerve terminal with synaptotagmin (SV48;

shown in red) in both types of muscle (Fig 4) PRiMA

(shown in green) was expressed at the NMJs, and its

distribution was wider than that of AChE and AChR,

extending into a peri-junctional zone where neither

Fig 3 Expression of PRiMA and G4AChE in different muscles (A) Samples of extracts from adult rat soleus and tibialis containing

40 lg of protein were loaded per lane for western blotting of PRiMA protein Adult rat brain served as a positive control The bottom panel shows the quantification of PRiMA protein The results are expressed as the ratio to soleus (basal) equal to unity; means ± stan-dard error of the mean, n = 4 (B) The relative amount of PRiMA-linked G4AChE was quantified by ELISA Tissue lysates from rat brain, tibialis and soleus containing equal AChE activities were loaded onto an ELISA plate precoated with serial dilutions of PRiMA anti-body for 2 h The retained AChE activity was determined (C) For immunodepletion, 1 mL samples of extracts from adult rat brain, tibi-alis and soleus were incubated with PRiMA antibody (10 lgÆmL)1) and protein G-agarose before sucrose density gradient analysis AChE activity was plotted as a function of the S value, estimated from the position of the sedimentation markers Enzymatic activities are expressed in arbitrary units, and representative sedimentation profiles are shown.

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Fig 4 Localization of PRiMA and AChE at

NMJs Sections from adult rat tibialis (top)

and soleus (bottom) muscles were triple

stained with rhodamine-conjugated or Alexa

647-conjugated a-bungarotoxin (red or

pseudo-blue) for postsynaptic AChR,

anti-AChE T (pseudo-blue), anti-synaptotagmin

(SV48; red) for presynaptic nerve terminal

and anti-PRiMA (green), and examined by

confocal microscopy Merged images of

AChR⁄ SV48 and PRiMA are shown on the

right Representative images are shown,

n = 4 Bar, 20 lm.

Fig 5 Developmental evolution of PRiMA and G 4 AChE in the spinal cord (A) Total RNAs were extracted from spinal cord at different developmental stages for detection of transcripts encoding PRiMA I (145 bp), PRiMA II (302 bp) and AChE T (671 bp) Representative results are shown (B) Samples of extracts of rat spinal cord (from birth to adult stages) containing 40 lg of protein were loaded per lane for wes-tern blotting PRiMA and AChETproteins were determined GAPDH served as a loading control (C) Quantification of proteins (from B) and AChE activity during development (D) One milliliter samples of extract from adult rat spinal cord, with and without depletion by the PRiMA antibody (as in Fig 3C), were analyzed by sucrose density gradients AChE activity was plotted as a function of the S value, estimated from the position of the sedimentation markers Enzymatic activities are expressed in arbitrary units, and representative sedimentation profiles are shown (E) G 4 AChE specific activity in the spinal cord at different developmental stages was quantified as in Fig 2E The results are expressed as the ratio to the value obtained at P1 (basal) equal to unity; means ± standard error of the mean (SEM), n = 4.

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AChE nor AChR was present in either muscle fiber

type However, the precise localization of PRiMA has

yet to be determined

Presence of PRiMA-linked G4AChE in motor

neurons

At NMJs, AChE may originate from the muscle fiber

and⁄ or from the motor neuron In order to examine the

presence of PRiMA and PRiMA-linked G4AChE, rat

spinal cords were collected at early postnatal and adult

stages Qualitative PCR indicated that both PRiMA I

and II transcripts were expressed in the spinal cord: the

PRiMA I transcript decreased slightly after birth, but

increased dramatically thereafter and was the

predomi-nant form in the adult, the PRiMA II transcript first

increased but disappeared in the adult (Fig 5A) As a

result of the absence of a specific primer for PRiMA I,

the expression level of the PRiMA I transcript could

not be analyzed by real-time PCR The PRiMA I

pro-tein level in the spinal cord, determined in western blots

with the PRiMA antibody (recognizing the cytoplasmic

domain of PRiMA I), increased after birth, as did

AChE (Fig 5B,C) This was consistent with an increase

in total AChE activity (Fig 5C) and with the

observa-tion that G4was the predominant form of the enzyme in

the adult spinal cord (Fig 5D) The majority of

G4AChE was associated with PRiMA I, as more than

70% was immunoprecipitated with the PRiMA

anti-body The relative amount of G4AChE determined

from sedimentation profiles allowed us to evaluate its

activity: the specific activity of G4AChE per milligram

of protein reached a plateau in the spinal cord about

10 days after birth (Fig 5E)

