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Báo cáo khoa học: Functional studies of crustacean hyperglycemic hormones (CHHs) of the blue crab, Callinectes sapidus – the expression and release of CHH in eyestalk and pericardial organ in response to environmental stress pot

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The functions of ES-CHH and PO-CHH in this species were studied with regard to expression and release in response to stressful episodes: hypoxia, emersion, and temperatures.. Hemolymph t

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(CHHs) of the blue crab, Callinectes sapidus – the

expression and release of CHH in eyestalk and pericardial organ in response to environmental stress

J Sook Chung and N Zmora

Center of Marine Biotechnology, University of Maryland Biotechnology Institute, Baltimore, USA

In recent years, crustacean hyperglycemic hormones

(CHHs), traditionally identified in the medulla

termi-nalis X-organ and sinus gland (SG) in the eyestalk

(ES), have been found in non-ES tissues Reported

sites for the synthesis of CHH-like neuropeptides in

non-ES tissues include the gut [1,2], subesophageal

ganglion (SOG) [3], pericardial organs (POs) [4,5], and

cells in the abdominal segments of embryos [6] In

Car-cinus maenas, the expression and translation of gut

CHH occurs exclusively during premolt [1,2], whereas

ES-CHH is molt stage independent [7] The amino acid

sequence of gut CHH is identical to that in the ES

[1,8], but only 66% homologous to PO-CHH [4,5,8] Thus, it seems that C maenas [1,4,8], Homarus americ-anus [3,9,10], Pachygrapsus marmoratus [5] and Mach-robrachium rosenbergii [11] exhibit multiple isoforms and synthesis sites for CHH, suggesting that this may

be a common feature among crustaceans

Many putative CHH sequences have been identified with the aid of cDNA cloning, but there is little infor-mation about the localization or the physiological function of active CHH neuropeptides in correspond-ing tissues Prototypical actions attributed to ES-CHH include induction of hyperglycemia, suppression of

Keywords

hypoxia; pericardial organ and sinus gland

crustacean hyperglycemic hormones;

temperature stress

Correspondence

J S Chung, Center of Marine

Biotechnology, University of Maryland

Biotechnology Institute, 701 East Pratt

Street, Columbus Center, Suite 236,

Baltimore, MD 21202, USA

Fax: +1 410 234 8896

Tel: +1 410 234 8841

E-mail: chung@comb.umbi.umd.edu

(Received 9 October 2007, revised 5

December 2007, accepted 11 December

2007)

doi:10.1111/j.1742-4658.2007.06231.x

The rapid increase in the number of putative cDNA sequences encoding crustacean hyperglycemic hormone (CHH) family in various tissues [either from the eyestalk (ES) or elsewhere] underscores a need to identify the corresponding neuropeptides in relevant tissues Moreover, the presence of provided structural CHH implies the level of the complexity of physiologi-cal regulation in crustaceans Much less is known of the functions of

non-ES CHH than of those of its counterpart present in non-ESs In the blue crab, Callinectes sapidus, we know little of CHH involvement in response to the stressful conditions that naturally occur in Chesapeake Bay We have iden-tified two isoforms of CHH neuropeptide in the sinus gland of the ES and isolated a full-length cDNA encoding CHH from the pericardial organ (PO) The functions of ES-CHH and PO-CHH in this species were studied with regard to expression and release in response to stressful episodes: hypoxia, emersion, and temperatures Animals exposed to hypoxic condi-tions responded with concomitant release of both CHHs In contrast, the mRNA transcripts encoding two CHHs were differentially regulated: PO-CHH increased, whereas ES-CHH decreased This result suggests a possible differential regulation of transcription of these CHHs

Abbreviations

AK, arginine kinase; CHH, crustacean hyperglycemic hormone; CPRP, crustacean hyperglycemic hormone precursor-related peptide; eIF4A, eukaryotic translation initiation factor 4A; ES, eyestalk; PO, pericardial organ; SALDI, surface-assisted laser desorption ⁄ ionization; SG, sinus gland; SOG, subesophageal ganglion; TD-PCR, touchdown PCR; TG, thoracic ganglia.

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ecdysteroid and methyl farnesoate synthesis, inhibition

of ovarian protein synthesis and osmoregulation [12–

19] Hyperglycemia, the commonly observed adaptive

response, is caused by the release of CHH from the ES

in response to changes in environmental conditions

such as oxygen, temperature, and salinity [19–24]

CHHs from the gut and the cells in embryonic

abdom-inal segments seem to be particularly involved in the

process of water uptake during ecdysis and hatching,

respectively [1,6] The physiological roles of

SOG-CHH and PO-SOG-CHH have not been defined [3–5,11]

