FINAL REPORT 

Sensitization Screen using the Direct Peptide Reactivity Assay 

(DPRA) 

Cyprotex Study Number: 

9320-101114 

Sponsor: 

International Flavors and Fragrances, Inc. 

800 Rose Lane 

Union Beach, NJ 07735 

Testing Facility: 

Cyprotex, LLC. 

4717 Campus Dr. 

Kalamazoo Ml 49008 
Study #: 9320-101 11 4 

Table of Contents 

Signatures ............................................................................................................................................... 3 

Contributing Personnel .......................................................................................................................... 4 

Study Dates ............................................................................................................................ ................. 4 

Executive Summary ................................................................................................................................ 5 

1. Sponsor .................................................................................... ......... ... ................................... 6 

2. Testing Facility ...................................................................................................................................................... 6 

3. Materials & Methods ............................................................................................................................................. 6 

a. Test & Reference Articles ........................................................................................................................... 6 

b . Justification of Test System ....................................................................................................................... 6 

c. Preparation of Samples ................................................................................................................................... 7 

d. Evaluation of Test Articles in the Assay .................................................................................................. 7 

e. Test Validity an Acceptance Criteria ............................................................................................................. 7 

4. Results & Discussion ........................................................................................................................................... 8 

5. References ................................................................................................................................................................. 9 

6. Appendix A: Summary LC/MS/MS data for Lysine peptide .............................................................................. 9 

7. Appendix B: Summary LC/MS/MS data for Cysteine peptide ......................................................................... 12 

Page 2 of 15 Confidential Document 
Prepared by: 

Donald Keller, MS 

Study Director 

Signatures 

Page 3 of 15 

Study#: 9320-101114 

Confidential Document 
Study#: 9320-101114 

Contributing Personnel 

The following scientists and supervisory personnel were involved in the conduct of this study: 

Donald Keller, MS, Study Director 

Briana Franz, BS, Director of Laboratory Operations 

Lisa Blakeman, BS, Associate Scientist 

Gregory Cavey, BS, Principle Investigators, Launch Ml Lab 

Francisca Wong , BS, Research Scientist, Launch Ml Lab 

Study Dates 

Experimental Start Date: April 8, 2014 

Experimental Termination Date: April 29, 2014 

Page 4 of 15 Confidential Document 
Study#: 9320-101114 

Executive Summary 

The purpose of this study was to screen test articles for their potential to act as chemical sensitizers 

using Direct Peptide Reactivity Assay (DPRA}, a test used to assay reactivity of test articles with small 

peptides. A summary of the results for the 8 test articles are given below. 

Table 1. Results of DPRA for 8 test articles with controls 

Compound Cvs Oep Lvs Deo Avf!.. Dep Classification 

Benzoic Acid -6.7 -1.1 -3.9 Minimal Reactivity 

p-Benzoquinone 98.3 97.9 98.1 High Reactivity 

TM05-0293 -10.4 2.6 -3.9 Minimal Reactivity 

TM08-0338 -7.6 20.7 6.6 Low Reactivity 

TM09-0035 -14.5 12.0 -1.3 Minimal Reactivity 

TM09-0536 22.9 1.8 12.4 Low Reactivity 

TM10-0210 70.7 5.7 38.2 Moderate Reactivity 

TMl0-0367 6.3 1.7 4.0 Minimal Reactivity 

TM11-0078 77.1 6.9 42.0 Moderate Reactivity 

TM11-0230 5.8 -4.5 0.6 Minimal Reactivity 

For this test: low, moderate, and high reactivity were considered positive; while minimal reactivity was 

considered negative. The data were based on the classification tree described by Gerberick, 2007 

(Figure 1 below). 

Figure 1: DPRA Classification Tree 

0:(29115/20/17) 

t:s.:~ . 

>--~SIW~ Avg Score< 22 62~ - ~ Avg Score > 22.62% 

/ ""'-.. 

---- > ----..__ / Test ' '-- / Tell \ 

Avg Score< 6.376% 

(29/11/~/0) (0 /1~ 

Avg Score > 6.376°k - ~ 

1. Sponsor 

Minimal Reactivity 

(2615/1/0) 

Avg Score < 42.47% vg Score > 42.47°k 

~--~----~ I I 

Low Reactivity 

(3 16 12 1 0) 

Moderate Reacttvity 

(0 / 1 / 6 / 3} 

DPRA classification tree from Gerberick et al., 2007. 