To determine the origin of AChE in the spinal

cord, the lumbar region of the spinal cord was

sectioned and stained with the PRiMA antibody The

label was mostly present in the ventral horn

(Fig 6A) As expected, PRiMA was detected in

AChE-positive cells in the ventral horn (Fig 6B)

These PRiMA-stained cells were motor neurons, as

shown by their reactivity with an anti-choline

acetyl-transferase (anti-ChAT) antibody This identification

was further supported by double staining of neuronal

nuclei with a neuronal marker (NeuN) In contrast,

no PRiMA was found in glial cells that were labeled

specifically with an antibody against glial fibrillary

acidic protein (GFAP) (Fig 6B) These results clearly

show that PRiMA is synthesized by motor neurons in

the spinal cord

Although motor neurons are able to synthesize

PRiMA and produce G4AChE, the restricted

localiza-tion of PRiMA-linked G4AChE at NMJs could still

be derived from three sources: muscle, Schwann cells and⁄ or motor neurons In order to determine the local-ization of PRiMA-linked G4AChE, sections of tibialis muscle were triple stained for PRiMA, SV48 and AChR The staining of PRiMA was coincident with that of SV48, rather than with that of AChR (Fig 7, left panel) Similar results were obtained with another

Fig 6 Motor neurons in the spinal cord express PRiMA (A) Sche-matic diagram showing the lumbar region of the spinal cord (left) The dorsal horn and ventral horn are indicated The right panel shows PRiMA staining in the lumbar region on the same scale at low magnification The boxed area is shown at higher magnification

in (B) Bar, 100 lm (B) Spinal cord sections were double stained with anti-PRiMA (green) and with anti-AChET(red), anti-ChAT (red), anti-NeuN (red) or anti-GFAP (red), and examined by confocal microscopy PRiMA was co-localized with AChE T , ChAT and NeuN, but not with GFAP Representative images are shown, n = 4 Bar,

20 lm.

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presynaptic marker, synaptosomal-associated

