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We used insect epidermis and cultured cells to define the role of the GBP signaling pathway in the enhancement of TH and DDC gene expression.. The downstream signaling pathways diverge to

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cascades regulate two separate groups of target genes

Yosuke Ninomiya1, Maiko Kurakake2, Yasunori Oda2, Seiji Tsuzuki2and Yoichi Hayakawa2

1 Graduate School of Environmental Earth Science, Hokkaido University, Sapporo, Japan

2 Department of Applied Biological Sciences, Saga University, Japan

In animals, tyrosine hydroxylase (TH, EC 1.14.16.2)

and 3,4-dihydroxy-l-phenylalanine (Dopa)

decarboxyl-ase (DDC, EC 4.1.1.26) are required for the

produc-tion of Dopa and dopamine [1,2] Because Dopa is

required for tanning of newly formed cuticle and

dopa-mine has been shown to exert many neurohormonal

functions in insects, both enzymes are essential for the

maintenance of life [3–6] Furthermore, Dopa and

dopamine are also oxidized by a system of

phenoloxid-ases and cofactors to form melanins that produce the

various black and brown patterns of the cuticles in a

broad range of insect species [7,8]

We previously demonstrated that transcription lev-els as well as enzyme activities of TH and DDC in larval cuticles are elevated during molt periods in the armyworm, Pseudaletia separata [9,10] Morpho-logical analysis showed preferential distribution of both enzymes in the epidermal cells beneath the black stripes in the dorsal surface of armyworm lar-vae Because the black stripes become much darker and wider after each larval ecdysis, both enzymes are thought to contribute to production of melanins during molts [9] Furthermore, the periodic expression of both enzyme genes was found to be

Keywords

calcium ion; Dopa decarboxylase;

extracellular signal-regulated kinase;

growth-blocking peptide; tyrosine hydroxylase

Correspondence

Y Hayakawa, Department of Applied

Biological Science, Saga University, Honjo-1,

Saga 840-8502, Japan

Fax ⁄ Tel: 81 952 28 8747

E-mail: hayakayo@cc.saga-u.ac.jp

(Received 9 October 2007, revised 4

December 2007, accepted 18 December

2007)

doi:10.1111/j.1742-4658.2008.06252.x

Growth-blocking peptide (GBP) is a 25 amino acid insect cytokine found

in lepidopteran insects that has diverse biological activities, such as larval growth regulation, paralysis induction, cell proliferation, and stimulation

of immune cells GBP also enhances expression of the tyrosine hydroxylase (TH, EC 1.14.16.2) and 3,4-dihydroxy-l-phenylalanine (Dopa) decarboxyl-ase (DDC, EC 4.1.1.26) genes, which elevate dopamine levels in insect epi-dermal cells We used insect epidermis and cultured cells to define the role

of the GBP signaling pathway in the enhancement of TH and DDC gene expression It has been recently reported that robust expression of the DDC gene requires activation of extracellular signal-regulated kinase (ERK) in epidermal cells of wounded Drosophila embryos This study con-firmed that GBP activates ERK, but this activation is not directly linked to the enhancement of TH and DDC gene expression One of the GBP path-way components is phospholipase C, whose activation is essential for the activation of ERK and elevation of expression of both enzyme genes The downstream signaling pathways diverge to ERK activation through acti-vated protein kinase C and expression of the enzyme genes through inositol triphosphate receptor-mediated Ca2+ influx from extracellular fluid Our data indicate that the diverged GBP signaling pathways enable GBP to exert completely different biological functions, even in a single cell type

Abbreviations

DAG, diacylglycerol; DDC, Dopa decarboxylase (EC 4.1.1.26); Dopa, 3,4-dihydroxy- L -phenylalanine; ERK, extracellular signal-regulated kinase; GBP, growth-blocking peptide; IP 3 , inositol triphosphate; MAP, mitogen-activated protein; MEK, mitogen-activated protein kinase kinase; PKC, protein kinase C; PLC, phospholipase C; PTTH, prothoracicotropic hormone; TH, tyrosine hydroxylase (EC 1.14.16.2).