Page 5 of 15 

High Reactivity 

(0 /3/11/14} 

Confidential Document 
International Flavor and Fragrances, Inc. 

800 Rose Lane 

Union Beach, NJ 07735 

2. Testing Facility 

Cyprotex US, LLC 

4717 Campus Drive 

Kalamazoo, Ml 49008 

Performing Laboratory 

Launch Ml Lab 

4717 Campus Drive, Kalamazoo Ml 49008 

Study#: 9320-101114 

Phase Performed: LC/MS/MS analysis of peptide/compound reactions 

3. Materials & Methods 

a. Test & Reference Articles 

Com~ound Name Lot Storage Condition Molecular Weight Notes/Purit~ 

Number 

TM 08-0338 RDJL2759 Rm. Temp in dark 194.31 soluble in DMS0/100% 

TM 11 -0078 RDNG22329 Refrig. In dark 182.13 soluble in DMS0/1 00%1 

TM 10-0210 RDR07895 Refrig. In dark 194.17 soluble in DMS0/1 00% 

TM 10-0367 RDNG22339 2-10 C, in dark 184.18 soluble in DMS0/1 00% 

TM 09-0536 RDIA5595 Rm. Temp in dark 192.3 soluble in DMS0/1 00% 

TM 11-0230 RDBB16179 refrigerated and 148 soluble in DMS0/1 00%1 protected from light 

TM 05-0293 RDRW23746 Rm. Temp in dark 156.2 soluble in DMS0/1 00% 

TM 09-0035 RDRW23748 Rm. Temp in dark 200.2 soluble in DMS0/1 00%1 

p-Benzoquinone MKBG6486V 2-10 C, in dark 108.09 soluble in DMS0/98% 

Benzoic acid MKBG6929V 

MKBG9391V Rm. Temp 122 12 soluble in DMS0/99.5% 

1 

Purity not ~rovided by Sponsor therefore assumed 100% 

b. Justification of Test System 

Direct Peptide Reactivity Assay: DPRA was developed by Frank Gerberick and colleagues (2004) 

and was further refined in 2007 (Gerberick et al., 2007). In this assay, the test articles were 

incubated concurrently in two separate buffers, one with cysteine (Ac-RFAACAA-COOH) and one 

with lysine (Ac-RFAAKAA-COOH). Reactive chemicals bind one or both of the peptides thereby 

reducing their free concentration levels. The disappearance of each peptide was measured by 

LC/MS/MS. This method did not require any biological material such as enzymes in order for this 

reaction to take place. It is important to note that the cysteine peptide captures soft electrophiles, 

while the lysine peptide captures hard electrophiles. It is also important to note that the standard 

glutathione reactivity assay commonly used to screen for skin sensitizers captures only soft 

electrophiles, as glutathione is a soft nucleophile. This makes the DPRA assay a good choice to 

screen for reactive chemicals which is associated with allergic contact dermatitis. 

Page 6 of 15 Confidential Document 
6-cyprotex 

Study#: 9320-101114 

c. Preparation of Samples 

Test Article Stocks: Test articles were received at Cyprotex and stored according 

A stock solution of each 

to section 3.a. 

OM SO: acetonitrile to yield a 

test article was prepared by adding an appropriate amount of 1:1 

final concentration of 100 mM. 

Reference materials: Control stocks were prepared in 1:1 DMSO:acetonitrile 

concentration of 100 mM

to yield a final 

. 

with 

Peptides

Peptide 

: A stock 

Reaction/Storage 

solution of the lysine peptide ( 125 mM) was prepared by diluting the peptide 

prepared by diluting 

buffer, and a stock solution of cysteine peptide (125 mM) was 

-aooc desiccated

the peptide with dimethylformamide. Peptides were stored at approximately 

. Peptides were from LifeTein LLC (South Plainfield, NJ). 

d. Evaluation of Test Articles in the Assay 

DPRA: DPRA was run according 

were prepared at 100 mM 

to Cyprotex SOP-2078. Test articles and reference articles 

prepared at 125 mM 

in 1:1 DMSO:acetonitrile as stated above. The cysteine peptide was 

in DMF (dimethylformamide) 

mM in lysine Peptide Reaction/Storage 

and the lysine peptide was prepared at 125 

test peptide to test article 

buffer. The reaction mix for cysteine peptide had a 1:1 0 

peptide had a 1

ratio (0.5 mM cysteine to 5 mM test article). The reaction mix for lysine 

:50 peptide to test article ratio (0.5 mM lysine to 25 mM test article). 