pro-tein 25 (SNAP-25): PRiMA also showed a better

co-localization with SNAP-25 than with AChR

(Fig 7, right panel) Such overlapping of PRiMA

staining with presynaptic molecules indicates that

PRiMA at NMJs is mainly provided by motor

neurons

Innervation regulates the expression of

PRiMA-linked G4AChE in the spinal cord

The expression of PRiMA and the pattern of AChE

molecular forms in muscles are known to be modified

by denervation [7] In order to determine whether

PRiMA expression in the spinal cord was regulated by

a retrograde influence of the muscle, a portion of the

sciatic nerve was surgically removed After 7 days, we

examined the expression of PRiMA in both spinal

cord (lumbar region) and tibialis muscles by real-time

PCR analysis: PRiMA mRNA (PRiMA I) was not

modified significantly in the tibialis, but was reduced

by over 60% in the spinal cord (Fig 8A) In contrast,

the mRNA level of AChET was decreased in both the

spinal cord and tibialis when compared with that of

the sham-operated control (Fig 8A) At the protein

level, western blot analyses showed that PRiMA and

AChET were reduced by about 50% after denervation

in both tissues (Fig 8B) This is consistent with a

decrease in AChE enzymatic activity of about 50% in

the spinal cord and tibialis muscle (Fig 8B) Sucrose

density gradient analyses showed a significant

reduc-tion of G1and G4forms in the spinal cord and of G1,

G4 and A12 forms in the tibialis (Fig 8C) Thus,

denervation induced a decrease in PRiMA and

G4AChE in the spinal cord and muscle

To investigate the contribution of the motor neuron

to PRiMA-linked G4AChE at NMJs, we analyzed the effect of denervation on the localization of PRiMA The NMJs of the denervated tibialis and sham-oper-ated muscle were stained for PRiMA, together with the postsynaptic marker AChR (shown in pseudo-blue) and a presynaptic marker SV48 (shown in red) Pre-synaptic labeling essentially disappeared at the dener-vated NMJs and PRiMA labeling was considerably reduced This suggests that a significant proportion of PRiMA was provided by the presynaptic motor neuron (Fig 8D) However, a small amount of PRiMA could still be detected in the denervated muscles, possibly of muscle origin

Discussion

The muscles of mice in which the PRiMA gene is inac-tivated contain essentially no G4AChE, suggesting that this enzyme form is entirely associated with PRiMA Our results show that G4AChE is, indeed, largely immunoprecipitated with a PRiMA antibody However, a fraction of G4AChE was not immunodepleted (Fig 3C), even when the amount of antibody was increased or with a second round of immunodepletion (not shown) The interaction of this fraction with the antibodies may be prevented by the presence of partner(s) associated with the C-terminal region of PRiMA In addition, no G4AChE was found in muscles of PRiMA knockout mice, implying that all G4AChE in muscle is linked with the mem-brane-anchoring protein PRiMA During muscle devel-opment, the amount of PRiMA-linked G4AChE progressively increased from birth to the adult stage

In addition, the expression of PRiMA and G4AChE

Fig 7 Presynaptic localization of PRiMA at NMJs Adult rat tibialis sections were triple stained with Alexa 647-conjugated a-bungarotoxin (pseudo-blue), anti-synaptotagmin (SV48; red) or anti-SNAP-25 (red) antibodies, and anti-PRiMA (green), and examined by confocal micros-copy Merged images allow a comparison of PRiMA with presynaptic markers (PRiMA + SV48 ⁄ SNAP-25) and a postsynaptic marker

(PRi-MA + AChR) The distribution of PRi(PRi-MA overlapped with that of SV48 and SNAP-25 Representative images are shown, n = 4 Bar, 20 lm.

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was dependent on the fast or slow nature of muscle

fibers The strong expression of PRiMA protein and

G4AChE in fast-twitch muscles is consistent with

previous results on PRiMA mRNA expression, i.e the

tibialis contains an approximately 10-fold higher level

of PRiMA mRNA than the soleus [9] The

develop-mental change of PRiMA-linked G4AChE in muscle

correlates with an increase in muscular activity and

muscle loading [15–17], which leads to the

differentia-tion of fast-twitch and slow-twitch muscle fibers The

specific role of this AChE form at NMJs remains to be elucidated

Various forms of AChE exist in both developing and mature NMJs The major form is the asymmetric collagen-tailed AChE, which is attached to the synap-tic basal lamina [18] Our study and others have shown that G4AChE is linked by PRiMA and localized in the membranes of postsynaptic and presynaptic cells [9] At NMJs, three cell types can contribute to synap-tic AChE: the postsynapsynap-tic muscle cell, the presynapsynap-tic

Fig 8 Denervation reduces the expression of PRiMA and G 4 AChE in the spinal cord and in muscles (A) The sciatic nerve was sectioned

to examine the effect of muscle on the expression of PRiMA in motor neurons After 7 days, tibialis and spinal cord were collected for analy-sis The mRNA levels of denervated muscles (Den) corresponding to PRiMA (top) and AChE T (bottom) were determined by PCR and normal-ized to those of control (sham-operated) muscles (B) Samples of extracts from control and denervated muscles containing 50 lg of protein were loaded per lane for the western blotting of PRiMA and AChET GAPDH served as a loading control The bottom panel shows the ratios

