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In 126 paraffin-embedded CRC samples, three differentially expressed proteins, identified as LASP-1, S100A9 and RhoGDI by proteomic analysis, were detected by immunohistochemical staining

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associated with the development and progression

of colorectal carcinoma

Liang Zhao1,2,*, Hui Wang3,*, Xuegang Sun4 and Yanqing Ding1

1 Department of Pathology, Nanfang Hospital, Southern Medical University, Guangzhou, China

2 Department of Pathology, School of Basic Medical Sciences, Southern Medical University, Guangzhou, China

3 Department of Medical Oncology, Affiliated Tumor Hospital of Guangzhou Medical College, China

4 School of Traditional Chinese Medicine, Southern Medical University, Guangzhou, China

Introduction

Colorectal cancer (CRC) is the third most common

cancer worldwide in both men and women, especially

in ageing populations It ranks third as the cause of

death from carcinoma, surpassed only by lung and

prostate neoplasms in men, and lung and breast

can-cers in women [1,2] As in most malignant diseases,

early diagnosis and especially detection of metastases

are of importance for patient prognosis Presently,

clinical parameters combined with histopathological

staging and grading are the most important diagnostic

and prognostic variables The evaluation of

carcino-embryonic antigen in serum has not fulfilled the prom-ise of a simple test that would offer early diagnosis of colon cancer A number of other, less well-explored, potential markers exist, but are currently not used in routine clinical diagnosis [3–5] Therefore, more exten-sive proteome tests are desirable for diagnosis, progno-sis evaluation and monitoring recurrent disease Using the technologies of two-dimensional electro-phoresis⁄ MS and immunohistochemistry in combina-tion, the aim of this study was to investigate the genesis- and metastasis-associated proteins, and to

Keywords

carcinogenesis; colorectal carcinoma;

proteomics; tumour progression;

two-dimensional electrophoresis

Correspondence

Y Ding, Department of Pathology, Nanfang

Hospital, Southern Medical University,

Guangzhou, China

Fax ⁄ Tel: +86 20 61642148

E-mail: dyqsmu@sina.com

*These authors contributed equally to this

paper

(Received 9 April 2010, revised 1 July 2010,

accepted 5 August 2010)

doi:10.1111/j.1742-4658.2010.07808.x

To better understand the mechanism underlying colorectal carcinoma (CRC) genesis or metastasis, and to search for potential markers for CRC prognosis, a comparative proteomic analysis was performed on CRC tissue Proteins were extracted from normal colorectal mucosa, non-metastatic CRC (nmCRC) and metastatic CRC (mCRC) tissue samples Protein pro-filing of each sample was performed by two-dimensional electrophoresis coupled with MALDI-TOF MS, followed by confirmation by Western blotting Thirty-one proteins were found to be differentially expressed between normal mucosa, nmCRC and mCRC tissue In 126 paraffin-embedded CRC samples, three differentially expressed proteins, identified

as LASP-1, S100A9 and RhoGDI by proteomic analysis, were detected by immunohistochemical staining to determine the clinicopathological charac-teristics of these proteins in CRC Increased expression levels of these proteins were found in CRC, especially mCRC, compared with normal mucosa The results provide the basis for searching for potential markers for CRC genesis and metastasis, and also provide clues for elucidating the mechanism of CRC progression The pattern changes identified have the potential to be used for the design of marker panels for assistance in diag-nostic and therapeutic strategies in CRC

Abbreviations

CRC, colorectal carcinoma; mCRC, metastatic colorectal carcinoma; nmCRC, non-metastatic colorectal carcinoma.

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evaluate the correlation between clinicopathological