Reactions for each test article were performed 

performed using 

in triplicate and LC/MS/MS analysis was 

sample reactions 

three injections for each reaction. A vehicle control was run in parallel with 

negative controls 

to 

were 

determine percent depletion relative to vehicle controls (N=3). Positive and 

reactions, peptides were 

included (N=3). In addition to making up test and reference article 

sealed and reactions were 

serially diluted in buffer to produce standard curves. Test plates were 

run for 24 hr at room temperature in the dark. 

2996 

Samples 

Photodiode 

were assessed 

Array detector 

via LC/MS/MS using a Waters Alliance 2795 HPLC equipped with a 

and a Micromass Quattro Premier mass spectrometer

sample was injected 

. Each 

in triplicate according to Cyprotex SOP. 

After determination of peptide remaining 

controls was calculated 

in the analysis, percent depletion relative to vehicle 

reported as percent depletion 

relative to time zero or no test article samples. Peptide reactivity was 

(1-(test compound area/ vehicle 

and was calculated using the following formula: % Dep Peptide = 

control area) x 100. 

e. Test Validity an Acceptance Criteria 

included 

For data 

means 

generated 

of 

at Cyprotex, basic statistical analysis was performed on the data, which 

varied from the mean 

replicates

by more 

, standard deviations, and CV%. Values within a dose group that 

calculation. 

than .!,2 standard deviations were omitted from the final mean 

The results of each assay was evaluated and compared 

were expressed as percent 

to reference controls. DPRA results 

determine reactivity classification

of control. All data were placed in a final datasheet and used to 

acceptable runs

. Reference controls were within Cyprotex criteria for all 

. 

Page 7 of 15 Confidential Document 
Study#: 9320-101114 

4. Results & Discussion 

DPRA was performed to analyze for sensitization potential. The results for the test articles are 

shown below: 

Compound Cvs Dep Lvs Dep Avf!. Dep Classification 

Benzoic Acid -6.7 -1.1 -3.9 Minimal Reactivity 

pBenzoquinone 98.3 97.9 98.1 High Reactivity 

TM05-0293 -10.4 2.6 -3.9 Minimal Reactivity 

TM08-0338 -7.6 20.7 6.6 Low Reactivity 

TM09-0035 -14.5 12.0 -1.3 Minimal Reactivity 

TM09-0536 22.9 1.8 12.4 Low Reactivity 

TM10-0210 70.7 5.7 38.2 Moderate Reactivity 

TM10-0367 6.3 1.7 4.0 Minimal Reactivity 

TM11-0078 77.1 6.9 42.0 Moderate Reactivity 

TM11-0230 5.8 -4.5 0.6 Minimal Reactivity 

Benzoic acid was minimally reactive while p-Benzoquinone was highly reactive with both peptides as 

expected. Test articles TM10-0210 and TM11-0078 were reactive with the cysteine peptide and as a 

result were ranked as moderately reactive overall. It should be noted that the cutoff for highly 

reactivity is 42.4 7% so TM 11-0078 is just below this cutoff. The remaining test articles showed low 

to minimal reactivity overall and varied in terms of which peptide was reacted with more strongly. 

For this test, low, moderate, and high reactivity were considered positive, while minimal reactivity 

was considered negative. 

