In the development
of modern analytical workflows, parameters such
as sample turnaround time, cost of analysis, and ease of use must
be prioritized. Automation enables reductions in total analysis time,
human intervention, and cost per sample. In this report, a suitable
automated coated blade spray (CBS) workflow is proposed for the screening
and quantitation of multiple substances (i.e., drugs of abuse and
pesticides) in complex matrices. In an attempt to reduce the total
sample analysis time, several parameters were investigated, including
tandem mass spectrometry (MS) dwell time, CBS spray time, and extraction
time. Solid-phase microextraction (SPME) method parameters are explored,
such as reduction of extraction time for increased signal-to-noise.
Model compounds with a moderately wide range of molecular weights
(150–500 Da), polarities, and structural diversity were selected
in order to monitor analytical figures of merit during method optimization.
The resultant automated CBS method proved capable of analyzing the
model compounds in human urine in under 10 s total analysis time with
excellent accuracy (95–120%) and precision (RSD < 12%).
As an application, an automated method for the screening and quantitation
of more than 150 pesticides from apple juice was demonstrated on both
triple quadrupole and orbitrap instruments in under 15 s total sample
analysis time.
As regulatory laboratories search for and implement consolidated methods for multiple matrix and analyte classes, compound lists increase to hundreds or thousands of targets. Multi-instrument approaches are often relied upon to analyze all pesticide targets, with the workload split between liquid chromatography–mass spectrometry (LC–MS) and gas chromatography–mass spectrometry (GC–MS) instrumentation. In this work, a simple solvent extraction approach was coupled with dual source electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) modes on an LC–tandem mass spectrometry (MS/MS) instrument to analyze 395 analytes extracted from black tea (345 compounds via ESI and 50 compounds via APCI, along with the internal standards). Excellent method performance (defined as an accuracy of 70–120% and a precision of <20% at one of two validation levels) was achieved for over 93% of analytes, including compounds normally analyzed by GC–MS, such as trifluralin, chlorfenson, chlormephos, fenchlorphos, etridiazole, and others. This approach can allow the consolidation of a pesticide method to a single instrument or significantly reduce the workload of a complementary GC–MS method.
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