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Tiêu đề Development of Renal-targeted Vectors Through Combined In Vivo Phage Display and Capsid Engineering of Adenoviral Fibers from Serotype 19p
Tác giả Laura Denby, Lorraine M Work, Dan J Von Seggern, Eugene Wu, John H McVey, Stuart A Nicklin, Andrew H Baker
Trường học University of Glasgow
Chuyên ngành Gene Therapy and Vector Engineering
Thể loại Research Article
Năm xuất bản 2007
Thành phố Glasgow
Định dạng
Số trang 8
Dung lượng 585,47 KB

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Development of Renal-targeted Vectors Through Combined In Vivo Phage Display and Capsid Engineering of Adenoviral Fibers From Serotype 19p 1 British Heart Foundation Glasgow Cardiovascu

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Development of Renal-targeted Vectors Through

Combined In Vivo Phage Display and Capsid

Engineering of Adenoviral Fibers From Serotype 19p

1 British Heart Foundation Glasgow Cardiovascular Research Centre, University of Glasgow, Glasgow, UK; 2 Department of Immunology,

Scripps Research Institute, La Jolla, California, USA; 3 Department of Biochemistry, Duke University Medical Center, Durham, North Carolina, USA;

4 Haemostasis and Thrombosis, Medical Research Council Clinical Sciences Centre, Imperial College London, London, UK

The potential efficacy of gene delivery is dictated by the

infectivity profile of existing vectors, which is often

restric-tive In order to target cells and organs for which no

effi-cient vector is currently available, a promising approach

would be to engineer vectors with novel transduction

profiles Applications that involve injecting adenovirus

(Ad) vectors into the bloodstream require that native

tropism for the liver be removed, and that targeting

moieties be engineered into the capsid We previously

reported that pseudotyping the Ad serotype 5 fiber for

that of Ad19p results in reduced hepatic transduction In

this study we show that this may be caused, at least in

part, by a reduction in the capacity of the Ad19p-based

virus to bind blood coagulation factors It is therefore

a potential candidate for vector retargeting, focusing

on the kidney as a therapeutic target We used in vivo

phage display in rats, and identified peptides HTTHREP

and HITSLLS that homed to the kidneys following

intra-venous injection We engineered the HI loop of Ad19p to

accommodate peptide insertions and clones Intravenous

delivery of each peptide-modified virus resulted in

selec-tive renal targeting, with HTTHREP and HITSLLS-targeted

viruses selectively transducing tubular epithelium and

glomeruli, respectively Our study has important

implica-tions for the use of genetic engineering of Ad fibers to

produce targeted gene delivery vectors

Received 15 December 2006; accepted 25 April 2007; published online

5 June 2007 doi: 10.1038/sj.mt.6300214

IntroductIon

Gene delivery is limited by the ability of available vector systems

(either viral or non-viral) to deliver sufficient levels of therapeutic

transgenes to target cells and tissues in vivo to provide an

effica-cious phenotype For strategies based on the commonly used

delivery that is restricted only to defined cell types such as liver

hepatocytes Access to local tissue can enable tissue transduction

to be carried out, but access to therapeutically relevant targets is often impossible or impractical In this context, there is a need to develop targeting strategies to enable gene delivery to these sites

in vivo Such strategies have evolved rapidly in recent years and

include utilization of alternate vector serotypes as well as meth-odologies to alter the infectivity of existing vectors, including peptides and antibody targeting systems In many of these strate-gies, however, the required route of delivery is via the bloodstream with “homing” of the vector to the target tissue Alternative sero-types of some commonly used vectors have been isolated, and many possess alternative tropism on account of differences in cell tethering and entry mechanisms, thereby enabling targeting

to defined tissues For example, adeno-associated virus serotypes

6 (AAV-6) and 9 (AAV-9) show significant levels of delivery of genes to skeletal and cardiac muscle following intravenous injec-tion, when compared with AAV-2, thereby potentially accelerat-ing the development of gene therapeutics for skeletal and cardiac

number of alternate serotypes are available, altered cell infectivity can be achieved For example, Ad vectors engineered with many subgroup B fibers target CD46, thereby altering infection at the

via the bloodstream The fiber protein exposed on the surface of the adenoviral capsid is the main determinant of tropism, and has been the predominant target of retargeting strategies (reviewed in Ref 9) In the case of Ad5, extensive mutagenesis of the fiber has resulted in reduced liver transgene expression but has not enabled

that there are still some uncertainties about the extent to which

receptors in the liver are utilized by Ad5 vectors in vivo Recently

there have been reports of the important role played by blood serum proteins, including coagulation factors IX (FIX) and X (FX), in driving hepatic delivery of Ad5 through heparan sulphate proteoglycans (HSPGs) and/or low-density lipoprotein

