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Related Manuals for CAMAG TLC-MS INTERFACE 2
Summary of Contents for CAMAG TLC-MS INTERFACE 2
- Page 1 INSTRUCTION MANUAL TLC-MS INTERFACE 2...
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Page 2: Table Of Contents
Content Introduction ..............................2 Precaution ............................... 2 Parts supplied ............................3 Unpacking/Installation ..........................4 Unpacking ............................... 4 Installation environment .......................... 4 Installation .............................. 4 Connection of the valve ........................... 5 Getting started .............................. 6 Intended use ............................6 Instrument .............................. 6 Functional principle .......................... -
Page 3: Introduction
Only authorized personnel may open the instrument. Service and repair is only to be performed by trained specialists. Use spare parts and consumables supplied by CAMAG only. The warranty is voided if parts from other sources are used. Check the service manual before you start service to reduce product-specific risks •... -
Page 4: Parts Supplied
Introduction • Lift/move/transport the system with the necessary care and with sufficient manpower (install the transport security devices if applicable, transport it only in the original packaging) • This symbol indicates that this equipment must not be disposed of as unsorted municipal waste but is to be collected separately as electrical and electronic equipment (WEEE-Directive 2002/96/EC). -
Page 5: Unpacking/Installation
CAMAG strongly recommends using an additional inline filter filter between the TLC-MS Interface 2 (Valve port 1) and the MS. The porosity of the filter is depending on the usage, CAMAG recommends to use a filter with the porosity of 0.2 µm 2.3 Installation... -
Page 6: Connection Of The Valve
Unpacking/Installation 2.4 Connection of the valve To inline filter and LCMS From LC pump Internal Bypass position filter Elution position Color sleeve Compressed air at cleaning Dummy plug 666.4008 Elution head Fig 1 Instruction Manual, Feb-17... -
Page 7: Getting Started
Getting started 3 Getting started 3.1 Intended use The TLC-MS Interface 2 is intended for the use described in this manual. 3.2 Instrument Fig. 2 Control elements: Laser cross hair on/off Piston up/down Cleaning on/off Screw for fixing the security cover... -
Page 8: Functional Principle
TLC/HPTLC plate or foil with separated substance zone Fig. 3: TLC-MS Interface 2 in bypass position After lowering the piston, switch the valve to elution position. The solvent passes through the elution head onto the silica gel, elutes the sample and transports it directly to the LC/MS-System. - Page 9 TLC/HPTLC plate or foil with separated substance zone Fig. 4: TLC-MS Interface 2 in elution position After each elution remove the plate/foil. Make sure the valve is in position “Bypass” and press the cleaning button at least 3 times for 3 seconds. The capillary from the plate to the valve and internal frit are cleaned with the help of compressed air.
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Page 10: Elution Process
Cleaning in upper position Pressure TLC/HPTLC plate or foil with separated substance zone Fig. 5: TLC-MS Interface 2 in bypass position , cleaning active 3.4 Elution process • Make sure, that the valve is in the rear, Bypass position •... -
Page 11: Operation Advice
Maintenance and Service 3.5 Operation advice • Elution of a sample–free area on the plate cleans the system from residues of the last elution. In this manner you can also measure the plate background for later correction • The positioning table must be wiped off before you put a plate or foil on it. •... -
Page 12: User Maintenance
The maintenance data sheet informs about maintenance interval of the respective instrument as well as the proposal for IQ/OQ interval if applicable. In addition, it identifies parts subject to wear with the respective replacement cycle and CAMAG order number. Maintenance interval Maintenance... -
Page 13: Replacing Of Elution Head
Technical data 4.5 Replacing of elution head • Remove the security cover • Remove the blue top cover • Remove the elution head capillaries to port 3 and port 6 (the filter) of the valve • Make sure the filter to port 6 of the valve is changed if the head is replaced •... -
Page 14: Application Hints
For the delivery of the eluent, a HPLC pump is needed. You may use the internal pump of the HPLC-MS. Remove the HPLC column if installed and connect the respective capillary from the TLC-MS Interface 2 to the solvent delivery capillary of the HPLC (as described in this manual). - Page 15 Application hints A general rule of thumb for HPLC-MS: Dilute the solutions you typically use for UV- detection (approx. 1 mg/mL in e.g. methanol) by a factor of 1000 or 100, resulting in concentrations of 1 to 10 µg/mL. Use flow injection analysis (FIA) of 0.1 µL and watch the MS signal.