characteristics of CRC and expression of these target

proteins, in order to better understand the mechanisms

underlying CRC progression

Results

Differential protein expression among normal

colorectal mucosa, nmCRC and mCRC tissue

A total of 1107 ± 27, 1130 ± 23 and 1135 ± 28

pro-tein spots were visualized in two-dimensional gels

using image analysis software Compared with the

nor-mal tissue control, the mCRC and nmCRC groups

had average matching rates of 70.2% and 72.6% To

identify a CRC genesis-specific protein expression

pat-tern, comparative two-dimensional analysis of normal

tissue and primary CRC tissue samples was performed

pdquest software analysis identified 22 spots that

were present in both CRC groups but not in the

nor-mal tissue With regard to determination of a CRC

metastasis-specific protein expression pattern,

compar-ative proteomic analysis identified 11 proteins

exhibit-ing consistent up-regulated expression in mCRC

compared with nmCRC Three representative gel

images for each group are shown in Fig S1 All the

protein spots of interest were successfully identified by

MALDI-TOF MS (Fig 1), and by subsequent

com-parative sequence searches in the Mascot database

(Table 1) The MSDB identification number, the theo-retical molecular mass, the theotheo-retical pI, the sequence coverage and the MASCOT score are shown in Table 1 Among them, the three proteins, identified as Rho GDP dissociation inhibitor alpha (RhoGDI), S100A9 and LIM and SH3 protein 1 (LASP-1), were found to be significantly up-regulated in tumour tissue specimens, especially in metastatic CRC Enlarged images of the three protein spots are shown in Fig 2A

Validation of the identify of differentially expressed proteins by Western blotting

To confirm and extend the two-dimensional electro-phoresis results, Western blotting was used to confirm that expression of RhoGDI, S100A9 and LASP-1 was significantly higher in mCRC tissue than in the nmCRC group, while the normal tissue had the lowest expression Equal protein loading was confirmed by parallel GAPDH immunoblotting, and signal quantifi-cation was performed by densitometric scanning A representative Western blotting result is shown in Fig 2B

Immunohistochemical analysis Expression and subcellular localization of proteins was determined by immunohistochemistry in paraffin-embedded normal colorectal mucosa and CRC tissues

A representative immunohistochemistry staining is shown in Fig 3 The rates of RhoGDI, S100A9 and LASP-1 over-expression in normal mucosa, nmCRC and mCRC tissue are shown in Table 2 Statistical analysis demonstrated that the mCRC samples had sig-nificantly higher positive over-expression rates of Rho-GDI, S100A9 and LASP-1 than the nmCRC samples (Table 2) However, there was no significant correla-tion between the three profiles (P > 0.05)

Discussion

In the present study, 31 proteins were identified as differentially expressed among normal colorectal mucosa, nmCRC and mCRC To some extent, this result is consistent with data reported by other groups [2,6–9], who listed several proteins involved in protein synthesis and folding (heat shock proteins), cell communication and signal transduction (annexin), cellular reorganization and the cytoskeleton (tropo-myosin, tubulin and actin) and toxin catabolism and water deprivation (glutathione transferase) in proteo-mic profiles of CRC cell lines and tissue However,

Fig 1 Two-dimensional gel pattern showing all the spots identified

(1–31) Table 1 gives the identities of the protein.

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there are some differences between our data and that

of other researchers, such as differential expression of

RhoGDI and LASP-1 We consider that

two-dimen-sional electrophoresis and MALDI-TOF MS-based

peptide mass fingerprinting analysis of human tissues

is more complex than for cell lines It is difficult for

a single laboratory to fully analyze extensive biological

information that are generated by two-dimensional

electrophoresis Systemic collection and analysis of

complementary data from various research groups

will assist in producing global protein profiles of

CRC Moreover, differences between races and region

distributions, as well as the various methods of tissue

collection and processing, may contribute to the

dif-ferences between laboratories The methods used in

this study, involving tissue washing and surface

scraping of tissue, are important in order to collect

pure tumour cell populations that are free of con-taminating serum proteins, red blood cells, connective tissue and necrotic tissue [10]

The 31 spots representing differentially expressed proteins among normal colorectal mucosa, nmCRC and mCRC were excised from the two-dimensional electrophoresis gels for subsequent analysis in this study All these spots were successfully identified The Western blotting results confirmed our proteomic identification of the proteins RhoGDI, S100A9 and LASP-1, showing elevated expression in the case of CRC, especially mCRC, compared with normal colo-rectal mucosa Immunohistochemical analysis revealed that over-expression of the three proteins was signifi-cantly associated with the genesis and progression of CRC The functional implications of the alterations in the levels of these proteins are discussed in detail

Table 1 The 31 proteins differentially expressed among normal colorectal mucosa, nmCRC and mCRC tissue.