Ad vectors based on serotype 5 will likely require elimination of coagulation factor binding Because coagulation factor binding

Correspondence: Andrew H Baker, British Heart Foundation Glasgow Cardiovascular Research Centre, University of Glasgow, 126 University Place,

Glasgow G12 8TA, UK E-mail: ab11f@clinmed.gla.ac.uk

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is probably mediated through the fiber,13 an alternative approach

would be to identify serotypes that show reduced coagulation

factor binding We previously reported that the fiber of serotype

19p, a subgroup D virus not associated with any known human

disease, exhibits severely reduced liver tropism when delivered

intravenously into rats, and this was in the absence of enhanced

potential platform on which to build a targeting system for

deliv-ery of genes to non-hepatic tissue

poten-tial for in vivo targeting of Ad following intravascular injection,

and appropriate targeting sequences can be identified by

tech-niques including in vivo phage display The flexibility of phage

display allows entire peptide repertoires to be screened in vitro,

ex vivo, or in vivo in order to isolate highly efficient and

that it is possible to identify small peptide motifs that target the

vasculature of defined tissues and organs following intravenous

tech-nology to the delivery of bioactive therapeutics, using peptides

isolated by phage display, has potential clinical utility, and this

has already been proven in a limited range of applications For

example, intravenous administration of peptides isolated for

spe-cifically targeting tumors or white fat, when coupled to drugs and

pro-apoptotic peptides, resulted in tumor regression or fat

and selective in vivo gene delivery by viral vector systems has been

somewhat slower to emerge, because this involves genetic

engi-neering of complex viral capsid proteins We have therefore

uti-lized Ad5 pseudotyped with the Ad19p fiber in order to develop

targeted viral gene therapy vectors by intravenous administration,

by combining in vivo phage display with the genetic engineering

of the HI loop of Ad serotype 19p fibers We have focused on the

kidney as a therapeutic target because it is fundamentally

impor-tant in a range of diseases and there is a clear absence of suitable

vector systems for non-invasive targeting

results

Binding of coagulation factors and resulting

cell infectivity is reduced with Ad19p as

compared to Ad5

We previously reported that replacing the Ad serotype 5 fiber with

has been found that an important mechanism for hepatic

seques-tration of Ad vectors is the binding of blood coagulation factors,

such as FIX and FX, to the capsid so as to “bridge” the virus to

HSPGs and/or low density lipoprotein receptor-related protein in

concen-trations of FIX or FX exerted any influence on Ad19p-mediated

transduction, and compared the results with Ad5 (using a

wild-type fiber, Ad5 and a coxsackievirus and Ad receptor

by both FIX and FX Ad19p-mediated transduction was also

significantly enhanced by FIX and FX, but to substantially lower

16

a

b

c

d

6 ) 14 12 10 8 6 4 2

160

3 )/mg protei

n 140 120 100 80 60 40 20 0 Ad5 Virus injection

�RU

�RU start

Time (s)

end

Ad5

Ad5

Ad19p-Eco47

Ad19p-Eco47

Ad19p-Eco47

+FIX +FX

CHO-KI CHO-pgsA745 Ad19p + FIX + FX + FIX + FX + FIX + FX

− +FIX +FX

+FIX +FX

− +FIX +FX

100 75 50 25 0 0.00 0.25 0.50 Virus titre (× 1011) 0.75 1.00 1.25

Figure 1 Assessment of coagulation factor binding by modified viruses (a) HepG2 cells were distributed in the plates 24 hours prior

to infection Plated cells were washed in phosphate-buffered saline (PBS) and 50 µl of serum free media with physiological levels (1 IU/ml)

of either factor IX (FIX) or FX added This was followed by infection with the appropriate Ad at 10,000 virus particles (VP)/cell Cells were incubated for 3 hours at 37 °C before being washed and the media replaced Cells were incubated for 72 hours before quantification of

transgene expression *P < 0.05 versus transduction in the absence

of clotting factors (b) CHO-K1 (wild-type) and CHO-pgsA745

the effects and mechanisms of coagulation factors on Ad19p-modi-fied vector transduction Plated cells were washed in PBS and 50 µl of serum free media with physiological levels (1 IU/ml) of either FIX or

