Application hints
Instruction Manual, Feb-17
21
Sample Application
HPTLC-Plates Si 60 F254 20x10 cm, Merck (Darmstadt), were pre-cleaned with methanol
in a CAMAG Twin-Trough Chamber and dried at 60°C for 20 minutes. Sample solutions
were applied with a CAMAG Automatic TLC Sam-pler ATS4, 5 µl band wise, 4 mm wide.
Distance from the lower edge 10 mm.
Solvent
Toluene: Ethyl acetate: Formic Acid
50:45:5
Chromatography
CAMAG ADC automatic development chamber with the following parame-ters:
Saturation 10 minutes; migration distance 60 mm; drying time 5 minutes.
Documentation
CAMAG Visualizer (or DigiStore 2) Documentation System at 254nm.
Fig. 14: Separation of Paracetamol, Caffeine, Acetylsalicylic Acid, mixture (from left to
right), 25µg substance per spot.
HPLC Conditions
Column:
none
Elution Solvent:
Eluent A: 95%
acetonitrile with 0.1% formic acid
Eluent B: 5%
H
2
O with 0.1% formic acid
Flow:
0.2 ml/min.
Run time:
6 minutes
The TLC-MS Interface 2 was directly connected to the HPLC pump (at the position of the
6-port valve of the HPLC normally connected to the column). The exit of the Interface was
directly coupled to the MS inlet valve.
MS conditions Agilent MSD Trap XCT plus
Source
APCI
Mode
positive
and negative
Corona
4'000nA
in negative mode 20'000nA
Summary of Contents for TLC-MS INTERFACE 2
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