Protein

index

Theoretical

Mr(kDa)⁄ pI

Summary score

Protein coverage (%) MSDB ID Protein description

Protein level (tumour ⁄ normal)

Protein level (mCRC ⁄ nmCRC)

isoform 2 variant

42 kDa fragment

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Rho GDIs (GDP dissociation inhibitors) have been

identified as key regulators of Rho family GTPases,

which are typified by their ability to prevent nucleotide

exchange and membrane association These function by

extracting Rho family GTPases from membranes and

solubilizing them in the cytosol Moreover, they interact

only with prenylated Rho proteins both in vitro and

in vivo [11,12] They also inhibit nucleotide exchange

and GTP-hydrolyzing activities on Rho proteins by

interacting with their switch regions and probably

restricting accessibility to guanine exchange factors

(GEFs) and GTPase-activating proteins (GAPs) We

used comparative proteomic analysis to identify a

mem-ber of the GDI family, namely RhoGDI, that is

up-reg-ulated in metastatic CRC, in agreement with results

obtained previously [13] Despite the initial negative

roles attributed to RhoGDI, recent evidence suggests that it may also act as a positive regulator that is neces-sary for correct targeting and regulation of Rho activi-ties by conferring cues for spatial restriction, guidance and availability to effectors [14,15] For example, Rac1 regulation of NADPH oxidase activity in neutrophils may require formation of a protein complex with RhoGDI [16–18] Similarly, Ras guanine nucleotide-releasing factor (RasGRF)-induced mitogen-activated protein kinase activation and Cdc42-mediated cellular transformation [2] may require formation of a complex between the respective GTPases and RhoGDI [19] It also appears that RhoGDI can serve as an escort to shuttle Rho GTPases to membrane-associated signalling complexes, which is crucial for coupling the GTPases

to their downstream effector proteins [20] In a

C

D

Fig 2 Identification and further validation of differentially expressed protein spots (A) Peptide mass fingerprinting of protein spots 14, 19 and 22, representing RhoGDI, S100A9 and LASP-1, respectively (B) Enlarged images of RhoGDI, S100A9 and LASP-1 in two-dimensional gels of normal colorectal mucosa, nmCRC and mCRC (C) Protein expression of RhoGDI, S100A9 and LASP-1 in normal tissue, nmCRC and mCRC determined by Western blotting There are three representative samples in each group, and the results show that expression of Rho-GDI, S100A9 and LASP-1 significantly increases in the nmCRC group GAPDH is used as an internal loading control (D) Immunosignals were quantified by densitometric scanning Protein expression in the individual tissue samples was calculated as protein expression relative to GAPDH expression Data are means ± SD from three independent experiments *P < 0.05 compared with protein expression in normal mucosa; **P < 0.05 compared with protein expression in nmCRC.

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comparative proteomic analysis of non-invasive versus

invasive ovarian tumours, RhoGDI was found to be

over-expressed in invasive human ovarian cancer

com-pared to non-invasive cancer [21] All these results

indi-cate that RhoGDI may play an important role in the

progression and metastasis of CRC

The S100A9 protein, formerly called calgranulin B,

MRP14 or LI heavy chain, is a protein of about

13 kDa that can occur in three different isoforms

depending on its level of phosphorylation [22] This

protein is found predominantly in the cytosol, but can

also be expressed on the cell surface or even secreted

into the extracellular environment The best

character-ized intracellular function proposed for S100A9 is that

of inhibition of casein kinase II, contributing to

regulation of normal cellular transcription and

transla-tion The possible extracellular functions assigned to

S100A9 include chemotactic activity on the one hand

and cytotoxic⁄ cytostatic activities against bacteria,

fungi and tumour cells on the other hand [23]