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regulated by the insect cytokine, growth-blocking

peptide (GBP) [10]

GBP was initially identified as the factor responsible

for the reduced growth exhibited by P separata larvae

after parasitization by the parasitic wasp Cotesia

kar-iyai[11–13] Analysis of the mechanism by which GBP

retards larval growth revealed that GBP activates

DDC activities in epidermal cells and elevates

dopa-mine concentrations in the integuments [14–16]

Subse-quent studies provided evidence that part of the

increased dopamine in the integuments is released into

the hemolymph, and consequently retards the normal

development of armyworm larvae [15] Furthermore,

recent studies showed that the activation of DDC is

induced by its transcriptional enhancement through

GBP-induced elevation of cytoplasmic Ca2+

concen-trations in the epidermal cells [10] Therefore, we

spec-ulated that the increased level of cytoplasmic Ca2+

affects a certain transcription enhancer that stimulates

expression of the DDC gene A previous study also

suggested the involvement of mitogen-activated protein

(MAP) kinases in epidermal DDC expression: in

wounded Drosophila embryos, activation of

extracellu-lar signal-regulated kinase (ERK) is required for the

activation of DDC gene expression near wounded sites

in the epidermal integument [17]

In this study, we characterized the signal

transduc-tion pathway of GBP to clarify whether GBP can

acti-vate ERK and whether its activation is required for

the expression of TH and DDC genes Using insect

integuments and cultured cells, we demonstrated that

GBP activates ERK but that its activation is not

nec-essary for the induction of expression of either enzyme

gene

Results

GBP-induced activation of ERK in integuments

Prior studies showed that expression of TH and DDC

genes was enhanced in integuments isolated from

armyworm larvae when they were incubated with GBP

[10] We examined whether GBP induces dual

phos-phorylation (activation) of ERK in the larval

integu-ments under the same conditions As shown in

Fig 1A, dual phosphorylation of ERK was clearly

enhanced when the integuments were incubated with

10 nm GBP for 5 min, but this phosphorylation was

completely blocked by U0126, a MAP kinase kinase

(MEK) inhibitor that reduces the phosphorylation and

activation of the ERK–MAP kinase In contrast,

addi-tion of U0126 to the incubaaddi-tion medium did not

pre-vent GBP-induced expression of TH and DDC genes

(Fig 1B), thus indicating that activated ERK is not required for GBP-induced gene expression of either enzyme in epidermal integuments isolated from army-worm larvae

GBP-induced ERK activation in MaBr4 cells For the detailed characterization of transcriptional reg-ulatory inputs involved in GBP-dependent activation

of expression of TH and DDC genes, we used cultured

dpERK

ERK

TH

DDC

Actin

4 3 2

1 0

*

0 n M GBP 10 n M GBP 10 n M GBP/U0126

0 n M GBP 10 n M GBP 10 n M GBP/U0126

A

B

Fig 1 Effect of GBP on ERK activation and expression of the TH and DDC genes in the dorsal integument of day 1 last instar larvae

of the armyworm (A) Western blots of ERK The antibody employed specifically recognizes dually phosphorylated (activated) ERKs Phosphorylation of ERK was observed in the integument after incubation with 10 n M GBP at 25 C for 5 min A MEK inhibi-tor (10 l M , U0126) inhibited GBP-induced phosphorylation of ERK Each bar indicates the mean ± SD of three independent determina-tions *Significantly different from control (0 n M GBP; P < 0.05, Student’s t-test) (B) RT-PCR analysis of TH and DDC gene expres-sion Clear bands of TH and DDC were expressed in the integu-ment after incubation with 10 n M GBP, and expression of both enzyme genes was not inhibited by U0126 dpERK, dually phos-phorylated ERK *Significantly different from control (0 n M GBP;

P < 0.05, Student’s t-test).