of AChE enzymatic activity after nerve section to control values The results are expressed as the ratio to control values (sham-operated) equal to unity; means ± standard error of the mean (SEM), n = 3 (C) Effect of nerve section on AChE molecular forms in the spinal cord and tibialis muscles Samples containing equal amounts of protein were loaded onto sucrose gradients AChE activity was plotted as a func-tion of the S value, estimated from the posifunc-tion of the sedimentafunc-tion markers Enzymatic activities are expressed in arbitrary units, and representative sedimentation profiles are shown (D) Sections from adult rat tibialis after 7 days of denervation (right) and sham-operated (left) were triple stained with Alexa 647-conjugated a-bungarotoxin (pseudo-blue) for postsynaptic AChR, anti-synaptotagmin (SV48; red) for presynaptic nerve terminal, and anti-PRiMA (green), and examined by confocal microscopy Merged images allow a comparison of PRiMA with presynaptic (SV48 + PRiMA) and postsynaptic (AChR + PRiMA) markers The disappearance of the presynaptic nerve terminals in denervated muscle is verified by the absence of SV48 labeling PRiMA labeling was considerably reduced, but not completely absent Repre-sentative images are shown, n = 3 Bar, 10 lm.

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motor neuron and the Schwann cell During

develop-ment, the muscle is the primary source of all forms of

AChE [1] In contrast, the contribution of the

Schw-ann cell, if any, is limited [14]; however, the possible

presence of PRiMA in the Schwann cell membrane

could only be distinguished by electron microscopy In

this study, we confirmed the expression of PRiMA, as

well as of PRiMA-linked G4AChE, in the motor

neu-rons of the spinal cord using a PRiMA antibody The

level of AChE increased during development, and was

reduced after section of the sciatic nerve The current

results are in line with our previous observation that

chick motor neurons contain collagen-tailed AChE as

well as globular forms [15,19,20] In contrast, frog

motor axons have been shown to produce

collagen-tailed AChE, which could be deposited in the synaptic

basal lamina at NMJs [14] The production of

asym-metric AChE by motor neurons and its secretion by

the motor nerve terminals at frog NMJs could be

induced by damaged target muscles Indeed, the

capac-ity of a motor neuron to express asymmetric AChE at

an intact frog NMJ is still controversial

In this study, confocal microscopy showed that

PRiMA-linked G4AChE was found in both pre- and

postsynaptic membranes at NMJs The distribution of

PRiMA appeared to be more extensive than that of

AChE This may result from a higher sensitivity for

the detection of PRiMA Alternatively, a fraction of

PRiMA may not be associated with AChET catalytic

subunits For example, PRiMA can be associated with

butyrylcholinesterase (BChE) Indeed, the expression

of G4BChE, together with G4AChE, has been

revealed in brain and retina during development [21]

Our current and past results [15] indicate that motor

neurons represent the major cell type expressing

PRiMA and AChET in the spinal cord In line with

this observation, it has been shown that AChE is

expressed in both neurotube and myotomes [22] In

addition, previous studies have also shown that AChE

synthesized in the motor neuron is transported by

axo-nal flow to the presynaptic termiaxo-nal, as revealed by

enzymatic and microscopic studies [13] The function

of pre- and postsynaptic PRiMA-linked G4AChE

expressed by motor neuron and muscle, particularly

during early stages of development, is an open

ques-tion One of the proposed functions of two-sided

expression of AChE in both pre- and postsynaptic

membranes is to play an active role during

synapto-genesis through the adhesive function of AChE [23,24]

In addition, the decrease in PRiMA and AChE

expres-sion in the rat spinal cord after section of the sciatic

nerve could be the consequence of trauma or of the

loss of retrograde influence from the muscle cells

Indeed, muscle-derived factors control the expression

of presynaptic proteins by motor neurons at NMJs [17,25]