FX added This was followed by infection with 20,000 VP/cell of the appropriate Ad Cells were incubated for 3 hours at 37 °C before being washed and the media replaced Cells were incubated for 48 hours

before quantification of transgene expression *P < 0.05 versus

trans-duction in the absence of clotting factors (c, d) Ad5 or Ad19p vectors

immo-bilised onto a CM-5 sensor chip in 50 mmol/l Tris pH 7.4; 150 mmol/l

25 °C Depicted are sensorgrams of c FX (showing specific binding) of

Ad5 and, to a lesser extent, Ad19p-Eco47 (d) The steady state change

(δRU) in respiratory unit (RU) on binding of the virus to the FX was

plotted against virus concentration CHO, Chinese hamster ovary; RLU, relative light units.

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levels than with AdKO1 and Ad5 (Figure 1a) This suggests that

Ad19p may show reduced binding to coagulation factors To

investigate this further we utilized two approaches, one

surface plasmon resonance (SPR) First, wild-type CHO-K1 cells

were transduced with Ad5 and Ad19p in the presence or absence

of FIX and FX Basal levels of transduction for both Ad5 and

Ad19p were low, likely reflective of lack of primary receptor

an effect that was ablated in CHO-pgsA745 cells, thereby

demon-strating that coagulation factor-mediated cell transduction relies

showed enhanced transduction in CHO-K1 cells but, in

in CHO-pgsA745, thereby demonstrating that binding of the

Ad19p:FX complex to the cell surface occurs through HSPG (Figure 1b) Next, in order to examine the direct interaction of the Ad5 and Ad19p viruses with FX, we carried out SPR analy-sis FX was covalently coupled to biosensor chips and the virus (at varying concentrations) was injected Both viruses showed specific binding to FX, but there was a substantially weaker

interac-tion was calcium-dependent, consistent with the characteristics

Ad19p showed substantially reduced binding to FX in

that viruses with fibers derived from Ad19p show lower levels of binding and sensitivity to the coagulation factor pathway than Ad5 does This, at least in part, may be the underlying cause of

suggests that Ad19p fibers have a potential role to play in vector targeting strategies with intravascular injection routes

Identification of renal homing peptides by in vivo

phage display

Using Wistar Kyoto (WKY) rats, we carried out three rounds of

in vivo phage display to identify peptides that had the ability to

Twelve- to thirteen-week-old WKY rats (n = 3 rats/phage display

were recovered, titered and normalized per gram of tissue By the third round, we observed selective enrichment of the phage display library for the kidney in comparison with non-target

analy-sis of phage in the kidneys (>200 individual phage for rounds 2

found in all tissues This highlights the fact that phage display has the potential to identify peptides on the basis of either ubiquitous

or tissue-selective markers From the sequencing analysis, the peptides HTTHREP (HTT) and HITSLLS (HIT) were selected for the experiments, as they were found to be exclusively selective

In order to assess the kidney targeting capacity of each pep-tide, we injected animals with a high titer stock of each individual phage We utilized a pre-dosing regimen wherein animals were injected with control (not expressing a peptide) phage 5 minutes prior to injection of the candidate peptide-expressing phage (Figure  3a), as we have described previously.25 Pre-dosing was

Phage IV infusion

5 min circulation,

saline perfusion

9

8 7 6 5 4 3 2

Kidney

1st RD 2nd RD 3rd RD

Lung Heart Brain

1

Kidney retrieval

Phage recovery

and amplification

Recycle

Sequence Titer restricted

libary

Figure 2 In vivo phage display (a) Schematic representation of in vivo

phage display in the rat, so as to identify renal targeting peptides

Recov-ered and amplified phage from the kidneys 5 minutes after injection were

subjected to a total of three rounds of in vivo phage display, followed by

sequence analysis after round 2 and 3 (b) Phage recoveries over

sequen-tial rounds of phage display *indicates P < 0.05, NS, nonsignificant

IV, intravenous.

table 1 consensus sequences identified for the kidney following three

rounds of in vivo phage display

linear 7mer library n/total phage sequenced round

A total of 214 phage were sequenced.

table 2 Phage isolated from non-target organs were sequenced

following the third round of in vivo phage display

APASLYN (4.88%) APASLYN (2.27%) APASLYN (2.27%) HAAIHIS (4.88%) LPKNWSS (4.55%) VLTAGPW (7.695) YLQAPVH (4.88%) LVSQPHP (4.55%)