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insect cells instead of the epidermal integuments,

because we had observed that addition of chemicals

and long incubation caused unexpected damage to the

isolated integument To select the best cultured cells

for following studies, we tested both enzyme gene

expression and ERK activation of some cultured cells,

including Sf9, MaBr3, and MaBr4 cells, and found

that only MaBr4 cells show clear expression of both

enzyme genes and the ERK activation, as shown in

Fig 2 Activation of ERK was observed 8 min after

the cells were simply transferred from 4 to 25C

(Fig 2A), and at that time, the TH and DDC genes were clearly expressed in the cells (Fig 2B) Further-more, the GBP-induced gene expression of both enzymes was highly enhanced only in the Ca2+ -con-taining medium (Fig 2C)

To check whether GBP elevates cytoplasmic Ca2+ concentrations in MaBr4 cells, Ca2+ concentrations in those cells were monitored using a laser confocal microscope Addition of GBP to the incubation med-ium elevated the cytoplasmic Ca2+ concentrations in MaBr4 cells, but BSA did not change the Ca2+ con-centrations at all (Fig 3), indicating that, in analogy

to the epidermal cells, MaBr4 cells have the property

of increasing cytoplasmic Ca2+ concentrations by GBP [10]

GBP showed a dose-dependent capacity to activate ERK, as shown in Fig 4A The activation of ERK was roughly proportional to the concentration of GBP

up to 100 nm Furthermore, GBP-induced activation

of ERK was detected with the presence of EGTA (Fig 4B) Whereas a slight enhancement of ERK phosphorylation was also observed when the concen-tration of Ca2+added to the medium exceeded that of EGTA (Fig 4B), the calcium ionophore A23187 did not activate ERK at all (Fig 4C) These results imply that GBP stimulates more than one signaling pathway leading to activation of ERK, and that among them,

at least one pathway is Ca2+-independent

GBP-induced ERK activation requires MEK The GBP-induced activation of ERK was observed transiently 5 min after addition of GBP to the culture medium of MaBr4 cells (Fig 5A) This GBP-depen-dent ERK activation was completely blocked by 10 lm U0126 (MEK inhibitor), indicating that the GBP sig-naling pathway requires MEK activity (Fig 5B) Furthermore, to test whether the GBP-induced expression of TH and DDC genes requires ERK acti-vation, expression of both enzyme genes was measured

in MaBr4 cells stimulated by GBP in the presence of U0126 GBP clearly enhanced expression of both enzyme genes even in the presence of 10 lm U0126, indicating that the GBP signaling pathway for the stimulation of TH and DDC gene expression does not require the activated ERK (Fig 5C)

Analysis of GBP signaling pathways

It is now apparent that the GBP signaling pathways diverge from a certain component into at least two pathways: one towards ERK activation, and the other towards TH and DDC gene expression To

On ice for 1h/25o C incubation time

dpERK

ERK

Marker TH DDC Actin

TH

DDC

Actin

6 min 8 min

* *

10 n M GBP

10 n M GBP 10 n M BSA

3 m M CaCl23 m M CaCl2 3 m M CaCl2

2 m M EGTA 2 m M EGTA 2 m M EGTA 2 m M EGTA 2 m M EGTA

5

4

3

2

1

0

A

B

C

Fig 2 ERK activation and expression of TH and DDC genes in

MaBr4 cells (A) Western blots of ERK Phosphorylation of ERK in

Mabr4 cells was observed 8 min after transfer from 4 to 25 C (B)

RT-PCR analysis of expression of TH and DDC genes RNAs were

prepared from MaBr4 cells 8 min after transfer from 4 to 25 C (C)

RT-PCR analysis of GBP-induced expression of TH and DDC genes.

Total RNA was prepared from MaBr4 cells after incubation with

the indicated chemicals at 25 C for 6 h Each bar indicates the

mean ± SD of three independent determinations *Significantly

different from control (0 n M GBP; P < 0.05, Student’s t-test).

**Significantly different from control (0 n M GBP; P < 0.01,

Student’s t-test).

