Supplementary Data

Collision-Induced Dissociation Pathways of H1-Antihistamines by Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry

Jung-Ah Do1, Eunyoung Noh1, Soon-Byung Yoon1, Ji Hyun Lee1, Sung-Kwan Park1, Suresh Mandava2, Sun Young Baek1,*, Jongkook Lee2,*

1Advanced Analysis Team, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si 28159, Republic of Korea

2College of Pharmacy, Kangwon National University, 1 Kangwondaehak-gil, Chuncheon, Gangwon-do 24341, Republic of Korea

Contents

1.  Supplementary Table S1–S3

2.  Supplementary Fig. S1–S7

3.  MS2 spectra of H1-antihistamines

1.  Supplementary Tables

Table S1 Structural classification of H1-antihistamines

Classification / H1-Antihistamines
Group 1
Alkylamines / Chloropheniramine
Bromopheniramine
Allylamines / Acrivastine
Triprolidine
Piperazines / Cetrizine (levocetrizine)
Hydroxyzine
Aminoethers / Diphenhydramine
Ebastine
Clemastine
Piperidines / Fexofenadine
Terfenadine
Group 2
Tricyclic compounds / Loratadine
Desloratadine
Cyproheptadine
Ketotifen
Olopatadine
Promethazine
Group 3
Others / Azelastine
Astemizole
Epinastine

Table S2 Molecular weights (MW) and calculated mass values (m/z) for protonated molecules [M+H]+ and the distinguishable fragment ions

H1-antihistamines / MW / [M+H]+ / Frag. 1 / Frag. 2 / Frag. 3 / Frag. 4 / Frag. 5
Acrivastine / 348.438 / 349.192 / 278.118 / 260.108 / 232.113
Astemizole / 458.570 / 459.256 / 308.156 / 242.109 / 218.154 / 135.081
Azelastine / 381.898 / 382.169 / 271.064 / 112.113
Bromopheniramine / 319.239 / 319.081 / 274.023 / 167.073
Cetirizine / 388.889 / 389.163 / 201.047 / 166.078
Chloropheniramine / 274.788 / 275.132 / 230.074 / 167.063
Clemastine / 343.890 / 344.178 / 215.063 / 180.094 / 137.016 / 130.123
Cyproheptadine / 287.398 / 288.175 / 215.086 / 191.086
Desloratadine / 310.821 / 311.132 / 294.105 / 282.105 / 259.136
Diphenhydramine / 255.356 / 256.170 / 167.086
Ebastine / 469.658 / 470.306 / 203.144 / 167.086
Epinastine / 249.310 / 250.134 / 231.092 / 193.089 / 178.078 / 165.070
Fexofenadine / 501.656 / 502.296 / 484.285 / 466.275 / 171.117 / 131.086
Hydroxyzine / 374.904 / 375.184 / 201.047 / 166.078
Loratadine / 382.883 / 383.153 / 337.111 / 294.105 / 280.089 / 267.081 / 259.136
Ketotifen / 309.425 / 310.127 / 221.042 / 213.037 / 197.042
Olopatadine / 337.412 / 338.176 / 293.118 / 247.112 / 165.055
Promethazine / 284.419 / 285.143 / 240.085 / 198.038
Terfenadine / 471.673 / 472.322 / 454.311 / 436.300 / 262.160
Triprolidine / 278.391 / 279.186 / 208.113 / 193.089

Table S3 Mass error in ppm for protonated molecules [M+H]+ and the distinguishable fragment ions

H1-antihistamines / [M+H]+ / Frag. 1 / Frag. 2 / Frag. 3 / Frag. 4 / Frag. 5
Acrivastine / 26 / 4 / 0 / 17
Astemizole / 2 / 3 / 8 / 0 / 0
Azelastine / 5 / 0 / 0
Bromopheniramine / 6 / 0 / 6
Cetirizine / 2 / 5 / 0
Chloropheniramine / 22 / 9 / 42
Clemastine / 29 / 5 / 6 / 7 / 0
Cyproheptadine / 14 / 5 / 5
Desloratadine / 0 / 10 / 4 / 0
Diphenhydramine / 12 / 6
Ebastine / 0 / 0 / 0
Epinastine / 0 / 4 / 0 / 0 / 0
Fexofenadine / 10 / 10 / 11 / 29 / 46
Hydroxyzine / 3 / 5 / 0
Loratadine / 3 / 0 / 3 / 0 / 0 / 0
Ketotifen / 0 / 5 / 5 / 5
Olopatadine / 6 / 24 / 0 / 12
Promethazine / 4 / 4 / 5
Terfenadine / 17 / 11 / 16 / 8
Triprolidine / 7 / 5 / 5

2.  Supplementary Figures

Fig. S1 Structures of 21 H1-antihistamines

Fig. S2 Proposed fragmentation pathway for triprolidine

Fig. S3 Proposed fragmentation pathway for clemastine

Fig. S4 Proposed fragmentation pathway for terfenadine

Fig. S5 Proposed fragmentation pathways for cyproheptadine and ketotifen

Fig. S6 Proposed fragmentation pathways for olopatadine and promethazine

Fig. S7 Proposed fragmentation pathway for epinastine

3.  MS2 spectra of H1-antihistamines

Acrivastine

Astemizole

Azelastine

Brompheniramine

Cetirizine

Chlorpheniramine

Clemastine

Cyproheptadine

Desloratadine

Diphenhydramine

Ebastine

Epinastine

Fexofenadine

Hydroxyzine

Ketotifen

Loratadine

Olopatadine

Promethazine

Terfenadine

Triprolidine

6