In previous studies, G4AChE could only be identi-fied by sucrose density gradients in the motor endplate region [16,26] In this study, we have provided the first analysis of the expression of PRiMA at NMJs, using

an antibody specific for the cytoplasmic domain of PRiMA I In both fast-twitch and slow-twitch NMJs, PRiMA was found in a peri-junctional region, suggest-ing that it is partly of muscle origin Such a peri-junc-tional distribution of G4AChE, which is more abundant in fast-twitch than slow-twitch muscles [16], may provide an AChE-rich environment embedding NMJs and control the diffusion of acetylcholine out of the synaptic cleft However, most PRiMA-linked

G4AChE was found to be located in the presynaptic membrane of the motor nerve terminal This is consis-tent with the presence of a significant amount of AChE activity in the presynaptic membrane at NMJs

of the rat lumbricalis muscle [27] The presence of AChE in the presynaptic membrane can facilitate the presynaptic re-uptake of choline resulting from the hydrolysis of acetylcholine

Materials and methods

Production of PRiMA antibody

The mouse PRiMA (amino acids 114–153)–glutathione S-transferase fusion protein was expressed in BL21 (DE3) pLysE Escherichia coli (Invitrogen, Carlsbad, CA, USA) and purified by glutathione bead chromatography (Amersham Biosciences, Piscataway, NJ, USA), according

to the manufacturer’s instructions After digestion by thrombin (Sigma, St Louis, MO, USA), the PRiMA (amino acids 114–153) antigen was purified by Superdex

75 10⁄ 300 gel filtration chromatography (Amersham Biosciences) Polyclonal antibodies were raised in a 2-kg male New Zealand White rabbit by immunization with

750 lg of antigen, mixed with an equal volume of complete Freund’s adjuvant (Sigma) The immunization was carried out with the same amount of antigen three times within 1 month The anti-PRiMA serum was col-lected and purified by protein G-Sepharose (Amersham Biosciences), according to the manufacturer’s instructions The amount of purified antibody was determined spectro-photometrically

DNA construction and transfection

The HEK293T cell line was obtained from the American Type Culture Collection (ATCC, Manassas, VA, USA) and

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cultured in Dulbecco’s modified Eagle’s medium (DMEM)

supplemented with 10% fetal bovine serum Cultured cells

were incubated at 37C in a water-saturated 5% CO2

incu-bator All reagents for cell cultures were from Invitrogen

cDNAs encoding full-length mouse PRiMA (PRiMA I) and

a COOH-terminal truncated mutant (PRiMADC-term;

