ACE UHPLC and HPLC Columns
Paralytic Shellfish Poisoning (PSP) Toxins
Reproduced with permission of CEFAS, Weymouth, UK
Time - Minutes
Parotoid Macrogland Secretions from South American Toads
1.6 1.6
1.4 1.4
1.2 1.2
1.0 1.0
(Volts)
(Volts)
0.8 0.8
0.6 0.6
0.4 0.4
0.2 0.2
0 0
118
0 2 0 2
4 6 8 10 12 14 16 18 20 22 24 26 28 30 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time - Minutes Time - Minutes
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1
3
1
3
- H H2N-COO
- H H2N-COO
- H O3S-NH-COO
- H OH
6
2
9
5
10
R. major 4
4
5
6 7 8
2
3
R. crucifer
1
2
3
4
5
6
7
8
1 2
3
4
5
6
7
8
Column: ACE UltraCore 5 SuperC18
Dimensions: 150 x 4.6 mm
Part Number: CORE-5A-1546U
Mobile Phase: A: 0.1 M ammonium formate
in H2O
B: 0.1 M ammonium formate
in H2O/MeOH (95:5 v/v)
Gradient: Time (mins) %B
0.00 0
2.00 0
4.00 80
5.50 80
5.51 0
7.00 0
Flow Rate: 2 mL/min
Injection: 30 μL
Temperature: 20 °C
Detection: Fluorescence lEx 340 nm,
lEm 395 nm
Sample: Prechromatographic oxidation
with hydrogen peroxide and
periodate
Application #AN3180
Conditions Analytes
1. dcGTX2,3
2. GTX1/4 + dcGTX2,3
3. C1,2
4. dcSTX + dcNEO
5. dcSTX + NEO
6. GTX2/3 + GTX1/4
7. GTX5
8. STX + NEO
PST
Variant
R1 R2 R3 R4
STX H H H HN-COO
2NEO OH H H HN-COO
2GTX1 OH H OSO- HN-COO
3
2- H2N-COO
GTX2 H H OSO3
GTX3 H OSO3
GTX4 OH OSO3
GTX5 (B1) H H H OS-NH-COO
3C1 H H OSO- OS-NH-COO
3
3C2 H OSO3
dcSTX H H H OH
dcNEO OH H H OH
dcGTX1 OH H OSO3
- OH
- OH
dcGTX2 H H OSO3
dcGTX3 H OSO3
Column: ACE 5 C18
Dimensions: 250 x 4.6 mm
Part Number: ACE-121-2546
Mobile Phase: A: 0.1% TFA in H2O
B: 0.1% TFA in MeCN/H2O
(90:10 v/v)
Gradient: Time (mins) %B
0 0
5 0
25 100
Flow Rate: 1 mL/min
Detection: PDA, 214 nm (Scanning 200-500 nm)
Application #AN3970
Conditions Analytes
1. Serotonin
2. N-Methylserotonin
3. N,N-Dimethylserotonin (bufotenine)
4. Dehydrobufotenine
5. Hellebrigenin
6. Marinobufagin
7. Telocinobufagin
8. Bufalin
9. Hellebrigenol-3-O-sulphate
10. Desacetylcinobufagin
1
3
1
3
6
2
9 5 10
R. major 4
R. Crucifer R. Major
Sciani JM, Angeli CB, Antoniazzi MM, Jared C, Pimenta DC. Differences and Similarities among Parotoid Macrogland Secretions in South American Toads: A
Preliminary Biochemical Delineation.The Scientific World Journal 2013, http://dx.doi.org/10.1155/2013/937407