A total of 111 phage were sequenced.

found only in one organ, while others such as APASLYN were the encoded peptides It was clear that there were some peptides

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carried out in order to pre-saturate non-specific phage binding

sites in the liver, so as to analyze peptide-mediated targeting

with-out the confounding factor of reticulo-endothelial entrapment

of the phage particle The biodistribution of each phage

elevated phage accumulation for HIT and HTT in the kidney as

compared to the control phage, with no significant changes seen

in the liver When the recovery of either HITSLLS, HTTHREP or

control phage from the kidney was expressed as a percentage of

the liver, it was approximately tenfold higher in HITSLLS infused

animals and approximately 100-fold higher in HTTHREP infused

In order to produce targeted gene therapy vectors based on

Ad19p, we genetically modified the fiber gene from Ad19p to

accommodate peptide insertions, and inserted oligonucleotides

encoding each peptide individually into the HI loop (a site that

Alignment of the Ad5 and 19p fiber nucleotide sequences

showed that the HI loop of 19p was considerably smaller than

Ad5 and did not contain a suitable restriction site for

inser-tion of oligonucleotides encoding each targeting peptide We

used a polymerase chain reaction (PCR) strategy (see Materials

site between amino acids 331 and 332 in order to facilitate the

insertion of oligonucleotides for renal-targeting peptides (see

Materials and Methods) The resulting virus (Ad19p-Eco47)

(Figure 4b) was compared with parental Ad19p (non-modified

fiber) to confirm there were no differences in in vitro infectivity

(Figure 4c) Subsequently we cloned oligonucleotides encoding

each candidate renal targeting peptide into the Ad19p-Eco47

fiber-expressing plasmid and produced peptide-modified

those observed with non-modified fibers, as assessed by Western

Having derived all peptides by in vivo phage display, and

given that the critical aspect of targeting is expression of the

encoded transgene in vivo, we proceeded to inject rats with each

virus We killed animals 5 days after injection of each virus (and

Ad5 as a further control) to determine the extent and selectiv-ity of renal targeting Immunohistochemical analysis of kidneys

peptide-modified vectors showed readily detectable levels of transgene

in the kidneys, to a significantly higher level than that seen in

differ-ent peptide-modified vectors produced differdiffer-ent cellular distri-bution patterns in the kidneys Ad19p-HIT showed extensive

2

−3 )

NS

NS NS

10 8

10 7

10 6

10 5

10 4

10 3

10 2

10 1

3

1

NS NS NS

7 × 10 10

7 × 10 11

2 × 10 11

Control

12 10

8 6 4

2 0.17 Control HIT HTT 1.17

10.84 HIT

HTT

Kidney Phage reco Kidney

Lung Heart

Figure 3 Analysis of selected peptide-expressing phage (a)

Demon-stration of saturation kinetics of M13 phage in the liver, kidney, lung,

and heart at increasing doses *indicates P < 0.05 versus control phage

(b) Phage recoveries from kidney and liver (plaque forming units (PFU)/g

control phage to saturate non-specific binding *P < 0.05 versus control

phage (c) Phage recoveries expressed as a percentage of phage in the

liver Individual values shown above each bar NS, non significant.

Ad19p

-Eco47 HTT HIT

Ad19p parental

5

5 10 15

20 20

20 25 30 35

3 )/mg protein 40

30 35 50 kd

Ad19p Ad19p-Eco47

Ad19p-Eco47

Ad19p

c a

e d

b

HI loop

Figure 4 engineering of Ad19p fibers for targeting peptide insertion

(a) Schematic illustrating the protocol followed for producing the modi-fied vectors (refer to Materials and Methods) (b) Model of the predicted

structure of the Ad19p fiber with and without insertion of the restriction

site to allow cloning (c) In vitro comparison of Ad19p and Ad19p-Eco47

Rat glomerular endothelial cells were infected with increasing doses of either virus for 3 hours at 37 ºC They were then washed and the media was replaced Seventy-two hours after infection, cells were harvested and

β-galactosidase was measured and normalized to protein (d) Model of

the predicted structure of the Ad19p fiber with each peptide inserted into

the HI loop (e) Western blot of fiber monomer Ten µg of viral protein

was loaded, and the membrane was probed with the anti-fiber antibody 4D2 (Neomarkers, Fremont, CA) at 1:1,000 Ad, adenovirus; PCR, poly-merase chain reaction; RLU, relative light units.