Table 1: Cysteine data summarized 

Avg 

Cysteine Peptide Area SO area %CV I % Dep 

BenzoicAcid 57460.6 3099.7 5.4 -6.7 

Para benzoquinone 903.4 93.3 10.3 98.3 

TM05-0293 59442.6 4187.9 7.0 -10.4 

TM08-0338 57936.7 7683.7 13.3 -7.6 

TM09-0035 61698.5 5053.7 8.2 -14.5 

TM09-0536 41544.3 4207.1 10.1 22.9 

TM10-0210 15769.9 2929.6 18.6 70.7 

TM10-0367 50449.4 6758.5 13.4 6.3 

TM11-0078 12340.7 1351.0 10.9 77.1 

TM11-0230 50752.0 2983.6 5.9 5.8 

Vehicle-ACN-DMSO 53861.9 5381.3 10.0 0.0 

Table 2: Lysine data summarized 

Page 8 of 15 Confidential Document 
Study#: 9320-101114 

Lysine peptide Avg Area SD area %CV % Dep 

BenzoicAcid 270521.6 26814.7 9.9 -1.1 

Para benzoquinone 5606.8 1786.9 31.9 97.9 

TM05-0293 260610.9 32836.5 12.6 2.6 

TM08-0338 212111.2 14263.6 6.7 20.7 

TM09-0035 235415.2 17730.1 7.5 12.0 

TM09-0536 262604.3 66508.3 25.3 1.8 

TM10-0210 252160.6 27173.0 10.8 5.7 

TM10-0367 263028.2 34965.3 13.3 1.7 

TMll-0078 249149.0 15785.0 6.3 6.9 

TMll-0230 279556.6 29572.9 10.6 -4.5 

Vehicle-ACN-DMSO 267534.7 36371.2 13.6 0.0 

5. References 

Gerberick 

Development 

GF, Vassallo JD, Bailey RE, Chaney JG, Morall SW, Lepoittevin JP (2004). 

of a Peptide Reactivity Assay for Screening Contact Allergens. Toxicological 

Sciences 81 , 332-343. 

Chemical 

Gerberick GF, Vassallo JD, Foertsch LM, Price 88, Lepoittevin JP (2007). Quantificaton of 

Peptide Reactivity for Screening Contact Allergens: A Classification Tree Model 

Approach. Toxicological Sciences 97 (2), 417-427. 

6. Appendix A: Summary LC/MS/MS data for Lysine peptide 

lnj. 