Although CHH secretion from the ES in response to

stress is well documented [19–24], the effect of stresses

on CHH transcription in the ES remains unanswered

Thus, despite > 90 putative cDNA structures for

CHH being deposited in GenBank, it is apparent that

much work is still required to address the physiological

roles and the localization of the corresponding

neuro-peptides in the tissues from which many CHH cDNAs

were derived

The blue crab, Callinectes sapidus, an economically

valuable euryhaline species in Chesapeake Bay,

experi-ences migration and seasonal changes in

environ-mental conditions, including temperature, salinity

and dissolved oxygen (http://www.dnr.state.md.us/bay/

monitoring/water/index.html) In particular, it is noted

that in the Bay, low temperatures during winter and

anoxia during summer, in combination with the

changes in salinity, are associated with high mortality

in this species [25–27] In view of CHH involvement in

response to stress in other crustacean species, it is

rea-sonable to think that Cal sapidus CHH may also play

an important regulatory role in adaptation to

natu-rally occurring stressful conditions Thus, we were

interested in isolating the cDNA of PO-CHH and

identifying the native CHH neuropeptide in the ES,

after the recent report of CHH cDNA from the ES

[28] Also, we examined the physiological responses of

the release and expression of these two CHHs under

stressful conditions, especially severe hypoxia,

hypo-thermia and hyperhypo-thermia, in an attempt to define

their functions

To address these questions, we cloned the

full-length cDNA of PO-CHH and identified the presence

of the neuropeptide forms in the ES and PO For the

first time in crustaceans, the expression profiles of

these two CHHs in response to oxygen and

tempera-ture changes were documented using quantitative

real-time RT-PCR To further define the physiological

role of PO-CHH, the levels of this CHH were

mea-sured from the same animals, along with ES-CHH,

using RIAs under control normoxic and hypoxic

con-ditions

Results Identification and bioactivity of CHHs from ES sinus glands and PO

Two RP-HPLC peaks (1 and 2) as presented in Fig 1 showed strong cross-reactivity with anti-ES-CHH (Fig 1) The result of a glucose bioassay with these peaks confirmed that peak 2 is the major type of Cal sapidus ES-CHH-II, as it is for Car maneas and Cancer pagurus [29,30] The molecular masses of peaks 1 and 2, determined by ESI MS, were 8494.20 Da and 8478.01 Da, respectively

The typical separation of PO extract (50 PO equiva-lents) by RP-HPLC is presented in Fig 2 Fractions

Retention time, min

0 10 20 30 40

0.0

0.2

1 2

Fig 1 CHH neuropeptide profile of single SG extract of Cal sapi-dus on an RP-HPLC C18 column The gradient condition was 30– 80% solution B over 45 min (solution A, 0.11% trifluoroacetic acid

in water; solution B, 0.1% trifluoroacetic acid in 40% water and 60% acetonitrile) Absorbance and flow rate were monitored at

210 nm at a flow rate of 1 mLÆmin)1 Peak 1, I; peak 2,

CHH-II The mass of each neuropeptide determined by ESI MS was as follows; CHH-I, 8494.2 Da; CHH-II, 8478.1 Da Fractions that posi-tively cross-reacted with Car maenas CHH antiserum are shown

as bars.

0.0

0.5

Retention time, min

0 10 20 30 40

Fig 2 Separation of the extract of PO (50 equivalents) on an RP-HPLC C18 column Elution conditions were the same as described for Fig 1 The cross-reacted fractions initially tested with Car mae-nas CHH antiserum are shown as bars.

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analyzed by ELISA are marked on a bar graph that

shows positive cross-reactivity with PO-CHH

anti-serum Immunopositive fractions (numbers 30–32)

were further analyzed by surface-assisted laser

desorp-tion⁄ ionization (SALDI) to localize fraction 31

con-taining PO-CHH PO-CHH retained in fraction 31

showed two masses with a 16 Da difference: 8373 Da

and 8356 Da This fraction was subjected to further

purification, and the final peak was collected for

bio-assay

Native PO-CHH (20 pmol) or ES-CHH (10 pmol)

of the blue crab was injected into intact blue crabs

ES-CHH increased hemolymph glucose five-fold, as

compared to controls, whereas the injection of

PO-CHH did not elevate hemolymph glucose (Fig 3)

Animals injected with 20 pmol of oxidized ES-CHH,

in which one of the Met residues was oxidized to give

a 16 Da higher molecular mass than that of

non-oxi-dized ES-CHH (peak 2, CHH-II), showed only a

mod-est two-fold increase in glucose level from 77.79 ± 7.3

to 151.58 ± 13.4 lgÆmL)1 hemolymph (n = 10,

P< 0.01, paired t-test) Interestingly, the injection of

20 pmol of Car maenas ES-CHH also induced a

sig-nificant increase (P < 0.05, paired t-test) in

hemo-lymph glucose from the blue crab (257 ± 34.6 to

633 ± 229 lgÆmL)1hemolymph, n = 10)