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localization within the glomerulus with little or no staining in

and selective staining within the epithelial cells of the tubules

(Figure 5) Immunohistochemical analysis revealed no transgene

Further analysis of non-target organs including spleen, heart

(Figure 6a), lungs, and brain (not shown) also failed to detect

transgene expression In our previous study on Ad19p liver

targeting following intravascular injection, we used a

pre-dos-ing regimen to assess hepatocyte transduction in the absence

assessed targeting of Ad5, Ad19p-Eco47, and both

peptide-modified vectors Levels of β-galactosidase-positive hepatocytes

were: for Ad5, (83 ± 1%); for Eco47, (9 ± 1%); for

is, liver targeting of modified Ad19p vectors was not altered as

compared to Ad19p control virus, whether in the presence or

absence of Kupffer cell clearance Hence, each peptide-modified

vector produced efficient and selective transgene expression in

the kidneys following intravenous administration

Finally, we harvested organs 1 hour after injection of the same

dose of virus in order to assess early virion accumulation in the

liver and kidneys As expected, virion levels in the liver were

relatively high but essentially equivalent for Eco47,

Ad19p-HIT and Ad19p-HTT, likely as a result of profound Kupffer cell interactions However, although levels in the kidney at 1 hour after injection were far lower than in the liver, significant increases were nevertheless observed with both peptide-modified Ad19p vectors (Figure 7) This highlights the potential of the engineered Ad19p

Low power

Ad5

Ad19p-Eco47

Ad19p-HIT

Ad19p-HTT

Ad19p-HIT

Ad19p-HTT

Ad19p-Eco47

Ad5

High power

60

50

40

30

10

0

PBS Ad5 Ad19p-Eco47Ad19p-HIT Ad19p-HTT

a

b

Figure 5 Analysis of kidney targeting in vivo Eight-week old male

of each modified vector or phosphate-buffered saline (PBS) and killed

5 days later (a) Immunohistochemistry performed in kidney sections

Black staining indicates β-galactosidase activity Representative sections

are shown (n = 6 rats per group) Scale bar = 100 µm (b) Quantitative

analysis of transgene-expressing cells *P < 0.05 versus

Ad19p-Eco47-injected rats and Ad5-Ad19p-Eco47-injected rats NS, not significant Ad, adenovirus.

Liver

a

b

Spleen

Heart

90 80 70 60 50

40 30 20 10 Ad5 Ad19p-Eco47 Ad19p-HIT Ad19p-HTT

Figure 6 Analysis of non-renal tissue for reporter gene activity

virus particles per rat of each modified vector or phosphate-buffered saline and killed 5 days later Immunohistochemistry was performed on

the liver, spleen, and heart Black staining indicates β-galactosidase activ-ity Representative sections are shown (n = 6 rats per group) Scale bar =

100 µm (b) Quantitative analysis of transgene-expressing cells from liver

sections of animals infused using a pre-dose strategy Ad, adenovirus.

10,000

1,000

100

10

0.1 Kidney

Liver

Ad19p Eco47

Ad19p HIT Ad19p HTT

1

Figure 7 Assessment of early particle delivery to liver and kidney

particles per rat of each modified vector or phosphate-buffered saline and killed following perfusion at 1 hour after injection Virion quanti-fication was carried out by means of Taqman Data Analysis software (Applied Biosystems), using SYBR green DNA was extracted from the

kidney and 200 ng total DNA was amplified using LacZ primers, and the products were quantified using Taqman *P < 0.05 versus Ad19p-Eco47

Ad, adenovirus.

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system for mediating selective kidney transduction even in the