Previous studies have reported that S100A8 and

S100A9 are frequently co-expressed, and their expres-sion appears to be coordinately regulated [24,25] Dif-ferential expression of S100A8 and S100A9 has been shown to contribute to the development and progres-sion of various types of cancer For example, S100A8 and S100A9 are over-expressed in pancreatic adenocar-cinoma [26], bladder cancers [27] and breast cancers [28] S100A9 expression is linked to de-differentiation

of thyroid carcinoma [29] Several studies have attempted to correlate the level of expression of S100A8 and S100A9 with the degree of non-inva-sive⁄ invasive behaviour Non-invasive MCF-7 breast cancer cells do not express S100A9 S100A9 expression

in MCF-7 is induced by the cytokine oncostatin m through the STAT3 signalling cascade [30] However, both S100 proteins are highly expressed in non-inva-sive MDA-MB-468 cells [31] The invanon-inva-sive breast can-cer cell line MDA-MB-231 shows only a low transcript level of S100A9 [32], but S100A9 is over-expressed in invasive ductal carcinoma of the breast [1,33] S100A8 and S100A9 have been suggested to represent novel

Fig 3 Immunohistochemical staining of

RhoGDI, S100A9 and LASP-1 in normal

colorectal mucosa, nmCRC and mCRC.

Immunoreactivity to RhoGDI, S100A9 and

LASP-1 staining was localized to the

cytoplasm region of benign and malignant

epithelial cells.

Table 2 Over-expression of RhoGDI, S100A9 and LASP-1 proteins in normal mucosa, nmCRC and mCRC.

Group

a

a The statistical analyses were performed among normal mucosa, nmCRC and mCRC groups.

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diagnostic markers when measured in the serum of

patients with prostate cancer and benign prostate

hyperplasia [34] In line with these observations, we

detected up-regulated expression of S100A9 proteins in

CRC tissues, especially in mCRC, indicating its

possi-ble role in the development and progression of CRC

LASP-1 was initially identify from a cDNA library

of metastatic axillary lymph nodes of breast cancer

patients, and the gene was mapped to human

chromo-some 17q21 [35,36] The exact functions of LASP-1 are

still not well known; however, its expression is

local-ized to multiple sites of dynamic actin assembly, such

as focal contacts, focal adhesions, lamellipodia

mem-brane ruffles and pseudopodia [30,35,37–39] It has

been reported that LASP-1 is over-expressed in

meta-static breast cancer, participating in migration of these

cancer cells Furthermore, silencing of LASP-1 in

met-astatic breast cancer cell lines resulted in strong

inhibi-tion of cell proliferainhibi-tion as well as migrainhibi-tion, and led

to a reduction of zyxin at the focal contacts [30,40]

Interestingly, a recent study also demonstrated that

LASP-1 is over-expressed in ovarian cancer tissues and

metastatic ovarian cancer cell lines [41] In vitro

silenc-ing of the gene encodsilenc-ing LASP-1 reduced cell

prolifer-ation and migrprolifer-ation and severely affected zyxin

localization [41] These results indicate that LASP-1

may play an important role in the progression and

metastasis of CRC

In summary, the techniques of proteomic analysis

provide a dramatic means of screening for genesis- and

metastasis-associated proteins in CRC The results

sug-gest that RhoGDI, S100A9 and LASP-1 may play an

important role in the development and progression of

CRC Further functional and clinical analysis of the

proteins is necessary to elucidate their precise role in

the process of CRC and the formation of metastases

Experimental procedures

Tumour samples

All cases were selected from the Nanfang Hospital tumour

tissue bank In total, 150 patients were involved in the

study In each case, a diagnosis of primary CRC had been made, and the patients had undergone elective surgery for CRC, in Nanfang Hospital, between 2001 and 2004 The Nanfang Hospital tumour tissue bank is linked to a com-prehensive set of clinicopathological data Clinical data for all the samples used for two-dimensional electrophoresis and immunohistochemical study are shown in Table 3 The tumour samples were submitted to the Department of Pathology, Nanfang Hospital, Southern Medical Univer-sity, for pathological diagnosis The tumour specimens were fixed in formalin, representative blocks were embedded in wax, and sections were stained with haematoxylin and eosin Permission for this study was obtained from the Eth-ics Committee of Southern Medical University The informed consent with a uniform format was designed by the Ethics Committee and signed by the patients involved

in the study before the trial All the patients understood the trial’s purpose and procedures