PO immunohistochemistry

Figure 4A shows the intrinsic multipolar cells in the

posterior bar of the PO;  50 cells, 30–40 lm in

length, were positive with anti-PO-CHH serum Most

cells (35–40) were located in the anterior (Fig 4A) and

posterior (Fig 4B) bars, whereas the rest were located

in trunks Two types of cells were observed: the

major-ity of cells showed homogeneous CHH staining in the

cytoplasm (Fig 4C) with a visibly large nucleus,

whereas others had less intensive but punctuated and

granulated cytoplasm (Fig 4D) Figure 4E shows the possible release sites on the surface of the PO and many nerve fiber tracts and varicosities in trunks of the PO

Cloning and sequencing of PO-CHH cDNA The first PCR of PO cDNA with a combination of a set

of primers LF1 and LR1 (Table 1) produced an ampli-con of 500 bp On the basis of this sequence, gene-specific primers for 5¢-RACE (LR and LR2) and 3¢-RACE (LF2) were generated A nested PCR with a combination of LF2 and 3¢ nested primer (Invitrogen, Carlsbad, CA, USA), using the template from a touch-down product, generated an amplicon of  1.7 kbp The sequencing of the cloned vector of this amplicon as

an insert was completed using M13 F and R and a walk-ing primer (PWF1, ATGGGATATGTTCTCAGT), revealing the presence of a long 3¢-UTR ( 1.5 kbp) The amplicon (132 bp) produced from the nested PCR of 5¢-RACE cDNA contained a 5¢-UTR and the remaining sequence of the 5¢-end of PO-CHH The complete cDNA sequence of PO-CHH, shown in Fig 5, contained a 5¢-UTR, a signal peptide (MQS IKTVCQITLLVTCMMATLSYTHA), a crustacean hyperglycemic precursor-related peptide (RSAEG LGRMGRLLASLKSDTVTPLRGFEGETGHPLE), a CHH, a non-amidated C-terminus (QIYDSSCK GVYDRAIFNELEHVCDDCYNLYRNSRVASGCR ENCFDNMMFETCVQELFYPEDMLLVRDAIRG) and a 3¢-UTR of  1.5 kbp

Saline ES-CHH PO-CHH

Glucose (ug/1 mL hemolymph) 0

300

600

900

1200

***

Fig 3 In vivo bioassay of PO-CHH and ES-CHH (A) Glucose

assay: open bars, controls at time = 0; closed bar, t = 2 h Results

are presented as mean ± 1 SE (n = 6–8) ES-CHH showed a

signifi-cant increase in hemolymph glucose (***P < 0.001, paired t-test).

A

B

C

D

E

Fig 4 Immunohistochemistry of PO staining with PO-CHH anti-serum (A, B) Intrinsic multipolar cells, located in anterior (A) and posterior (B) bars (C, D) Cells at · 1200 magnification (E) PO-CHH staining shown in nerve fibers located in trunk Scale bars = 50 lm.

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Hemolymph titers of PO-CHH and ES-CHH in

response to changes in dissolved oxygen

Hypoxia induced the release of CHHs from the PO

and ES of the juvenile crabs (Fig 6) At the initial

control normoxic condition, the amount of ES-CHH

(376 ± 67 fmolÆmL)1) in hemolymph was  9-fold

higher than that of PO-CHH (45.6 ± 8.6 fmolÆmL)1)

One hour of exposure of hypoxia induced CHH

secre-tion both from the ES and PO ES-CHH doubled in

level from 376 ± 67 to 762 ± 143 fmolÆmL)1

hemo-lymph (n = 9, P < 0.05) The level of PO-CHH

increased from 45.6 ± 8.6 to 74.5 ± 19.8 fmolÆmL)1

hemolymph (n = 9) but there was no statistical

differ-ence Interestingly, ES-CHH levels in the hemolymph

of animals 10 min after they were returned to

con-trol normoxic seawater, after previous exposure to

hypoxia for 1 h, significantly decreased to 156 ± 50

and 44.5 ± 12.8 fmolÆmL)1 hemolymph (n = 9,

P< 0.05), respectively

Effects of stresses on the levels of glucose and

lactate in hemolymph and gene expression in the

ES and PO

Hypoxia and emersion

Hypoxia and emersion caused hyperglycemia and

hyperlactemia (Fig 7A,B) Crabs exposed to hypoxia

and emersion showed a  3-fold increase in glucose and a more than 30-fold increase in lactate, whereas the levels in controls remained constant The arginine kinase gene (AK) and the eukaryotic translation initia-tion factor 4A gene (eIF4A, DQ667140) were initially selected as control genes, but the expression levels in both tissues were significantly increased in response to hypoxia and emersion Thus, all the expression levels were presented as total copy number⁄ tissue, as in Fig 7 The ES and PO from the animals that experi-enced 1 h of hypoxia and emersion showed significant changes in CHH gene expression As shown in Fig 7C, hypoxia and emersion greatly reduced ES-CHH gene expression ( 10-fold and five-fold) from 1.36 ± 0.42· 108 to 1.06 ± 0.16· 107 and 2.49 ± 0.35· 107 (copy number⁄ tissue, one-way anova, P< 0.05), respectively In contrast, the expression level of the PO-CHH gene was dramatically increased from 1.95 ± 0.5· 107 to 1.45 ± 0.45· 109

and 2.21 ± 0.79· 109 (copy number⁄ tissue, one-way anova, P < 0.05)