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characterize these pathways, the possible participation

of some components of a classic signal transduction

cascade was tested Neither elevation of the gene

expression of both enzymes nor ERK activation was

observed after the addition of 2 lm U73122, a

phos-pholipase C (PLC) inhibitor, to the MaBr4 cell culture

medium (Fig 6) However, whereas the addition of

10 lm chelerythrine chloride, a protein kinase C

(PKC) inhibitor, did not abolish the GBP-dependent

expression of both enzyme genes, it did block the

ERK activation (Fig 6) In contrast, the addition of

10 lm TMB-8, an inositol triphosphate (IP3) receptor

antagonist, did not inhibit the GBP-induced ERK

acti-vation, but abolished the elevation of expression of

both enzyme genes (Fig 6)

These results clearly indicate that the GBP signaling

events initially activated PLC, which activates ERK

through activation of PKC Furthermore, IP3produced

by activated PLC initiates the signaling cascade that

ultimately triggers Ca2+ entry from the extracellular

fluid The elevation of the cytoplasmic Ca2+

concen-tration enhances the expression of TH and DDC genes (Fig 7)

Discussion

In the present study, we demonstrated that GBP induces dual phosphorylation (activation) of ERK in the integuments of armyworm larvae This observa-tion, together with a previous report indicating that robust induction of DDC gene expression requires activated ERK–MAP kinase in wounded Drosophila embryos [17], suggested the possibility that the GBP-induced enhancement of expression of TH and DDC genes also requires activated ERK To assess this pos-sibility, the GBP–ERK pathway was examined in epi-dermal integuments Addition of the MEK inhibitor U0126 to the isolated integument culture medium com-pletely blocked GBP-induced ERK phosphorylation in the tissues, but expression of the TH and DDC genes was enhanced These results were interpreted to mean that the GBP signaling pathway towards the

A

B

Fig 3 Monitoring cytoplasmic Ca2+concentrations in MaBr4 cells incubated with BSA (A) and GBP (B) Ca2+concentrations in MaBr4 cells containing Fluo-3AM were monitored at 5 min after addition of 10 n M BSA or GBP (a) Laser transmission images (b) Ca 2+ indicator Fluo-3AM fluorescence images (green) (c) Fluorescence images overlaid with the laser transmission images.

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expression of both enzyme genes is mediated

indepen-dently of ERK activation To assess this interpretation,

follow-up analysis was conducted using cultured

MaBr4 insect cells

Although MaBr4 cells were originally derived from

the larval fat body of Mamestra brassicae, a species

closely related to P separata, their morphology is

rather hemocyte-like [18] GBP-induced activation of

dpERK ERK

dpERK ERK

4

2

0

4

2

0

4

2

0

*

*

*

*

dpERK ERK

0 n M GBP 1 n M GBP 10 n M GBP 100 n M GBP

2 m M EGTA 2 m M EGTA

10 n M GBP

2 m M EGTA/3 m M CaCl2

10 n M GBP

10 n M GBP 0 0.5 5

DMSO

A23187 concentration (µ M )

A

B

C

Fig 4 Effect of Ca 2+ on GBP-induced activation of ERK in MaBr4

cells (A) Effects of various concentrations of GBP on ERK

phos-phorylation MaBr4 cells were incubated with GBP at 25 C for

5 min *Significantly different from control (0 n M GBP; P < 0.05,

Student’s t-test) (B) Requirement of Ca 2+ for GBP-induced

phos-phorylation of ERK MaBr4 cells were incubated with the indicated

chemicals at 25 C for 5 min **Significantly different from control

(0 n M GBP; P < 0.01, Student’s t-test) (C) Effect of various

concen-trations of the calcium ionophore A23187 on ERK phosphorylation.