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Page 16: Fittings
Application hints If available use HPTLC plates. Prior to use, prewash plates by developing once to the upper edge with neat methanol. Dry the plates for 10 min at 60°C in a vacuum drying oven or by heating for 20 min at 120°C in a clean (!) convection oven. The preferred sample application technique is the spray-on technique using the Automatic TLC Sampler 4 or the Linomat 5. - Page 17 Application hints bottom of the receiving port. Improper cutting of the tubing could lead to dead volume, resulting in peak distortion such as fronting, tailing or broadening. Procedure with stainless steel nuts and ferrules: Slide the fitting at least 5 mm from the end of the clean cutting tube. •...
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Page 18: Dead Volumes
Application hints port, the tubing pocket beyond the ferrule will be completely filled to help avoid dead volume in the connection. Tubing sleeves also offer several side benefits. One is the structural support sleeves provide to the outside of the capillary tubing, helping prevent damage to the tubing as it leaves the fitting. -
Page 19: System Leaks
Application hints 6.4 System leaks Telltale signs of system leaks Before you even see your first drip from a fitting, your system can tell you that the problem exists. The most common signs of system leaks are as follows: No flow or pressure Pump pressures up, but no flow Noisy baseline Baseline drift... -
Page 20: Application Example
Application hints 6.5 Application example Sample: diclofenac in methanol at a concentration of 0.113 mg/mL Layer: 20x10 cm HPTLC plate Si60 F254, prewashed with methanol; UV 254 nm Application: 1, 2, 4, and 10 μL as 8 mm bands Mobile phase: toluene – ethyl acetate – acetic acid 50 : 40 : 1 (v/v/v) Development: ADC2, saturated chamber, 70 mm from lower edge of plate Under UV 254nm mark zones with a soft pencil. -
Page 21: Separation Of Caffeine, Paracetamol, Acetylsalicylic Acid
Application hints Place the elution head over the first sample zone, lower the elution head and switch the valve to elution position. Make a note of the time, when the elution started. After approx. 1 to 1.5 minutes, the elution is finished. Switch the valve to rear position to stop the elution. - Page 22 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.
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Page 23: Results
All MS runs were started manually. CAMAG TLC-MS Interface 2 The selected sample zone is positioned below the elution head (either by means of the laser crosshairs, or by means of the x-y-scale). The elution head is lowered onto the HPTLC plate. - Page 24 Application hints Fig. 16: Same plate as in Fig. 15, partially extracted with CAMAG TLC-MS Interface 2. Resulting detection limits Detection limits in MS strongly depend on the ability of substances to be ionized, as well as on the selected ionization source (mainly ESI, APCI or APPI).
- Page 25 Application hints Measurement near the limit of quantity Fig. 18: Upper part: Elution of 25 ng caffeine per spot, registration of the TIC (total ion cur-rent), baseline shows relative high noise. Lower part: MS of caffeine with APCI ionization, [M+H]+ ion (195.1 Da) is still clearly visible, background noise from the plate reaches approx.
- Page 26 49 30 516 55 50 · Fax 49 30 795 70 73 · E-Mail: infoberlin@camag.com CAMAG Scientific Inc. (USA) · 515 Cornelius Harnett Drive · Wilmington, NC 28401 Telephone 800 334 3909 · Fax 910 343 1834 · E-Mail: tlc@camag.com www.camag.com...
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