Emersion caused significantly higher expression

of eIF4A (5.85 ± 2.38· 107) than in controls (2.86 ± 0.73· 106) in the ES, at P < 0.05 (one-way anova), whereas hypoxia induced slightly higher expression of eIF4A (3.81 ± 2.49· 106) than in con-trols (2.86 ± 0.73· 106), which was not statistically significant Hypoxia and emersion, on the other hand, greatly increased eIF4A expression in the PO (1.34 ± 0.637· 108, 9.99 ± 2.68· 107, respectively),

as compared with controls (1.31 ± 0.163· 107) Lev-els of increase in AK expression in the ES and PO were approximately 3–5-fold, as compared with controls

Temperature

A 2 h exposure to hyperthermic (29C) conditions caused a 2.5-fold increase in glucose levels in hemo-lymph, as shown in Fig 8A, whereas in controls and under hypothermic conditions (4C) there was a slightly higher glucose level In contrast to the modest increase in glucose, the levels of lactate from all three groups were significantly elevated after 2 h, as com-pared with those at the beginning of the experiment The increase in lactate levels was pronounced, in that both thermal stresses caused increases from seven-fold (hypothermal) to 13-fold (hyperthermal), whereas a 3.5-fold increase was observed in animals maintained

at 22C

The effect of different temperatures on gene expres-sion in the ES and PO is shown in Fig 8C The expression of ES-CHH was modestly increased at

29C (P = 0.08, one-way anova) as compared with

Table 1 List of primers used for cloning of 5¢-3¢-RACE of PO-CHH.

LF and LR primers were used for standard cRNA production for

quantitative RT-PCR, whereas SF and SR primers were for

quantita-tive RT-PCR A combination of CHH-SF and ES-SR was used for

ES-CHH, and for PO-CHH, PO-SR primer was used Cal sapidus

AK, Q9NH49; Cal sapidus CHH, AY536012; Cal sapidus eIF4A,

DQ667140; Cal sapidus PO-CHH, DQ667141.

Primers Sequence (5¢- to 3¢)

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that in controls at 22C; whereas the level of

PO-CHHexpression was only slightly higher, at 29C In

contrast to the results obtained with hypoxia and

emersion, as shown in Fig 7, there was little change in

AK and eIF4A expression in the ES and PO at 22C

and 29C, except that animals exposed to 4 C

showed higher AK expression in the PO, as compared

with those exposed to 22C and 29 C

Discussion

In this article, we describe studies on the identification,

localization and bioactivity of CHH neuropeptides of

the blue crab, Cal sapidus, using biochemical,

molecu-lar and immunological methods Blue crabs produce a

CHH neuropeptide in the PO that shows a 66%

deduced amino acid sequence identity with ES-CHH

[28] We have also demonstrated, for the first time in

crustaceans, the differential expression of these two

CHHs in response to changes in the following environ-mental conditions: hypoxia, emersion, and tempera-ture More important with respect to physiology, we measured the hemolymph titers of these two CHHs under different dissolved oxygen levels in seawater Our results indicate that the regulatory mechanisms governing the expression of ES-CHH and PO-CHH are different Yet, the release of both CHHs seems to

be sensitive to dissolved oxygen in seawater, suggesting

an adaptive role

A single SG in the ES of Cal sapidus contains two isoforms of CHH The molecular mass difference sug-gests that the major CHH may have pyroglutamate at the N-terminus via post-translational cyclization of Glu of peak 1 This feature appears to be common in CHHs of brachyuran crab species, including Car mae-nas [29] and Cancer pagurus [30], and differs from those in astacuran species [10,31–33] The relative abundance of these CHH isoforms in the SG among

Fig 5 Sequence alignments of nucleotide and deduced amino acids of full-length PO-CHH (DQ667141) and ES-CHH (AY536012) PO-CPRP and ES-CPRP are in bold italic, and both CHHs are in bold The 5¢-UTR and a signal peptide are italicized A dibasic cleavage site (KR) is underlined The stop codon (TAA) is marked as *, and a putative polyadenylation site (AATAAA) is underlined.