MaBr4 cells were incubated with various concentrations of A23187

at 25 C for 5 min Because A23187 was dissolved in

dimethylsulf-oxide, dimethylsulfoxide (final concentration 0.1%) was added to

the incubation medium Only the control incubation contained GBP

(10 n M ) **Significantly different from control (10 n M GBP;

P < 0.01, Student’s t-test) Each bar indicates the mean ± SD of

three independent determinations.

dpERK

ERK

dpERK

ERK

5 4 3 2 1 0

4

0 2

4

2

0

4

2

0 4

0 2

TH DDC Actin

*

A

B

C

Fig 5 Effect of MEK inhibitor on GBP-induced ERK activation and enhancement of TH and DDC gene expression inMaBr4 cells (A) Effect of incubation time on GBP-induced phosphorylation of ERK MaBr4 cells were incubated with or without 10 n M GBP in the medium containing 0.1% dimethylsulfoxide at 25 C Phosphoryla-tion of ERK was observed 5 min after addiPhosphoryla-tion of GBP to the MaBr4 incubation medium Closed and open bars: with and without GBP, respectively **Significantly different from control (0 min;

P < 0.01, Student’s t-test) (B) Effect of MEK inhibitor on GBP-induced ERK phosphorylation U0126 (10 l M ), a MEK inhibitor, completely inhibited GBP-induced ERK phosphorylation Other explanations as in (A) (C) Effect of MEK inhibitor on enhancement

of TH and DDC gene expression MaBr4 cells were incubated at

25 C for 6 h after addition of the indicated chemicals, and total RNA was prepared The GBP-induced expression of TH and DDC mRNAs was not blocked by the MEK inhibitor *Significantly differ-ent from control (0 n M GBP; P < 0.05, Student’s t-test) Each bar indicates the mean ± SD of three independent determinations.

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ERK was transiently observed at 5 min after addition

of GBP to the incubation medium of MaBr4 cells The

involvement of a MAP kinase kinase (MEK) in the

ERK activation pathway [19] was tested by evaluating

the effect of U0126 U0126 completely abolished the

temperature-dependent activation of ERK, indicating

that ERK activation in MaBr4 cells proceeds through

the common pathway characterized in mammalian

cells

Prior studies indicated that GBP induces Ca2+

influx into brain synaptosomes and epidermal cells

[10,20] Especially in the latter, the enhancement of

TH and DDC gene expression was demonstrated to be

accompanied by GBP-induced elevation of the cyto-plasmic Ca2+concentration We examined whether the GBP-induced activation of ERK requires Ca2+ influx into MaBr4 cells Excess amounts of EGTA did not block the GBP-induced ERK activation Furthermore, the calcium ionophore A23187 did not activate ERK

at all, even at a concentration of 5 lm, suggesting that the GBP-dependent activation of ERK does not require Ca2+ influx into MaBr4 cells However, the GBP-induced enhancement of TH and DDC gene expression was completely abolished by EGTA Fur-thermore, the GBP-dependent expression of both enzyme genes was observed in the presence of the MEK inhibitor, thereby demonstrating that the GBP-dependent enhancement of expression of the enzyme genes in MaBr4 cells is independent of the ERK–MAP kinase pathway

As U73122 (PLC inhibitor) has been shown to block the formation of IP3 in several insect tissues [21,22],

we applied it to MaBr4 cells The inhibitory effect of U72122 on ERK and expression of the enzyme genes clearly demonstrated that GBP signaling events ini-tially activate PLC The PLC-triggered metabolism of membrane phospholipids produces diacylglycerol (DAG) and IP3 Because chelerythrine chloride, a PKC inhibitor, abolished GBP-dependent activation of ERK, the PLC-produced DAG would contribute to activation of PKC [23–25] In contrast, the observation that TMB-8, an IP3receptor antagonist, blocked

GBP-TH

DDC

Actin

Control PLC inhibitor IP 3 R antagonist PKC inhibitor

*

*

*

*

5

4

3

2

1

0

Control PLC inhibitor IP 3 R antagonist PKC inhibitor

**

**

dpERK

ERK

5

4

3

2

1

0

Fig 6 ERK activation and TH and DDC gene expression in the

presence of various inhibitors MaBr4 cells were incubated with or

without 10 n M GBP in the medium containing 0.1%

dimethylsulfox-ide with 2 l M U73122 (PLC inhibitor), 10 l M TMB-8 (IP3receptor

antagonist), or 10 l M chelerythrine chloride (PKC inhibitor) at 25 C

for 6 h, and total RNA was prepared from cells after incubation.