Name RT Response Type Vol uM 

BenzoicAcid 040914 Lys 1A 2.22 266208.5 Analyte 3 524.9781 

BenzoicAcid 040914 Lys 1B 2.23 306049.6 Analyte 3 605.8758 

BenzoicAcid 040914 Lys 1C 2.23 235803.9 Analyte 3 463.6611 

BenzoicAcid 040914 Lys 2A 2.22 272406.8 Analyte 3 537.5226 

BenzoicAcid 040914 Lys 2B 2.23 305442.9 Analyte 3 604.6393 

BenzoicAcid 040914 Lys 2C 2.23 261621.6 Analyte 3 515.7045 

BenzoicAcid 040914 Lys 3A 2.22 257355.7 Analyte 3 507.0875 

BenzoicAcid 040914 Lys 3B 2.22 294290.8 Analyte 3 581.9339 

BenzoicAcid 040914 Lys 3C 2.22 235514.8 Analyte 3 463.0796 

Parabenzoquinone 040914 Lys 1A 2.23 3469.02 Analyte 3 6.4472 

Parabenzoquinone 040914 Lys 1B 2.23 5185.1 Analyte 3 9.7542 

Parabenzoquinone 040914 Lys 1C 2.23 6907.44 Analyte 3 13.0743 

Parabenzoquinone 040914 Lys 2A 2.22 3520.45 Analyte 3 6.5463 

Page 9 of 15 Confidential Document 
Study#: 9320-101114 

Parabenzoquinone 040914 Lys 2B 2.23 7513.36 Analyte 3 14.2426 

Parabenzoquinone 040914 Lys 2C 2.23 6296.61 Analyte 3 11.8967 

Parabenzoquinone 040914 Lys 3A 2.23 5575.09 Analyte 3 10.5059 

Parabenzoquinone 040914 Lys 3B 2.22 8270.1 Analyte 3 15.7018 

Parabenzoquinone 040914 Lys 3C 2.23 3723.92 Analyte 3 6.9383 

TM05-0293 040914 Lys 1A 2.22 263283.5 Analyte 3 519.0636 

TM05-0293 040914 Lys 1B 2.22 259127.8 Analyte 3 510.6662 

TM05-0293 040914 Lys 1C 2.23 240411.2 Analyte 3 472.9295 

TM05-0293 040914 Lys 2A 2.22 242184.9 Analyte 3 476.4999 

TM05-0293 040914 Lys 2B 2.22 312666.1 Analyte 3 619.372 

TM05-0293 040914 Lys 2C 2.24 241424.8 Analyte 3 474.9697 

TM05-0293 040914 Lys 3A 2.22 292759.1 Analyte 3 578.8191 

TM05-0293 040914 Lys 3B 2.24 287913.6 Analyte 3 568.9724 

TM05-0293 040914 Lys 3C 2.24 205727.3 Analyte 3 403.3561 

TM08-0338 040914 Lys 1A 2.23 238291.7 Analyte 3 468.6647 

TM08-0338 040914 Lys 1B 2.22 224764.3 Analyte 3 441.486 

TM08-0338 040914 Lys 1C 2.24 192956.6 Analyte 3 377.8543 

TM08-0338 040914 Lys 2A 2.22 215796.2 Analyte 3 423.5062 

TM08-0338 040914 Lys 2B 2.23 210200.8 Analyte 3 412.3038 

TM08-0338 040914 Lys 2C 2.23 197324.9 Analyte 3 386.5704 

TM08-0338 040914 Lys 3A 2.23 218452.6 Analyte 3 428.8286 

TM08-0338 040914 Lys 3B 2.22 210826 Analyte 3 413.5549 

TM08-0338 040914 Lys 3C 2.24 200387.6 Analyte 3 392.6857 

TM09-0035 040914 Lys 1A 2.22 238628.2 Analyte 3 469.3416 

TM09-0035 040914 Lys 1B 2.23 257224.5 Analyte 3 506.8224 

TM09-0035 040914 Lys 1C 2.23 241609 Analyte 3 475.3405 

TM09-0035 040914 Lys 2A 2.22 253406.1 Analyte 3 499.1156 

TM09-0035 040914 Lys 2B 2.23 248676.2 Analyte 3 489.5767 

TM09-0035 040914 Lys 2C 2.22 237212.6 Analyte 3 466.494 

TM09-0035 040914 Lys 3A 2.23 205849.6 Analyte 3 403.6007 

TM09-0035 040914 Lys 38 2.23 220471.4 Analyte 3 432.8755 

TM09-0035 040914 Lys 3C 2.23 215658.7 Analyte 3 423.2309 

TM09-0536 040914 Lys 1A 2.23 310296.6 Analyte 3 614.5367 

TM09-0536 040914 Lys 1B 2.23 312523.1 Analyte 3 619.0802 

TM09-0536 040914 Lys 1C 2.24 178842.7 Analyte 3 349.7418 

TM09-0536 040914 Lys 2A 2.22 291006.7 Analyte 3 575.257 

TM09-0536 040914 Lys 2B 2.22 310953.7 Analyte 3 615.8775 

TM09-0536 040914 Lys 2C 2.23 167661 Analyte 3 327.5224 

TM09-0536 040914 Lys 3A 2.23 304474.6 Analyte 3 602.6657 

TM09-0536 040914 Lys 3B 2.24 310879.4 Analyte 3 615.7258 

Page 10 of 15 Confidential Document 
Study #: 9320-101114 

TM09-0536 040914 Lys 3C 2.23 176801 Analyte 3 345.6811 I TM10-0210 040914 Lys 1A 2.23 243666.5 Analyte 3 479.4831 ! 