presence of rapid Kupffer cell uptake It also illustrates that

strate-gies to ablate the Kupffer cell interaction of Ad19p-based vectors

may further enhance targeting potential

dIscussIon

In this study we rationally combined in vivo phage display with

engineering of the Ad19p fiber to accommodate incorporated

peptides within the constraints of the fiber’s minimal HI loop We

showed that Ad19p-based vectors have lower coagulation factor

binding and sensitivity to this pathway when compared with Ad5,

thus contributing to the reduced hepatic tropism of the vectors

Furthermore, we developed in vivo phage display to identify renal

targeting peptides and demonstrated the incorporation of these

peptides into Ad19p pseudotyped vectors In vivo we showed

selective targeting to the kidney Of particular importance is the

finding that specific cell types in the kidney are targeted by

differ-ent peptides, because this suggests a broadly applicable approach

to targeting not only selected organs but also individual cell types

within each organ

Retargeting of Ad vectors for selective gene therapy via the

intravenous route has been widely attempted but has been

ham-pered by a number of issues including complex interplay in vivo

may contribute to the tropism of Ad and also to the host innate

immune responses Although a variety of capsid modifications

and peptide insertions have been utilized to generate convincing

data showing enhanced and/or selective gene delivery in vitro or

convinc-ingly retargeted genetically-engineered Ads following

intrave-nous injection We used in vitro cell gene transfer experiments

and SPR to assess direct FX:virus binding as well as to show that

viruses based on Ad19p showed reduced sensitivity to

coagula-tion factor binding when compared with Ad5 The binding of FIX

view of the fact that Ad5 infection has been shown to be heparin

sensitive, the KKTK motif in the fiber shaft has been suggested

mutation of the KKTK motif reduces liver transduction of Ad5

in vivo.10–12 However, an Ad5 vector with a mutated KKTK motif

binds coagulation FX as effectively as does non-modified virus,

thereby demonstrating that this is not the site of direct

to clarify and interpret the lowered binding capacity observed

with Ad19p fibers In parallel with this, we have recently shown

that many other Ad5-based vectors with fibers from subgroup

of cells in vitro In future studies, therefore, it will be critically

important to ascertain affinity constants for different

interac-tions between Ad vectors with alternative fibers

Although Ad5 viruses have been targeted using different

sites within capsid proteins, including the fiber HI loop, penton,

HI loop, because SWISS-MODEL analysis suggested that peptide

exposure at the fiber surface would be optimal Although the HI

loop of Ad19 is much smaller than that of Ad5, we were able to

document efficient virus production with each of the peptide-modified viruses created The incorporation of relatively small peptides into this site was shown not to hinder virus assembly propagation The principal thrust of our strategy was to modify a virus fiber that naturally shows poor liver tropism and combine this with peptide engineering Depending on the extent of modi-fication in the Ad19p fiber HI loop that can be tolerated without hindering virus production, it may be possible to use engineered peptides in tandem or, indeed, direct larger targeting peptides into this locale However, targeting with 7-mer peptides isolated

by phage display has been shown to be efficient for renal gene delivery It may be possible to improve targeting even further by strategies to block Kupffer cell interactions This would (poten-tially) enhance the bioavailability of peptide-modified Ad for the kidney While the receptor(s) for Ad19p remains unknown, we have shown previously that the Ad19p fiber supports the

cells (data not shown), thereby suggesting that the receptor(s) utilized by Ad19p is present on rat tissue This allows the sys-tematic analysis of vector retargeting strategies under conditions

in which the primary receptor for the parental fiber is present Ad19p can also infect human saphenous vein endothelial cells

would suggest that the primary receptor targeted by Ad19p has a similar pattern of expression in rats and humans, although fur-ther work is required to elucidate these similarities fully

To date, renal gene therapy has been achieved by applying the

using an alternative, easily accessible tissue or organ such as liver,

useful for analyzing individual transgenes in pre-clinical settings, its use is limited to secreted transgene products only The vectors

we used in our study will allow high-level transgene expression locally, but via the non-invasive intravenous route Additionally, strategies for targeting individual cells within the kidney can

be adopted, with specific peptide-modified vectors to target the glomerulus or tubular epithelium, as required Furthermore, these vectors are especially important in studies on rats, and represent unique molecular tools, given that transgenic strategies are by no means routine

In the process of our study, with all aspects taken together, we have rationally designed a new generation of adenoviral vectors that achieve efficient transgene expression in the kidneys follow-ing intravenous delivery We further demonstrate targetfollow-ing of defined cell types within this organ This has important implica-tions for the future design of genetically engineered Ad vectors

as well as for the development of renal gene therapy, an area of research hitherto hampered by a lack of suitable vectors

MAterIAls And MetHods

All in vivo work was carried out under the UK Home Office regulation

Animals (Scientific Procedures) Act 1986.