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these species varies as a ratio of two isoforms (peaks 1

and 2), ranging from 1 : 5 for Cal sapidus, to 1 : 8 in

Car maenas, to 1 : 10 in Can pagurus [29,30], yielding

peak 2 as the major CHH

The immunohistochemistry studies show that the

intrinsically staining cells are responsible for PO-CHH

synthesis The staining patterns are similar to those of

Car maenas, in that most cells (approximately 35–40)

were localized in the anterior and posterior bars [4]

However, PO-CHH staining appears to be somewhat

different from that of crustacean cardioactive peptide

(CCAP) in the PO, where it is known mainly at its

release site [34] Overall, the immunohistochemisty of

PO-CHH in the PO indicates its role as a

neurotransmit-ter, as it may be directly targeted into the specific sites in

which the nerve fibers of the PO innervate the anterior

ramifications On the other hand, as a neurohormone,

PO-CHH may be released from the surface of the PO

and into branchiocardiac veins through the direct

open-ings of anterior and posterior bars [35] Furthermore,

considering the localization of PO-CHH-producing

cells in the pericardial chamber, it may be pertinent to

suggest that these intrinsic multipolar PO-CHH cells

may be sensitive to homeostasis of hemolymph

Cloning of cDNA of PO-CHH of Cal sapidus

pro-duced only one size (2004 bp) that is translated into

PO-CHH neuropeptide The cDNA sequence of

PO-CHH encodes a preprohormone containing a

signal peptide (26 amino acid residue), one crustacean

hyperglycemic hormone precursor-related peptide

(CPRP, 36 amino acid residue), and PO-CHH, not

amidated at the C-terminus (71 amino acids) This cDNA of Cal sapidus PO-CHH contains a much longer long 3¢-UTR ( 1.5 kbp) than that of Car maenas (518–759 bp) [4] Interestingly, a putative cDNA encoding a PO-CHH type has been cloned in thoracic ganglia (TG) of Cal sapidus and other tissues [28] However, the immunohistochemisty study using

C o n t

r o l n

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o x i a

H y p o

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C o n t

r o l n

o r

o x i a

0

20

40

60

80

100

ES-CHH (fmol/mL hemolymph) 0

200

400

600

800

1000

a

b

c

Fig 6 Changes in hemolymph titers of PO-CHH and ES-CHH in

response to dissolved oxygen CHH control values were obtained

from animals in control normoxic water The closed bar shows a

significantly increased level of ES-CHH (P < 0.05, one-way ANOVA ,

Krustal–Wallis test, INSTAT ); the open bar is PO-CHH Bars represent

mean ± 1 SE (n = 9) Note the difference in the y-axis scales

between ES-CHH and PO-CHH.

Control Emersion

Glcuose (ug/mL hemolymph) 0

100

200

300

400

**

***

ES-

C

H ES-AK

E S-

eI F 4A

PO

CH

H

P O -A K PO-e

IF 4A

10 10

10 9

108

107

106

a

b

b a

b

b

b

b

b

a a

a

a a b

Hypoxia

Lactate (ug/mL hemolymph) 0

150

300

450

600

** *

** *

Control Emersion Hypoxia

A

B

C

Fig 7 Effect of hypoxia and emersion on glucose (A), lactate (B) and gene expression (C) (A, B) Open bars: controls at t = 0 Closed bars: 2 h after exposure Paired t-test showed the statistical signifi-cance at **P < 0.01 and ***P < 0.001 (C) The profiles of CHH,

AK and eIF4A expression in the ES and PO in response to hypoxia and emersion Closed bar: controls Hatched bars: hypoxia Crossed bars: emersion Bars represent mean ± 1 SE (n = 6) Statistical analysis was performed using one-way ANOVA (P < 0.05, Krustal– Wallis test, INSTAT ).

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anti-PO-CHH revealed exclusive positive staining in

the PO but not in TG (our unpublished observation),

suggesting that the putative cDNA encoding the

PO-CHH type cloned in TG is not translated into a

protein Similarly, for Car maenas, nine putative

cDNA sequences of PO-CHH are listed in GenBank, despite the fact that only one of these encodes the conceptual neuropeptide sequence of PO-CHH [4] The results of homologous and heterologous bio-assays of Cal sapidus ES-CHHs reflect high sequence identity (> 75%) of ES-CHHs between two crab spe-cies Our finding is in agreement with a previous report that the injection of Cal maenas ES-CHH triggered hyperglycemia in Can pagurus [30] Overall, such results of heterologous bioassays indicate that CHH receptors among these crab species may share some degree of similarity

Cal sapidus PO-CHH injection (20 pmol) did not cause hyperglycemia in the blue crab This finding is not unexpected, as a similar result was observed in Car maenas [4] The close sequence analysis of ES-CHH and PO-ES-CHH shows that the greatest homology

is in the first 40 amino acids, with much more differ-ence in the latter half of the sequdiffer-ence Such differdiffer-ences are common in all CHH sequences currently available

in GenBank, indicating that functionality inducing hyperglycemia may lie in the first 40 amino acid resi-dues [36–40] Therefore, it is suggested that these two CHHs may have separate receptors in their target tis-sues, where PO-CHH may be mobilizing glucose but not be directly involved in hyperglycemia in hemo-lymph PO-CHHs among Cal sapidus, Car maenas and P marmoratus share overall 67% sequence iden-tity, of which 85% and 68% are contributed by the first 40 residues and by the C-terminus, respectively [4,5] Thus, on the basis of the sequence identity among PO-CHHs, it is proposed that the physiological function of this CHH may be conserved in at least these crab species, although it has not yet been fully defined and understood