TM10-0210 040914 Lys 1B 2.23 284724.3 Analyte 3 562.4962 

TMl0-0210 040914 Lys 1C 2.23 260436.5 Analyte 3 513.31 

TM10-0210 040914 Lys 2A 2.22 228315.1 Analyte 3 448.6132 

TM10-0210 040914 Lys 2B 2.23 271798.3 Analyte 3 536.2904 

TM10-0210 040914 Lys 2C 2.22 252806.3 Analyte 3 497.9054 

TM10-0210 040914 Lys 3A 2.22 195044.3 Analyte 3 382.0191 

TMl0-0210 040914 Lys 3B 2.23 272946.7 Analyte 3 538.6159 

TM10-0210 040914 Lys 3C 2.23 259707 Analyte 3 511.8362 

TM10-0367 040914 Lys 1A 2.23 216953.2 Analyte 3 425.824 

TM10-0367 040914 Lys 1B 2.22 284468.7 Analyte 3 561.9773 

TM10-0367 040914 Lys 1C 2.23 295581.8 Analyte 3 584.5596 

TMl0-0367 040914 Lys 2A 2.24 204033.5 Analyte 3 399.9702 

TM10-0367 040914 Lys 2B 2.23 284704.9 Analyte 3 562.4568 

TM10-0367 040914 Lys 2C 2.23 294904.5 Analyte 3 583.1819 

TMl0-0367 040914 Lys 3A 2.23 239301.4 Analyte 3 470.6961 

TM10-0367 040914 Lys 3B 2.23 259812 Analyte 3 512.0483 

TM10-0367 040914 Lys 3C 2.24 287494.4 Analyte 3 568.1209 

TM11-0078 040914 Lys 1A 2.22 271425.9 Analyte 3 535.5362 

TM11-0078 040914 Lys 1B 2.23 253797 Analyte 3 499.9042 

TM11-0078 040914 Lys 1C 2.23 251718.2 Analyte 3 495.7106 

TM11-0078 040914 Lys 2A 2.23 247741.4 Analyte 3 487.6926 

TM11-0078 040914 Lys 2B 2.22 260233.6 Analyte 3 512.9 

TM11-0078 040914 Lys 2C 2.23 237834.8 Analyte 3 467.7456 

TM11-0078_040914 Lys 3A 2.23 214656.2 Analyte 3 421.2228 

TM11-0078 040914 Lys 3B 2.22 251011.2 Analyte 3 494.2847 

TM11-0078 040914 Lys 3C 2.24 253922.3 Analyte 3 500.1571 

TM11-0230 040914 Lys 1A 2.24 264924.1 Analyte 3 522.3805 

TM11-0230 040914 Lys 1B 2.23 327290.4 Analyte 3 649.2652 

TMll-0230 040914 Lys 1C 2.22 250085.5 Analyte 3 492.418 

TMll-0230 040914 Lys 2A 2.23 271451.5 Analyte 3 535.5882 

TM11-0230 040914 Lys 2B 2.23 307518.3 Analyte 3 608.8702 

TM11-0230 040914 Lys 2C 2.23 251278.4 Analyte 3 494.8235 

TMll-0230 040914 Lys 3A 2.23 280230.3 Analyte 3 553.3776 

TM11-0230 040914 Lys 3B 2.23 313072.9 Analyte 3 620.2024 

TM11-0230 040914 Lys 3C 2.24 250157.6 Analyte 3 492.5634 

Vehicle-ACN-DMSO 040914 Lys 1A 2.22 266190.7 Analyte 3 524.9419 

Vehicle-ACN-DMSO 040914 Lys 1B 2.24 313505.9 Analyte 3 621.0863 

Vehicle-ACN-DMSO 040914 Lys 1C 2.23 242638 Analyte 3 477.4121 

Page 11 of 15 Confidential Document 
Study#: 9320-101114 

Vehicle-ACN-DMSO 040914 Lys 2A 2.22 241690.8 Analyte 3 475.5051 

Vehicle-ACN-DMSO 040914 Lys 2B 2.23 300830.4 Analyte 3 595.2422 

Vehicle-ACN-DMSO 040914 Lys 2C 2.22 234929.1 Analyte 3 461.9022 

Vehicle-ACN-DMSO 040914 Lys 3A 2.23 254614.9 Analyte 3 501.5548 

Vehicle-ACN-DMSO 040914 Lys 3B 2.23 325044.3 Analyte 3 644.6683 

Vehicle-ACN-DMSO 040914 Lys 3C 2.23 228368.3 Analyte 3 448.72 

7. Appendix 8: Summary LC/MS/MS data for Cysteine peptide 

lnj. 