obtained by deleting the COOH-terminal region, residues

122–153, of PRiMA I) were tagged with a FLAG epitope

(obtained by inserting the FLAG epitope DYKDE at

posi-tion 36 between the putative signal sequence and the NH2

terminus) in pEF-BOS mammalian expression vector

Transfection in cultured HEK293T was performed by

calcium phosphate precipitation

Western blot analysis

HEK293T cultures or tissues were homogenized in lysis

buffer (10 mm HEPES, pH 7.5, 1 m NaCl, 1 mm EDTA,

1 mm EGTA, 0.5% Triton X-100 and 1 mgÆmL)1

bacitra-cin), followed by centrifugation at 12 000 g for 20 min at

4C Protein samples were denatured at 100 C for 5 min

in a buffer containing 1% SDS and 1% dithiothreitol,

and separated by 8% or 12% SDS–PAGE For western

blot analysis, our PRiMA polyclonal antibody (purified at

0.5 lgÆmL)1), an AChE antibody E19 (1 : 2000; Santa

Cruz Biotechnology Inc., Santa Cruz, CA, USA), a

mono-clonal FLAG antibody (1 : 1000; Sigma) and

anti-glyceral-dehyde-3-phosphate dehydrogenase (GAPDH) antibodies

(1 : 10 000; Sigma) were used The immune complexes

were visualized using the enhanced chemiluminescence

method (Amersham Biosciences) The intensities of the

bands in the control and stimulated samples, run on the

same gel and under strictly standardized enhanced

chemi-luminescence conditions, were compared on an image

analyzer using, in each case, a calibration plot constructed

from a parallel gel with serial dilutions of one of the

samples

Immunofluorescence analysis

Transfected cell cultures or tissue sections (16 lm) were

fixed by 4% paraformaldehyde in NaCl⁄ Pi for 15 min,

followed by 50 mm ammonium chloride (NH4Cl) treatment

for 25 min Samples were permeabilized by 0.2% Triton

X-100 in NaCl⁄ Pifor 10 min and blocked by 5% BSA in

NaCl⁄ Pi for 1 h at room temperature Cultures were

stained with PRiMA (2 lgÆmL)1) or FLAG (1 : 500,

Sigma) antibodies Tissue sections were double or triple

stained by rhodamine-conjugated or Alexa 647-conjugated

a-bungarotoxin (dilution 1 : 500; Molecular Probes,

Eugene, OR, USA), PRiMA antibody (2 lgÆmL)1), AChE

antibody (dilution 1 : 500, Santa Cruz Biotechnology),

anti-synaptotagmin (SV48) (1 : 500, BD Biosciences Clontech,

San Jose, CA, USA), SNAP-25 (1 : 200, Sigma),

anti-ChAT (1 : 200, Millipore, Bedford, MA, USA), anti-NeuN

(1 : 500, Millipore) and Cy3-conjugated anti-GFAP (1 : 500, Sigma) for 16 h at 4C, followed by the corre-sponding fluorescence-conjugated secondary antibodies (Alexa 488-conjugated anti-rabbit, Alexa 555- or Alexa 647-conjugated anti-mouse and anti-goat) for 2 h at room temperature The specificity of the PRiMA antibody was established by pre-incubation with the PRiMA antigen (10 lgÆmL)1) for 2 h at 4C Samples were dehydrated serially with 50%, 75%, 95% and 100% ethanol and mounted with fluorescence mounting medium (DAKO, Carpinteria, CA, USA) The samples were then examined using a Leica confocal microscope with excitation at

488 nm⁄ emission at 505–535 nm for green, excitation at

543 nm⁄ emission at 560–620 nm for red, and excitation

at 647 nm⁄ emission at 660–750 nm for pseudo-color

Sucrose density gradient analyses

Separation of the various molecular forms of AChE was performed by sucrose density gradient analysis, as described previously [28] In brief, sucrose gradients (5% and 20%) in lysis buffer were prepared in 12 mL polyallo-mer ultracentrifugation tubes with a 0.4 mL cushion of 60% sucrose at the bottom Sample extracts (0.2 mL) mixed with sedimentation markers (alkaline phosphatase, 6.1S; b-galactosidase, 16S) were loaded onto the gradients and centrifuged at 175 000 g in a Sorvall TH 641 rotor at

4C for 16 h Approximately 45 fractions were collected and AChE enzymatic activity was determined according to the method of Ellman [29]; the reaction medium contained 0.1 mm tetra-isopropylpyrophosphoramide, an inhibitor of BChE Absorbance at 410 nm was recorded as a function

of the reaction time The proportions of the various AChE forms were determined by summation of the enzy-matic activities corresponding to the peaks of the sedimen-tation profile In the immunoprecipisedimen-tation of G4AChE by PRiMA antibody, 1 mL samples of tissue extracts were incubated for 4 h at 4C with purified PRiMA antibody (10 lgÆmL)1) Then, 50 lL of washed protein-G agarose gel (Santa Cruz Biotechnology) was added and incubated for 1 h at 4C After centrifugation, the supernatants were loaded onto sucrose gradients for sedimentation analysis

ELISA for PRiMA-linked G4AChE

Fifty microliter samples of serially diluted PRiMA antibody were coated in a 96-well ELISA plate (Nunc Maxisorp Immunoplate, Roskilde, Denmark) for 16 h The antibody was removed and the plate was washed twice with 200 lL NaCl⁄ Picontaining 0.1% Tween-20 The plate was blocked

by NaCl⁄ Pi with 5% fetal bovine serum for 2 h at room temperature Tissue lysates containing equal AChE activity were loaded onto the precoated ELISA plate and incubated for 2 h The plate was washed three times with 200 lL

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