Proteomics Proteomics analysis, including two-dimensional gel electro-phoresis, gel visualization and assessment, and mass spec-trometry, was performed as previously described [42] Proteins were extracted from normal colorectal mucosa (n = 12), non-metastatic CRC (nmCRC) (n = 12) and metastatic CRC (mCRC) (n = 12) tissue samples Tissue samples (50–100 mg) were crushed in liquid nitrogen, and lysed in 1 mL lysis buffer consisting of 7 m urea, 2 m thio-urea, 4% Chaps, 65 mm dithiothreitol and 2% pharmalyte (pH3-10; GE Healthcare, Piscataway, NJ, USA) by sonica-tion on ice The lysates were cleared by centrifugasonica-tion at

12 000 g for 1 h at 4C The protein concentration of the supernatants was determined by the modified Bradford method [43], and aliquots of the protein samples were stored at)80 C Prior to two-dimensional electrophoresis, the protein samples were purified using a 2D Clean-Up kit (GE Healthcare) according to the manufacturer’s instruc-tions Differentially expressed proteins were identified using two-dimensional gel electrophoresis and mass spectrome-try Two-dimensional gel electrophoresis was performed using Immoboline strips (pI range, 3–10; GE Healthcare, Piscataway, NJ, USA), with proteins being separated according to charge, and subsequently molecular weight The gels were then stained with silver in order to visualize

Table 3 CRC tissue samples used in the study.

Samples for two-dimensional electrophoresis Samples for immunohistochemisty

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proteins, and scanned using a Power-Look 1100 imaging

scanner (Umax, Dallas, TX, USA) The pdquest 7.1

soft-ware package (Bio-Rad, Hercules, CA, USA) was used for

image analysis, including background abstraction, spot

intensity calibration, spot detection and matching The

intensity of each spot was quantified by calculation of spot

volume after normalization of the gel image Each

experi-ment was performed in triplicate, and the paired Student’s

ttest was used to evaluate the mean change in protein

abundance corresponding to each target spot across the

gels The protein spots of interest were cut from the gels

Proteins were digested with trypsin, and peptide mass

mapping was performed by MALDI-TOF MS using an

ABI Voyager DE-STR mass spectrometer (Applied

Biosys-tems, Foster City, CA, USA) Protein identification using

peptide mass fingerprinting was performed using the

MAS-COT search engine (http://www.matrixscience.com/, Matrix

Science Ltd, London, UK) against the MSDB protein

database (http://www.proteomics.leeds.ac.uk/bioinf/msdb

html) The database search was restricted to human

pro-teins, with no constraints on either the molecular weight

or the isoelectric point of the protein The errors in

pep-tide mass were in the range of 25 ppm One missed tryptic

cleavage site per peptide was allowed during the search

Proteins matching more than four peptides and with a

MASCOT score higher than 63 were considered significant

(P < 0.05) Carboamidomethylation of cysteine was used

as the static modification and oxidation of methionine as

the differential modification The protein identification

results were filtered using peakerazor software

(Light-house Data, Odense, Denmark)

Western blot analysis

Samples from the different population were selected for

Western blot validation Sample preparation for

immuno-blotting was performed as previously described [44] Briefly,

proteins were obtained from tissue samples as described

above The protein concentration was determined using the

modified Bradford method [43] Equal amounts of proteins

were separated electrophoretically on 12% SDS⁄

polyacryl-amide gels, and transferred onto polyvinylidene difluoride

membranes (PVDF) (Amersham Pharmacia Biotech,

Piscat-away, NJ, USA) The membrane was probed using rabbit

anti-RhoGDI IgG (1 : 1000; Cell Signalling Technology,

Danvers, MA, USA), mouse anti-S100A9 IgG (1 : 1000;

Abcam, Cambridge, UK) and mouse anti-LASP-1 IgG

(1 : 2000; Chemicon, Temecula, CA, USA) Expression of

proteins was determined using horseradish

peroxidase-conjugated anti-rabbit IgG (1 : 20 000; Jingmei Biotech,

Shanghai, China) and enhanced chemiluminescence (ECL)

(Pierce, Rockford, IL, USA) The immunoreactive bands

were visualized on a Kodak 2000M camera system (Eastman

Kodak, Rochester, NY, USA) according to the

manufac-turer’s instructions An anti-GAPDH goat polyclonal IgG

(1 : 500; Santa Cruz Biotechnology, Santa Cruz, CA, USA) was used to confirm equal loading The experiments were repeated three times