Name RT Response Type Vol uM 

BenzoicAcid 042914 Cys 1A 2.38 54564.48 Analyte 3 314.45 

BenzoicAcid 042914 Cys 1B 2.4 56505.727 Analyte 3 320.89 

BenzoicAcid 042914 Cys 1C 2.42 57540.203 Analyte 3 317.43 

BenzoicAcid 042914 Cys 2A 2.41 61364.672 Analyte 3 361.21 

BenzoicAcid 042914 Cys 2B 2.4 55079.891 Analyte 3 310.92 

BenzoicAcid 042914 Cys 2C 2.41 57490.797 Analyte 3 307.19 

BenzoicAcid 042914 Cys 3A 2.4 62591.41 Analyte 3 371.11 

BenzoicAcid 042914 Cys 3B 2.41 53168.629 Analyte 3 317.17 

BenzoicAcid 042914 Cys 3C 2.41 58839.176 Analyte 3 324.87 

Parabenzoquinone 042914 Cys 1A 2.4 928.169 Analyte 3 11.34 

Parabenzoquinone 042914 Cys 1B 2.41 969.609 Analyte 3 11.03 

Parabenzoquinone 042914 Cys 1C 2.42 876.435 Analyte 3 10.17 

Parabenzoquinone 042914 Cys 2A 2.41 780.325 Analyte 3 9.98 

Parabenzoquinone 042914 Cys 2B 2.43 1094.463 Analyte 3 11.67 

Parabenzoquinone 042914 Cys 2C 2.42 854.748 Analyte 3 10.04 

Parabenzoquinone 042914 Cys 3A 2.39 823.232 Analyte 3 10.35 

Parabenzoquinone 042914 Cys 3B 2.42 860.172 Analyte 3 11.39 

Parabenzoquinone 042914 Cys 3C 2.41 943.894 Analyte 3 10.49 

TM05-0293 042914 Cys 1A 2.41 63791.508 Analyte 3 374.02 

TM05-0293 042914 Cys 1B 2.41 55743.16 Analyte 3 329.26 

TM05-0293 042914 Cys 1C 2.41 52999.602 Analyte 3 299.84 

TM05-0293 042914 Cys 2A 2.41 65470.41 Analyte 3 352.89 

TM05-0293 042914 Cys 2B 2.41 57368.285 Analyte 3 344.58 

TM05-0293 042914 Cys 2C 2.42 56805.051 Analyte 3 312.82 

TM05-0293 042914 Cys 3A 2.41 63675.801 Analyte 3 364.27 

TM05-0293 042914 Cys 3B 2.41 58993.984 Analyte 3 348.98 

TM05-0293 042914 Cys 3C 2.41 60136.031 Analyte 3 327.75 

TM08-0338 042914 Cys 1A 2.4 65931.852 Analyte 3 331.51 

TM08-0338 042914 Cys 1B 2.4 59976.742 Analyte 3 316.43 

Page 12 of 15 Confidential Document 
Study#: 9320-101114 

TM08-0338 042914 Cys 1C 2.41 50066.715 Analyte 3 269.94 

TM08-0338 042914 Cys 2A 2.39 67661.688 Analyte 3 327.49 

TM08-0338 042914 Cys 2B 2.39 58192.637 Analyte 3 319.54 

TM08-0338 042914 Cys 2C 2.41 45776.211 Analyte 3 253.21 

TM08-0338 042914 Cys 3A 2.41 64809.23 Analyte 3 492.02 

TM08-0338 042914 Cys 3B 2.41 58317.852 Analyte 3 301.63 

TM08-0338 042914 Cys 3C 2.42 50697.648 Analyte 3 266.76 

TM09-0035 042914 Cys 1A 2.39 66370.43 Analyte 3 391.49 

TM09-0035 042914 Cys 1B 2.4 60817.523 Analyte 3 363.2 

TM09-0035 042914 Cys 1C 2.41 55916.969 Analyte 3 322.48 

TM09-0035 042914 Cys 2A 2.39 69678.031 Analyte 3 392.73 

TM09-0035 042914 Cys 2B 2.41 59218.453 Analyte 3 343.59 

TM09-0035 042914 Cys 2C 2.41 57344.992 Analyte 3 313.09 

TM09-0035 042914 Cys 3A 2.4 68066.984 Analyte 3 388.3 

TM09-0035 042914 Cys 3B 2.39 57576.77 Analyte 3 330.05 

TM09-0035 042914 Cys 3C 2.42 60295.922 Analyte 3 326.43 

TM09-0536 042914 Cys 1A 2.4 45463.344 Analyte 3 260.16 

TM09-0536 042914 Cys 1B 2.4 41606.348 Analyte 3 247.15 

TM09-0536 042914 Cys 1C 2.41 35923.719 Analyte 3 204.54 

TM09-0536 042914 Cys 2A 2.4 46152.043 Analyte 3 265.79 

TM09-0536 042914 Cys 2B 2.42 43359.809 Analyte 3 256.1 

