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High-sensitivity and simultaneous analysis of Psychoactive drugs
using LC-MS/MS with full-automated pretreatment system
MS MS
Analytical column
Trap column Mobile phase
for trapping
Mobile phase
for trapping
Mobile phase A+B Mobile phase A+B
Drain
Drain
Position 0 Position 1
Figure 5 Flow diagram of trapping system
LC/MS/MS conditions (Nexera system and LCMS-8060)
Ionization : ESI, Positive/Negative MRM mode
Trap column : Unison UK-C18 (10×2 mm, 3 m, Imtakt)
Analytical column : Unison UK-C18 (75×2 mm, 3 m, Imtakt)
Mobile phase for traping : 5% MeOH / 0.1% Formic acid
Mobile phase A : 10mM Ammonium formate, 5% Methanol
B : 10mM Ammonium formate, 95% Methanol
Time program : B conc. 0 % - (1 min) - 5 % - (7 min) - 95 % (3 min)
Result
Recovery rate
Usually LC-MS/MS analysis of biological samples require were only ltration. The treated samples were trapped
some manual preparation steps such as protein for cleaning and concentration, then separated by
precipitation, solid phase extraction or liquid/liquid Unison UK-C18 in HPLC Unit.
extraction before the injection. With the aim to reduce
the operator involvement, to increase the throughput The recovery of whole blood spiked with sixty
and the data quality, we completely eliminated the psychoactive drugs were more than 70% and the
manual sample preparation procedure by the use of a recovery of serum and urine spiked with them were
novel automatic preparation unit including precipitation, more than 80%. We completed analysis of their
ltration, incubation, shaking and pipetting. Serum and psychoactive drugs in several biological matrices using
whole blood spiked with sixty psychoactive drugs were the automated sample preparation system coupled to
pretreated with organic solvent and ltration by the LC-MS/MS
unit. On the other hands, urine spiked with their drugs
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