To define the physiological function of PO-CHH, the release pattern was evaluated along with that of ES-CHH in response to hypoxia The basal level in the

PO was surprisingly high at 10)11m, although it was 10-fold less than that of ES-CHH This difference in the concentrations of two CHHs seems to reflect the amount present in these tissues, approximately 2–

5 pmol, at least 20–50-fold less than that of ES-CHH (100 pmolÆES)1) It is noteworthy that the basal level

of ES-CHH is an order of magnitude greater in Cal sapidus (10)10m) than in Car maenas (10)11m) [24] or Can pagurus (< 10)11m) [20,23] Such a high CHH concentration in hemolymph of Cal sapidus may explain the high basal level of hemolymph glucose, which may reflect the behavioral differences among these species Moreover, crabs under hypoxia and emersion have shown differential redistribution of hemolymph to increase the flow, especially to the

60

120

180

*

**

***

22 to 22 22 to 29 22 to 4

100

200

300

Temperature (°C)

22 to 22 22 to 29 22 to 4 Temperature (°C)

**

S

-H C E A -S K -S I e

A 4

F -CH O P

K -O P O P

-eIF

A 4

C 1e+6

1e+7

1e+8

1e+9

a a b

A

B

C

Fig 8 Effect of hypothermia and hyperthermia on glucose (A),

lactate (B), and gene expression (C) (A, B) Open bars: controls at

t = 0 Closed bars: 2 h after exposure The results were analyzed

for statistical significance using a paired t-test (*P < 0.05,

**P < 0.01, ****P < 0.001) (C) The profiles of CHH, AK and eIF4A

expression in the ES and PO in response to hypothermia and

hyperthermia Closed bar: controls Hatched bar: hypothermia.

Crossed bar: hyperthermia Bars represent mean ± 1 SE (n = 6).

Statistical analysis was performed using one-way ANOVA (P < 0.05,

Krustal–Wallis test, INSTAT ).

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sternal artery, and overall cardiac output [41–43] Our

finding of the elevated ES-CHH level in hemolymph is

congruent with previous reports on CHH secretion

under hypoxia or emersion [20–24] Thus, our finding

supports the suggestion that PO-CHH and ES-CHH

have an adaptive role in the physiological response to

hypoxia

In crustaceans, it seems to be rather difficult to find

an ideal control gene for quantitative RT-PCR, the

level of which does not change during molting or

the reproductive cycle [7,44] As eIF4A, a member of

the DEAD box and ATP-dependent RNA helicase

family, may be considered as a temporal translation

indicator, because of its involvement in the assembly

of active polysome by unwinding secondary structure

in the 5¢-UTR of mRNAs [45], we reasoned that eIF4A

would be a good control gene as an indicator of the

level of translation Therefore, Cal sapidus cDNA of

the eIF4A gene was initially isolated, but the

expres-sion level of this gene was unexpectedly changed,

suggesting that it is sensitive to oxygen level

One hour of acute hypoxia and emersion induced

different expression levels of PO and ES-CHH

Chronic hypoxia caused downregulation of the

hemo-cyanin gene in the hepatopancreas in the same species

[46] Moreover, the degree of decrease in CHH

expres-sion in the ES is in proportion to that of CCAP

expression in the same tissue, as described in Chung

et al [47], but there is no change in CCAP of TG,

indicating the tissue-specific regulation of CCAP

expression Likewise, the present results concerning

PO-CHH and ES-CHH expression in response to

oxygen level suggest that the regulation of CHH

expression is different and tissue specific, perhaps via

tissue-specific alternative splicing or tissue-specific gene

expression through different regulatory arrangements

in the upstream promoter regions [37,38]

It is reasonable to suggest that the levels of

tran-scription of PO-CHH are in proportion to the demand

for its release, whereas the inhibition of ES-CHH

tran-scription may be caused by high glucose levels in

he-molymph On the other hand, the elevated hemolymph

glucose might have inhibited ES-CHH expression, as

a previous report indicated that CHH neurons are

hyperpolarized in response to 25 mm glucose in the

media [48] Hyperglycemia may also inhibit the further

release of CHH, whereas the low glucose level in

hemolymph may have a positive influence on the

release of CHH from SG in the ES, as described in

Chung & Webster [24] With these observations, it

would be interesting to see if in vitro incubation of the

ES in high-glucose media causes the inhibition of

CHH gene expression

We have shown the presence of ES-CHH neuropep-tides and the putative cDNA sequence of PO-CHH that

