Page 91 - CRFTApplication Compendium_090613

5 Thermo Scienti c Poster Note • PN ASMS13_M011_KHassel_E 07/13S
Conclusion
 Chemotherapeutic research
with method durations of 4
 The Prelude SPLC system
systems, resulting in sample
time also results in reduced
 The Prelude SPLC system
the need for pulse dampene
pumps, does not need prop
check valves. The result: far
and down time.
References
1. Lambert, W.E., et al. Anal
2. Haouala, A. et al. J. Chrom.
3. Panderi, I. J. Chrom. B. 20
Acknowledgeme
I would like to thank everyone in th
providing support and troubleshoo
For re
All trademarks are the pro
arity (r2 ) Recovery
5-0.998 89.4-93.5
1-0.998 92.0-110.2
2-0.998 102.0-110.2
Low QC Mid QC High QC
1.1-10.9 1.8-3.3 1.6-4.2
1.0-1.9 1.1-7.4 1.3-6.2
3.3-7.5 0.6-5.9 2.8-7.8
Intraday Precision (%RSD)
Low QC Mid QC High QC
5.6 5.4 3.9
4.0 2.0 5.9
5.5 2.8 7.5
Interday Precision (%RSD)
100 200 300 400 500 600 700
Methotrexate
Concentration (ng/mL)
0.5 1.0 1.5 2.0 2.5 3.0 0
5000
10000
15000
20000
Busulfan
Time (min)
Intensity (mv)
0.5 1.0 1.5 2.0 2.5 3.0 0
2000
4000
6000
8000
10000
12000
14000
Imatinib
Time (min)
Intensity (mv)
0.5 1.0 1.5 2.0 2.5 3.0 0
50
100
150
200
250
300
350
Methotrexate
Time (min)
Intensity (mv)
sted Using a Prelude SPLC
FIGURE 3. Representative Chromatograms at the LOQ for Each Compound
Tested Using a Prelude SPLC System with TSQ MS
pler Stability Selectivity (% of LOQ)
1-111.3 0.01-7.08
2-96.5 N/A
4-102.5 2.14-5.50
and Selectivity. Prelude SPLC System & TSQ E
Cross-validation of chemotherap
coupled to the new Thermo Scie
spectrometry platform.
Discussion
LC/MS methods for these chemotherapeutic drugs have been done previously with liquid-
liquid extraction and longer HPLC methods (7-15 minutes) 1-3. Off-line techniques such as
liquid-liquid extraction are time consuming and costly from both a material and waste
disposal point of view. On-line sample clean-up lowers the sample preparation duration
and variability of the methods by and minimizing sample handling. Utilizing the new
Prelude SPLC system reduced the run time to under 4 minutes. The shorter method time
allows for higher sample throughput, which is increased further by the multiplexing
capabilities of the Prelude SPLC system. The shorter run time also dramatically reduced
the solvent consumption, leading to further reductions operating cost.
The Prelude SPLC system was specifically designed to reduce instrument maintenance,
down time, and operating costs for high-throughput LC/MS/MS applications that require
sample clean-up prior to HPLC analysis. The Prelude SPLC system utilizes syringe pumps
designed to deliver the volume of mobile phase required for each sample analysis with a
single push of the piston. This pump design greatly reduces the wear and tear on pump
seals and check valves because the pistons in dual piston reciprocating pumps can move
several hundred if not thousands of times per sample run. The majority of maintenance
required on traditional HPLC pumps results from the wear of the seals and check valves;
therefore, syringe pumps are more robust than traditional HPLC pumps. In addition, the
Prelude SPLC system syringe pumps have no need for pulse dampers. The result is that
the Prelude SPLC system has extremely low dead volumes, making rapid changes in
mobile phases possible. The time required for many of the steps in a method to occur are
reduced, resulting in shorter run times and lower solvent costs for equivalent methods
FIGURE 4. Comparison of the Method Run Time for Docetaxel on a Prelude
SPLC System with TSQ MS to that of a Conventional HPLC System
0 50 100 150 200 250 300 350
Prelude SPLC
Conventional HPLC Sample
Clean-up
Sample
Clean-up
Sample
Transfer
Sample
Transfer
Sample Elution
Sample Elution
Column
Clean-up
Column
Clean-up
Equilbration
Equilbration
Time (sec)