Phosphorylation of ERK was observed 5 min after addition of

10 n M GBP to the MaBr4 incubation medium Each bar indicates

the mean ± SD of three independent determinations *Significantly

different from control (0 n M GBP; P < 0.05, Student’s t-test)

**Sig-nificantly different from control (0 n M GBP; P < 0.01, Student’s

t-test).

Fig 7 Schematic representation of hypothesized GBP signaling pathways in MaBr4 cells Stimulation of the putative GBP receptor activates PLC DAG, newly formed by activated PLC, stimulates PKC, and activated PKC induces ERK activation Independently of this signaling pathway, the IP 3 produced by activated PLC stimu-lates the IP3receptor to release Ca 2+ from the endoplasmic retic-ulum, which leads to the extracellular Ca 2+ influx that induces robust enhancement of TH and DDC gene expression ER, endo-plasmic reticulum; GBPR, growth-blocking peptide receptor; IP3R,

IP3receptor.

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dependent expression of both enzyme genes suggested

that the IP3 receptor-mediated Ca2+ influx from the

extracellular fluid plays an essential role in the

tran-scriptional enhancement of TH and DDC genes

(Fig 7) Although the GBP signaling pathways were

characterized by analyzing MaBr4 cells, it is

reason-able to assume that these pathways are employed in

armyworm epidermal cells It has been reported that

prothoracicotropic hormone (PTTH) stimulates Ca2+

influx into the prothoracic gland and also activates

ERK in the tobacco hornworm Manduca sexta

[26–28] PTTH-induced ERK activation is strongly

dependent on external Ca2+, and ERK activation is

induced by substitution of the calcium ionophore

A23187 for PTTH Therefore, the PTTH-induced

events in the prothoracic gland seem to be completely

different from those observed in the GBP signaling

pathway in the epidermis and MaBr4 cells

Once GBP was identified as a growth inhibitory

pep-tide in insects, a series of follow-up studies revealed its

diverse biological functions, including paralysis

induc-tion, cell proliferainduc-tion, and stimulation of immune cells

[29–31] This study clearly characterized two different

signaling pathways of GBP in epidermal cells and

cul-tured MaBr4 cells Although the multiple activities

reported for GBP may reflect differences in the types

of GBP receptors expressed by specific tissues or

devel-opmental stages of insects, divergence of the GBP

signaling pathway must also enable GBP to exert

different activities in the same cell

In summary, this study provides unequivocal

evi-dence that GBP stimulates Ca2+ influx into cultured

MaBr4 cells and subsequent enhancement of

expres-sion of the TH and DDC genes Furthermore, GBP

stimulates ERK phosphorylation, which is not

essen-tial for the enhancement of expression of either

enzyme gene One of the GBP pathway components

is PLC, from which the downstream signaling

path-ways diverge to ERK activation through PKC and

enzyme gene expression through IP3

receptor-medi-ated Ca2+ influx Therefore, it is reasonable to

con-clude that the GBP signaling pathway to expression

of the TH and DDC genes is unique in its ability to

function independently of the ERK–MAP kinase

kinase pathway

Experimental procedures

Animals

Pseudaletia separata larvae were reared on an artificial diet

at 25 ± 1C with a 16 h light ⁄ 8 h dark photoperiod [10]

Penultimate instar larvae undergoing ecdysis between 4 and

4.5 h after starting the light period were designated as day 0 last instar larvae

Chemicals Polyclonal antibody to MAP kinase (ERK-1, ERK-2), U0126, U73122, TMB-8 and chelerythrine chloride were purchased from Sigma-Aldrich Co (St Louis, MO, USA) Monoclonal antibody to active MAP kinase was obtained from Promega Co (Madison, WI, USA) A23187 (calcium ionophore) and Grace’s medium (Cat No 11595-030) were purchased from Nacalai Tesque Co (Kyoto, Japan) and Invitrogen Co (Carlsbad, CA, USA), respectively All other chemicals were of reagent grade