is translated into a neuropeptide in the PO The location

of intrinsic multipolar cells and structure of nerve branches in the PO indicate that these cells may be sensi-tive to changes in hemolymph homeostasis Changes in dissolved oxygen levels in seawater immediately affect the release of CHHs from the PO and SG, strongly suggesting that PO-CHH has an adaptive role, in partic-ular, in response to oxygen level Defining the phy-siological function of PO-CHH may seem to be a challenge, as the structural similarity of PO-CHH places

it as ‘a tacit CHH’, despite the fact that it does not induce hyperglycemia in hemolymph However, we have taken a positive step towards identifying a physiological function of PO-CHH, as its release is recorded under the changes in dissolved oxygen levels in seawater For the future, binding studies are required to identify its target tissues and second messenger, as the next step towards defining the physiological function of PO-CHH Furthermore, given the high sequence similarity of PO-CHH among Cal sapidus, Car maenas and P mar-moratus, the function of this neuropeptide may be simi-lar in these crab species, as is the function of ES-CHH

Experimental procedures Animals

Juvenile Cal sapidus (carapace width: 45–80 mm) were obtained from the blue crab hatchery program [49], Aqua-culture Research Center, Center of Marine Biotechnology, University of Maryland Biotechnology Institute, Baltimore,

MD and were maintained in individual compartments in artificial seawater [15 parts per thousand (p.p.t.) salinity and 22C] under ambient daylight conditions Experimen-tal animals were fed daily with chopped frozen squid and pelleted sea bream (EWOS, Surrey, Canada) All experi-mental animals were at intermolt stage [50]

Identification, isolation and quantification of neuropeptides from SGs and POs

Neuropeptides of SGs in the ES and PO were purified using RP-HPLC, as described in Chung & Webster [29] and Dir-cksen et al [4], respectively CHH peaks were initially iden-tified using ELISA with a combination of Carcinus CHH antisera, the method described in Wilcockson et al [23] Amino acid analysis was carried out for the quantification

of neuropeptides [29], and ESI MS of SG neuropeptides was used for mass determination Confirmation of the RP-HPLC fraction containing PO-CHH and its mass determi-nation were performed using SALDI

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RACE of PO-CHH

Total RNA from POs was extracted in TRIzol reagent and

quantified using RIBO green (Invitrogen) The GeneRacer

protocol (Invitrogen) was employed for the synthesis of

5¢-RACE and 3¢-5¢-RACE cDNAs from 1 lg of total RNA For

the first amplification of 3¢-RACE cDNA, a touchdown

PCR (TD-PCR) was used with a forward gene-specific

primer (LF1: 5¢-CAATCCATCAAAACCGTGTG-3¢) and

3¢ universal primer (Invitrogen) Conditions of TD-PCR

were as follows: initial denaturation at 94C for 3 min;

three cycles at 94C for 30 s, 54 C for 30 s, and 72 C for

2 min; three cycles at 94C for 30 s, 52 C for 30 s, and

72C for 2 min; three cycles at 94 C for 30 s, 50 C for

30 s, and 72C for 2 min; 24 cycles at 94 C for 30 s,

55C for 30 s, and 72 C for 2 min, and a final extension

at 72C for 7 min A nested PCR was carried out with

a forward gene-specific primer (LF2: 5¢-TGCTACAG

CAACTGGTGATCAGAAGGG-3¢) and 3¢ universal

nested primer (Invitrogen), with the following conditions:

after initial denaturation at 94C for 3 min, 30 cycles at

94C for 30 s, 60 C for 30 s, and 72 C for 2 min, and a

final extension at 72C for 7 min The PCR product was

electrophoresed on 1% agarose gel, and the band was

excised, extracted and cloned into a TOPO-TA vector for

sequencing The sequence of the 3¢-UTR was obtained by

primer walking using the gene-specific forward primer

(5¢-ATATAAGCTTATCCTCTGATAGC-3¢)

For 5¢-RACE, the same PCR conditions were employed

as described above for 3¢-RACE, using a gene-specific

reverse primer (LR1: 5¢-TTCCTGATCACCATGTT

GCTGT-3¢) and a 5¢ universal primer for the first PCR

Following this, the nested PCR was conducted using LR2

(5¢-GGGTGATTTGACACACGGTTTTGATGGA-3¢) and

5¢ nested universal primers (Invitrogen) The methods of

PCR analysis and cloning were as described above

Quantitative real-time RT-PCR

The cRNA standards of quantitative RT-PCR, including

PO-CHH and ES-CHH, AK and eIF4A, were initially

PCR amplified using a combination of LF and LR

prim-ers (Table 1) Further cRNA synthesis and RNA

quantifi-cation were performed as described in Chung & Webster

[6,7], with a modification for purification of in vitro

tran-scribed cRNAs (Ambion, Austin, TX, USA), eluting on a

spin-column (BD Biosciences, Mountainview, CA, USA)