Virus preparation and purification Stocks of recombinant pseudotyped Ads expressing the modified fibers were generated by transfection of 293T cells (American Type Culture Collection, Manassas, VA) with the modi-fied plasmids followed by superinfection with a fiber-deleted Ad5 vector 44,45 Briefly, 293T cells were transfected with the appropriate fiber-expressing

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plasmid Sixteen hours later cells were superinfected with an E1, E3,

fiber-deleted rAd5 (Ad5ΔF) (β-galactosidase) at 2,000 virus particles (VP)/cell

Virus particles were purified by CsCl ultracentrifugation and dialyzed into

10 mmol/l Tris (pH 8.1), 150 mmol/l NaCl and 10% glycerol Virus particles

were quantified by protein assay against bovine serum albumin standards

according to the conversion: 1 μg protein = 4 × 10 9 VP 44 Fiber expression was

checked by sodium dodecyl sulfate polyacrylamide gel electrophoresis and

Western blot assay using monoclonal anti-fiber antibody 4D2 (Neomarkers,

Fremont, CA).

were distributed in a 96-well plate 24 hours prior to infection, incubated

with serum-free media containing 20,000 VP/cell and 1 IU/ml of either

human Factor IX or human Factor X (Haemotological Technologies,

VT), left for 3 hours at 37 °C, washed, and maintained until harvesting

Forty-eight hours after infection β-galactosidase activity was quantified

by plate assay using a Wallac Victor luminometer and recombinant

β-galactosidase as a standard A bicinchoninic acid assay on the cell lysates

was performed to determine protein concentration, and the results were

expressed as relative light units/mg of protein Similarily, for transduction

experiments, cells were distributed in a 96-well plate 24 hours prior to

infection, incubated with fresh media containing the required multiplicity

of infection (as indicated), left for 3 hours, washed, and maintained until

harvesting Seventy-two hours after infection β-galactosidase activity was

quantified.

SPR SPR experiments were carried out with a Biacore X instrument

(Biacore, Stevenage, UK) Blood coagulation FX was immobilized onto a

CM5 biosensor chip according to the manufacturer’s instructions (1,926

respiratory unit of FX was immobilized) Virus in 50 mmol/l Tris pH 7.4;

150 mmol/l NaCl; 5 mmol/l CaCl2; 0.005% Tween 20 was passed over the

chip at a flow rate of 20 μl/min Sensor chips were regenerated by injection

of 10 mmol/l HEPES pH 7.4; 150 mmol/l NaCl; 3 mmol/l EDTA; 0.005%

Tween 20.

purchased from New England Biolabs (Hertfordshire, UK) Phage display

was carried out as previously described 46 Briefly, 12–13-week-old WKY

rats (n = 3 rats/phage display round) were anesthetized (halothane/O2

mix-ture) For round 1, 2 × 10 11 PFU of PhD 7 library were infused into the

fem-oral vein, and for rounds ×2 and 3, 2 × 10 11 PFU of amplified phage from

the kidney were infused (Figure 2) Five minutes after infusion the animals

were perfused through the heart at physiological pressure (120 mm Hg),

and the organs were removed and snap frozen Phage were recovered and

titered and normalized/gram of tissue.

Peptide sequencing Peptide-encoding DNA of phage were sequenced after

rounds 2 and 3 Up to 96 individual plaques/rat were selected and

ampli-fied PCR was utilized for amplifying the region of the peptide insertion

using sense GCA ATT CCT TTA GTG GTA CC-3′ and antisense

5′-CCC TCA TAG TTA GCG TAA-3′ primers PCR products were sequenced

using BigDye  Terminator v3.1 Cycle Sequencing Kit (Applied Biosystems,

Warrington, UK) and analyzed on an ABI 377 automated sequencer.

Analysis of selected peptide-expressing phage Animals were infused with 2

× 10 11 PFU/rat of a control M13 phage lacking the LacZ α-complementation

Control phage was administered to block non-specific binding Five

min-utes after infusion 2 × 10 10 PFU of each individual phage (HITSLLS and

HTTHREP) were infused Five minutes after infusion animals were

per-fused through the heart at physiological pressure (120 mm Hg), and organs

removed and snap frozen 25 Phage in target and non-target organs were

recovered and titered and normalized/gram of tissue.

Generation of peptide-modified Ad19p fibers The Ad19p fiber

comple-mentary DNA in the plasmid pDV145 was constructed as previously

described 15 The HI loop fragment of Ad19p was excised on the Eco065I

and XbaI sites The HI loop was modified using primers to insert a unique cloning site Eco47III Using PCR, overlapping fragments were amplified

using two sets of primers The initial set of primers (i) 5′-GGA GTC GCG CAG CTT GTT GAC CAG CTC GGC-3′ and (ii) 5′-CCA ACT AAA GTC AAA TGT GAT AGA GTA TTC ACA TCC AGC GCT AGT TTC TTG