TM09-0536 042914 Cys 2C 2.41 35493.949 Analyte 3 196.62 

TM09-0536 042914 Cys 3A 2.4 45496.813 Analyte 3 267.34 

TM09-0536 042914 Cys 3B 2.42 42873.539 Analyte 3 252.14 

TM09-0536 042914 Cys 3C 2.41 37529.488 Analyte 3 206.18 

TM10-0210 042914 Cys 1A 2.4 19793.67 Analyte 3 122.95 

TM10-0210 042914 Cys 1B 2.41 15582.106 Analyte 3 146.32 

TM10-0210 042914 Cys 1C 2.41 13485.937 Analyte 3 82.26 

TMl0-0210 042914 Cys 2A 2.41 19420.537 Analyte 3 119.64 

TM10-0210 042914 Cys 2B 2.4 13957.505 Analyte 3 84.88 

TM10-0210 042914 Cys 2C 2.41 13073.902 Analyte 3 79.47 

TM10-0210 042914 Cys 3A 2.41 19447.652 Analyte 3 114.93 

TMl0-0210 042914 Cys 3B 2.41 13939.77 Analyte 3 84.49 

TM10-0210 042914 Cys 3C 2.43 13227.693 Analyte 3 77.3 

TM10-0367 042914 Cys 1A 2.39 53708.742 Analyte 3 318.78 

TM10-0367 042914 Cys 1B 2.41 52859.918 Analyte 3 308.07 

TM10-0367 042914 Cys 1C 2.42 42359.691 Analyte 3 231.43 

TM10-0367 042914 Cys 2A 2.39 58097.18 Analyte 3 332.63 

TM10-0367 042914 Cys 2B 2.41 53929.074 Analyte 3 313.49 

TM10-0367 042914 Cys 2C 2.41 41068.949 Analyte 3 232.12 

Page 13 of 15 Confidential Document 
Study#: 9320-101114 

TM10-0367 042914 Cys 3A 2.4 57663.582 Analyte 3 591.12 

TM 10-0367 042914 Cys 3B 2.4 52254.34 Analyte 3 305.33 

TM10-0367 042914 Cys 3C 2.41 42103.457 Analyte 3 226.74 

TM11-0078 042914 Cys 1A 2.4 14194.23 Analyte 3 87.89 

TM11-0078 042914 Cys 1B 2.42 12062.03 Analyte 3 75.12 

TM11-0078 042914 Cys 1C 2.41 10940.657 Analyte 3 65.11 

TM11-0078 042914 Cys 2A 2.39 13846.869 Analyte 3 83.21 

TM11-0078 042914 Cys 2B 2.4 12626.575 Analyte 3 77.3 

TM11-0078 042914 Cys 2C 2.41 10731.423 Analyte 3 128.23 

TM11-0078 042914 Cys 3A 2.4 13840.578 Analyte 3 80.69 

TM11-0078 042914 Cys 3B 2.41 11738.11 Analyte 3 73.26 

TM11-0078 042914 Cys 3C 2.41 11085.54 Analyte 3 66.57 

TM11-0230 042914 Cys 1A 2.39 53818.813 Analyte 3 318.54 

TM11-0230 042914 Cys 1B 2.4 50481.371 Analyte 3 287.96 

TM11-0230 042914 Cys 1C 2.4 50874.363 Analyte 3 273.04 

TM11-0230 042914 Cys 2A 2.39 54379.434 Analyte 3 328.81 

TM11-0230 042914 Cys 2B 2.4 48010.168 Analyte 3 273.56 

TM11-0230 042914 Cys 2C 2.4 49198.027 Analyte 3 274.68 

TM11-0230 042914 Cys 3A 2.42 51539.563 Analyte 3 313.54 

TM11-0230 042914 Cys 3B 2.4 45146.973 Analyte 3 266.76 

TM11-0230 042914 Cys 3C 2.41 53319.477 Analyte 3 278.94 

Vehicle-ACN-DMSO 042914 Cys 1A 2.43 45209.895 Analyte 3 240.2 

Vehicle-ACN-DMSO 042914 Cys 1B 2.41 62032.066 Analyte 3 349.25 

Vehicle-ACN-DMSO 042914 Cys 1C 2.4 52292.09 Analyte 3 275.11 

Vehicle-ACN-DMSO 042914 Cys 2A 2.4 49670.344 Analyte 3 296.23 

Vehicle-ACN-DMSO 042914 Cys 2B 2.4 59084.539 Analyte 3 326.38 

Vehicle-ACN-DMSO 042914 Cys 2C 2.41 52632.48 Analyte 3 283.59 

Vehicle-ACN-DMSO 042914 Cys 3A 2.4 50711.883 Analyte 3 304.82 

1- Vehicle-ACN-DMSO 042914 Cys 3B 2.41 59454.906 Analyte 3 325.49 

Vehicle-ACN-DMSO 042914 Cys 3C 2.41 53668.621 Analyte 3 277.83 

Page 14 of 15 Confidential Document 
Study#: 9320-101114 

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