Dissection and culture of integument

A whole abdominal integument between the first and sec-ond segments was dissected from the test day 1 last instar larva of the armyworm Care was taken to remove all the adhering fat body tissue from the integument The dissected integument was separated into dorsal and ventral parts After being washed with NaCl⁄ Pi, the tissues were lightly blotted with filter paper, weighed, and immediately used for experiments

Pieces of dorsal larval integument were cultured in Grace’s medium with or without 10 nm GBP at 25C As

a control, 10 nm BSA was added to the medium To remove extracellular free Ca2+, Grace’s medium containing

1 mm EGTA was used A23187 was dissolved in dimethyl-sulfoxide and added to the medium

Cell culture The MaBr4 cell line established from M brassicae fat bodies was kindly provided by T Hiraoka (Tokyo Univer-sity of Agriculture and Technology), and maintained in Mitsuhashi⁄ Maramorosh insect medium (MM medium) at

25C [18]

RT-PCR and quantitative PCR Total RNA was isolated from integuments of test tissues or cultured cells using TRIzol reagent (Gibco-BRL, Rockville,

MD, USA), according to the manufacturer’s instructions Two micrograms of total RNA was reverse transcribed with oligo(dT) primer using ReverTra Ace (Toyobo, Osaka, Japan) The cDNA was amplified with a TH-specific primer pair (5¢-CAGCTGCCCAGAAGAACCGCGAGATG-3¢, +11 to +36 bp and 5¢-GAACTCCACGGTGAACCAGT-3¢, +1286 to +1305 bp), a DDC-specific primer pair (5¢-ATGGAGGCCGGAGATTTCAAAG-3¢, +1 to +22

bp and 5¢-ACGGGCTTTAAGTATTTCATCAGGC-3¢, +1405 to +1428 bp), and an actin primer pair (5¢-TTCG

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AGCAGGAGATGGCCACC-3¢ and 5¢-GAGATCCACAT

CTGYTGGAAGGT-3¢) PCR was conducted under the

following conditions: 25 cycles at 94C for 1 min, 50 C

for 1 min, and 72C for 2 min

Real-time quantitative PCR was used to determine the

relative expression levels of TH and DDC Quantitative

PCR was carried out with 2.5% of the reverse transcription

product in a 20 lL reaction volume of LightCycler Fast

DNA Master SYBR Green I (Roche Applied Science,

Indi-anapolis, IN, USA), using the Light-Cycler 1.2 instrument

and software (Roche Applied Science)

Immunoblotting analysis

Integuments dissected from larvae or cultured cells were

homogenized in 80 mm Tris⁄ HCl buffer (pH 8.8)

contain-ing 1% SDS and 2.5% 2-mercaptoethanol, and centrifuged

at 20 000 g for 10 min at 4C The supernatant was boiled

for 5 min and applied to SDS⁄ PAGE gel Proteins

sepa-rated by SDS⁄ PAGE were electrically transferred to a

poly(vinylidene difluoride) membrane filter, blocked, and

probed with the indicated primary antibody After being

washed thoroughly with 0.05% Tween-20 in Tris-buffered

saline (10 mm, 150 mm NaCl, pH 7.5), antigens were

detected using peroxidase-conjugated secondary antibody

and a 4-chloro-1-naphtol (4CN) Immun-Blot Colorimetric

Assay kit (Bio-Rad Laboratories, Hercules, CA, USA) [32]

All positive bands were quantified using imagej (NIH)

Confocal calcium imaging

MaBr4 cells were washed with Ca2+-free Carlson solution

(120 mm NaCl, 2.7 mm KCl, 0.5 mm MgCl2, 1.7 mm

NaH2PO4, 1.4 mm NaHCO3, 2.2 mm glucose), and loaded

with 10 lm Fluo-3AM (Dojindo Laboratories, Kumamoto,

Japan) at 25C for 30 min After loading, the cells were

washed twice in Ca2+-free Carlson solution by

sedimenta-tion and resuspension, and placed on the slide glass The

cells were stimulated with Grace’s medium with or without

1 nm GBP and immediately excited with light of 488 nm

wavelength by a confocal imaging system CellMap (Carl

Zeiss, Oberkochen, Germany)

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