Immunohistochemistry Immunohistochemistry was performed to study altered tein expression in 126 human CRC tissue samples The pro-cedures used were similar to previously described methods [44] Briefly, 4 lm sections mounted on aminopropylethox-ysilane slides and pre-treated for immunohistochemistry were de-waxed using xylene, and rehydrated through a graded series of ethanol and deionized water An antigen retrieval step was performed Before staining for immuno-histochemistry, the sections were incubated in a 750 W microwave oven for 15 min in 10 mm buffered citrate, pH 6.0, to complete antigen unmasking The classical avidin– biotin peroxidase complex procedure was used for immuno-histochemistry In the avidin–biotin peroxidase complex system, endogenous peroxidase was quenched by incubation

of the sections in 0.1% sodium azide with 0.3% hydrogen peroxide for 30 min at room temperature Non-specific binding was blocked by incubation with non-immune serum (1% bovine serum albumin for 15 min at room temperature) The sections were incubated with primary anti-RhoGDI (1 : 50), mouse anti-S100A9 (1 : 100) and anti-LASP-1 (1 : 500) antibodies overnight at 4C The following con-trols were performed: (a) omission of the primary antibody, and (b) substitution of the primary antiserum with non-immune serum diluted 1 : 500 in blocking buffer

No immunostaining was observed after any of the control procedures Biotinylated secondary goat rabbit anti-bodies (MaiXin, Fuzhou, China) and subsequently a horse-radish peroxidase–streptavidin complex (MaiXin) were applied for 15 min each Peroxidase activity was developed

by use of a filtered solution of 5 mg 3,3-diaminobenzideine tetrahydrochloride (dissolved in 10 mL 0.05 m Tris buffer,

pH 7.6) and 0.03% H2O2 Mayer’s haematoxylin was used for nuclear counterstaining The sections were mounted using a synthetic medium

Evaluation of immunohistochemical staining Two observers independently reviewed and assessed the cel-lular localization and intensity of immunostaining in each section Staining for proteins in tumour cells was scored semi-quantitatively using a quality control system The pro-portion of cells expressing the proteins varied from 0% to 100%, and the intensity of staining varied from weak to strong Scores representing the percentage of tumour cells stained positive were as follows: 0% (absent), 1–5% (spo-radic), 6–25% (local), 26–50% (occasional), 51–75% (majority) and 76–100% (large majority) The intensity of tumour cell staining was scored as 0 (no staining), 1 (weak staining, light yellow), 2 (moderate staining, yellowish

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brown) and 3 (strong staining, brown) Using this method

of assessment as mentioned above, we evaluated the

expres-sion of proteins in benign colorectal mucosa and malignant

lesions as described previously [45] Cut-off values were

chosen on the basis of a measure of heterogeneity An

optimal cut-off value was identified An intensity score of

‡ 2 with at least 50% of malignant cells showing positive

staining was used to classify tumours with high expression

(or over-expression), and < 50% of malignant cells with

staining or an intensity score < 2 identified tumours with

low expression The small number of discrepancies (< 5%)

were resolved by re-evaluation

Statistical analysis

All statistical analyses were performed using the spss 12.0

statistical software package (SPSS, Chicago, IL, USA) The

pdquest 7.1 software package (Bio-Rad) was used for

image analysis, and a paired Student’s t test was used to

evaluate the mean change in protein abundance

corre-sponding to each target spot across the gels For Western

blot analysis, expression of differential protein between two

groups was compared using a paired Student’s t test For

immunohistochemistry analysis, the significance of

correla-tion between the protein expression and clinicopathological

factors was determined using Pearson’s chi-square test A P

value < 0.05 was considered statistically significant in all

cases

Acknowledgements

This work was supported by the Key Science and

Technology Research Program of Guangdong

Prov-ince (grant number 2003A308401), the National

Natu-ral Science Foundation of China (grant number

30901792) and the Presidential Foundation of the

School of Basic Medical Sciences of Southern Medical

University (grant number JC0802)

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Supporting information

The following supplementary material is available: Fig S1 Three representative gel images of normal tissue, mCRC and nmCRC

This supplementary material can be found in the online version of this article

Please note: As a service to our authors and readers, this journal provides supporting information supplied

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