Purospher® STAR RP-18 Endcapped for LC-MS Applications
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"Ghost" mass peaks present a challenge frequently encountered in gradient LC-MS. It is impossible to determine whether ghost peaks originate from an unknown compound in the sample, from an impurity in the mobile phase, or from bonded phase leaching. However, a three-step procedure can help you avoid spurious LC-MS peaks and ensure consistent ghost-peak-free HPLC separations. The simple process includes cleaning the columns and choosing appropriate solvents for LC-MS. These steps increase ionization efficiency, thus improving the sensitivity and reproducibility of LC-MS results.
Simple, 3-Step Process for Optimized Performance in LC-MS
- Flush the column for 60 minutes with a special solvent mixture to remove possible trace impurities. The recommended LC-MS wash solvent is 2-propanol with 0.1% formic acid at a flow rate of 0.5 mL/min (for 3 mm ID columns).
- To reduce the LC-MS background signal, work with extremely high-purity solvents. The recommended solvent is LiChrosolv® Hypergrade with special MS specifications.
- Finally, the column must be re-equilibrated with the mobile phase. Best results are obtained when two blank solvent gradients (without sample injection) are run prior to analysis. Purospher® STAR RP-18 endcapped HPLC columns produce very low and stable background signals in LC-MS, simply after washing with 2-propanol / 0.1% formic acid.
Extracted Ion Chromatograms of "Profens" in Negative Ion Mode Separated on Purospher® STAR RP-18 Endcapped
The combination of LiChrosolv® Acetonitrile Hypergrade solvents and Purospher® STAR RP-18 endcapped columns demonstrates ghost-peak-free MS spectra for Ketoprofen, Fenoprofen, and Ibuprofen (100 ng).
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Column
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Purospher® STAR RP-18 endcapped (3µm) LiChroCART® 55-2 HPLC column |
Mobile Phase A
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0.1% acetic acid in acetonitrile |
Mobile Phase B
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0.1% acetic acid in water |
Gradient
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From 25% A to 50% A in 3 min, then isocratic |
Flow rate
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300 µL, without split |
Detection
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UV 220 nm, Ion Trap MS |
Temperature |
Ambient |
Inj. volume
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1 µL |
Sample |
Ketoprofen, Fenoprofen, Ibuprofen; 0.1 µg/µL |
MS Conditions |
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Ionization |
ESI(-) |
Nebulizer |
36 psi |
Dry gas |
8.5 L/min |
Dry temperature |
330°C |
Smart mode optimization |
Target mass 205 |
Ion charge control
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Target 50.000, max 50 ms |
Scan mode |
Standard/Normal |
Scan range |
50-600 m/z |
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