Total RNA extracted from the tissues as described above

was treated with DNase, and each of 1 lg or 0.5

equiva-lent of PO RNAs were primed with random hexamers

for cDNA synthesis using avian myeloblastosis virus or

Moloney murine leukemia virus reverse transcriptase

Final cDNA samples were diluted to 40 lL, and 2 lL of

each sample was analyzed for the expression of genes

using SYBR gold (ABI, Foster City, CA, USA) on ABI

Prism with a pair of gene-specific primers (SFs and SRs; Table 1)

PO-CHH and ES-CHH antisera production C-terminal fragments of PO-(FDNMMFETCVQELFY PEDMLLVRDAIRG; Proteintech Group Inc., Chicago,

KIQVV-NH2; Invitrogen) were synthesized with the addi-tion of Cys at the N-terminus These modified synthetic peptides, after being N-terminally conjugated with bovine thyroglobulin using m-maleimidobenzoyl-N-succinimide ester [47], were used for antisera production in rabbits (Pro-teintech Group Inc., Chicago)

Whole-mount immunohistochemistry of PO Immediately after dissection, POs were fixed in a fixative containing 7% picric acid and 4% paraformaldehyde

in 0.1 m phosphate buffer (pH 7.4) overnight Procedures for washing and application of primary (· 1000 dilution) and secondary antiserum (Vector Laboratories, Burlingame,

CA, USA) were as described in Chung & Webster [5] Z-stacked images of PO preparations were collected using a Zeiss Confocal Microscope with a BioRad program (COMB, UMBI)

Bioassays of CHH neuropeptides Levels of glucose in hemolymph were estimated before and

2 h after injection of 10 or 20 pmol of each of ES-CHH and PO-CHH, oxidized CHH, and Car maenas ES-CHH, using the glucose assay described in Webster [20]

Iodination of neuropeptides and RIA The detailed procedures for iodination of ES-CHH and C-terminal synthetic peptide of PO-CHH, RIA and hemo-lymph sample preparation were as described in Chung & Webster [24,29] Standards of both RIAs ranged from

500 fmol per tube to 3.8 fmol per tube, and the detection limit was < 3 fmol per tube for both CHHs ED50values were 120 ± 5 and 134 ± 8 (fmol per tube) for SG-CHH and PO-CHH, respectively The results were analyzed using assayzap(Biosoft, Cambridge, UK)

Effects of environmental factors on the levels

of hemolymph and gene expression of CHH – dissolved oxygen, emersion and temperature Thirty minutes before the experiment, 5 L of artificial sea-water (15 p.p.t., 22 C) was continuously purged with nitro-gen to reduce the level of dissolved oxynitro-gen to < 0.5%

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(YSI 58 Dissolved Oxygen Meter) Test juvenile animals

(60–80 mm carapace width) were exposed for 1 h to

hyp-oxic seawater under continuous nitrogen purging, whereas

controls remained in aerated normoxic seawater At the

end of the 1 h exposure, either to anoxia or the control,

hemolymph samples were withdrawn from the

hypobran-chial sinus through the arthrodial membrane between the

chelae and the first walking leg, using a 1 mL syringe with

a 23-gauge needle The ES and PO were dissected out,

immediately frozen on dry ice, and kept at )80 C until

further processing

For emersion experiments, juvenile crabs were exposed to

air for 1 h at 22 C, whereas controls were maintained in

15 p.p.t artificial seawater at 22 C At the end of the

experiment, the hemolymph and tissue samples were

col-lected as described above

Hemolymph CHHs were estimated using RIAs after the

elution of hemolymphs on a Sep-Pak C18 column (Waters;

360 mg cartridges), as described in Chung & Webster

[24,29]

Temperatures

Juvenile crabs (45–60 mm carapace width) were initially

held at 22 C (15 p.p.t.) Once hemolymph samples were

drawn as described above at time 0, animals (n = 6) were

subjected for 2 h to the following temperatures: 29 C,

22 C, and 4 C The second hemolymph and tissue

sam-ples were collected at the end of exposure Total RNA was

extracted using the method described above

Statistical analysis

The data were tested for statistical significance using

graphpad instat version 3.0 (GraphPad Software, San

Diego, CA, USA)

Acknowledgements

The authors wish to thank Drs S G Webster

(Univer-sity of Wales, Bangor, UK) for amino acid analysis of

neuropeptides, and M M Ford for comments on the

manuscript We also wish to thank to Dr S Moore for

SALDI (Ciphergen) and Mr M Prescott for ESI MS

analyses (University of Liverpool) We are indebted to

Mr O Zmora and hatchery personnel for the young

juvenile crabs, and S Rogers and E Evans for

main-taining the water quality of the recirculation system

This article is contribution no 07-177 of the Center of

Marine Biotechnology (University of Maryland

Bio-technology Institute, Baltimore, MD) The work is

supported by a program grant (NA17FU2841) from

NOAA Chesapeake Bay Office to the Blue Crab

Advanced Research Consortium

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