GTT AAA GG-3′ (Eco47III site underlined) amplified a 1,316-basepair

fragment containing the HI loop Similarly, a second set of primers, (iii) 5′-C CAA GAA ACT AGC GCT GGA TGT GAA TAC TCT ATC ACA TTT GAC TTT AGT TGG-3′, and (iv) 5′-GGC TGG CAA CTA GAA GGC

ACA GTC GAG GCT GAT CAG C-3′ (Eco47III site underlined) amplified

a 190-basepair fragment The two fragments were then subjected to PCR using the flanking primers 1 and 4 to produce a HI loop fragment (1,435

basepairs) with an additional Eco47III site to create a HI loop sequence

of NQETSAGCE (inserted amino acids underlined) The mutated HI

loop fragment was excised using the Eco065I and XbaI sites and ligated into pDV145 to create pDV145-Eco47III Oligonucleotides encoding the

selected peptides HTTHREP and HITSLLS were purchased from MWG

(Milton Keynes, UK) and ligated into Eco47III-digested pDV145-Eco47III

and sequenced to ensure correct orientation The plasmids pDV145-HITSLLS and pDV145-HTTHREP were produced and used for generating Ad19p-HIT and Ad19p-HTT viruses, respectively.

Peptide:fiber modelling Ad19p fiber knob protein sequences with selected insertions in the HI loop were submitted to SWISS-MODEL (http://swissmodel.expasy.org/) and modeled using ExPDB templates derived from 1uxb.pdb, 47 a crystal structure of Ad19p fiber knob in com-plex with sialic acid The bound sialic acid does not change the conforma-tion of the fiber knob 47 and was therefore ignored during modeling The models generated were visualized through Swiss-PdbViewer (http://www expasy.org/spdbv/).

In vivo virus administration and analysis of virion levels and gene delivery

In order to assess transgene expression, 8-week-old male WKY rats were infused with 3.5 × 10 11 VP each Five days after infusion, the animals were killed and the organs were removed For assessing transgene expression in the absence of Kupffer cells, a pre-dose protocol was followed 15 Briefly, 8-week-old male WKY rats were infused with 3 × 10 11 VP Ad null (no trans-gene) followed 4 hours later by 5 × 10 10 VP of peptide-modified Ad or control virus Five days after infusion, the animals were killed and the organs were removed In order to detect transgene expression, the organs were fixed

in formalin and wax-embedded Immunohistochemistry was performed

on 6 μm sections, using a rabbit polyclonal anti-β-galactosidase antibody

diluted 1/1,000 or matched rabbit IgG non-immune control (DAKO, Ely, UK) Detection was with biotinylated anti-rabbit secondary antibody, ABC kit and diaminobenzidine staining supplemented with nickel (all Vector Laboratories) Sections were counterstained with haematoxylin For the purpose of assessing particle delivery at an early time point after injection

(1 hour) animals (n = 4 per group) were perfused at physiological blood

pressure with saline, and the organs were removed and snap frozen DNA was extracted from a defined tissue mass (Qiagen, Crawley, UK) and

quan-tified using the Nanodrop ND-1000 (Wilmington, NC) A LacZ

quantifi-cation standard curve was constructed from serial dilutions of each Ad by use of SYBR green (Applied Biosystems, Warrington, UK) with 200 nmol/l sense (5′-TAC TGT CGT CGT CCC CTC AAA-3′) and antisense (5′-TAA

CAA CCC GTC GGA TTC TCC-3′) LacZ primers The total DNA was

amplified, and the products were quantified using Taqman Data Analysis software (Applied Biosystems, Warrington, UK) The following reaction conditions were in use: denaturation, 10 minutes at 95 °C; amplifica-tion, 15 seconds at 95 °C and 1 minute at 60 °C (45 cycles); dissociaamplifica-tion,

15 seconds at 95 °C, 15 seconds at 60 °C, and 15 seconds at 95 °C.

Statistical analysis Phage display was performed in groups of three animals per round The results represent mean values and SEM of the

data In vitro studies were carried out in triplicate on three independent

occasions In vivo studies were performed in groups of three animals each

Trang 8

The results represent mean values and SEM of the data Students t-test was

performed, and statistical significance was defined as P < 0.05.

AcknowledgMents

The authors thank Nicola Britton and Crawford Halliday (BHF GCRC,

University of Glasgow, UK) for technical assistance This work was

funded by the National Kidney Research Fund, the Biotechnology and

Biological Research Council, UK, and the British Heart Foundation.

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