Page 8 - Shimadzu LCMS-8040

Ultra-High Reliability to

Withstand Wide Range of Complex Matrices

Exceptional Durability
Blood plasma samples were spiked with verapamil and warfarin, and warfarin by ESI − was performed. Chromatograms for the 1st, 250th,
then deproteinized according to the pretreatment process indicated and 450th measurements are shown below. This resulted in 1 pg
below. The area values from 450 consecutive LCMS-8040 analyses on-column area repeatability of 4.18% for verapamil and 6.61% for
were then plotted. Simultaneous analysis of verapamil by ESI + and warfarin.

×10 4
3.0 Column: Shim-pack XR-ODS II
Verapamil (2.0 mmI.D. × 50 mmL, 2.2 μm)
2.5
Warfarin Mobile Phase A: 5 mmol/L
ammonium acetate –water
2.0
Mobile Phase B: Acetonitrile
Gradient Program:
Area 1.5 60%B (0 –1.50 min) –
90%B (1.51–3.00 min) –
1.0 60%B (3.01–4.50 min)
Flow Rate : 0.4 mL/min.
0.5
0.0
0 50 100 150 200 250 300 350 400 450
Injection
200 μL plasma sample
Add 200 μL Acetonitrile, 50 μL 50% methanol aqueous solution and 50 μL verapamil and warfarin standard solutions.
Vortex and centrifuge (10000 rpm, 3 min.) followed by freeze drying.
Add 500 μL dilution solution.
Vortex and centrifuge (12000 rpm, 5 min.).

(×1,000) (×1,000) (×1,000)
6.0 1 st injection 6.0 250 th injection 6.0 450 th injection
5.0 5.0 5.0
4.0 4.0 4.0
3.0 3.0 3.0
2.0 2.0 2.0
1.0 1.0 1.0
0.0 0.0 0.0
0.3 0.4 0.5 0.6 0.7 min 0.3 0.4 0.5 0.6 0.7 min 0.3 0.4 0.5 0.6 0.7 min

Ultra Fast Speed Combined with Lower Femtogram Detection

Using the same chromatography parameters as described above, analysis Verapamil Warfarin
of plasma samples spiked with 40 fg/μL verapamil and warfarin were 455.25 >165.05(+) 300 307.20 >161.05(-)
1200
injected into the LCMS-8040 for signal to noise determination. For 100
fg on-column, a S/N ratio of 146 (rms) was obtained for verapamil and 250
1000
30 (rms) for warfarin.
800 200
600 150
The resulting lower limits of detection for S/N = 3 (rms) were 2.05 fg for
verapamil and 9.88 fg for warfarin.
400 100
Compounds Verapamil Warfarin 200 50
S/N: 100 fg on column (rms) 146 30
0 0
LOD(fg) Calculated at S/N = 3 2.05 9.88 0.25 0.50 min 0.50 0.75 1.00 min
Chromatograms of 100 fg Verapamil and Warfarin On-Column

8 Sp e e d B eyond C o mp ari s on E n h a nc e d Se n s itivit y