Evaluation of a new column backflushing set-up in the gas chromatographic–tandem mass spectrometric analysis of pesticide residues in dietary supplements

This study evaluated the use of a new concurrent backflushing set-up in the multiresidue analysis of pesticides in dietary supplement matrices using gas chromatography–tandem mass spectrometry (GC–MS/MS). The backflushing configuration employed a purged union installed between a short, 5-m long capillary column and a 15-m analytical column of the same column diameter (0.25 mm i.d.), stationary phase type (HP-5MS UI) and film thickness (0.25 μm). This set-up is more time- and cost-effective than the use of post-run or mid-column backflushing configurations because the backflushing starts as soon as the last analyte elutes from the short column, thus preventing the less volatile matrix components from reaching the longer analytical column and MS source. As opposed to the analysis without backflushing, the column does not need to be kept at a higher temperature for an extended period of time, resulting in about 50% increased sample throughput on the instrument (a run time of 20 min). Optimization of the GC–MS/MS method is discussed in detail, especially when it comes to the selection of MS/MS transitions, optimization of injection conditions using a programmable temperature vaporizer (PTV) inlet in solvent vent mode, and optimization of the backflushing parameters. The optimized method showed very good long-term performance, which was evaluated in a 2.5-day uninterrupted sequence (without any system maintenance) of repeated injections of various dietary supplement extracts containing over one hundred pesticides, mainly those with limits set for herbal drugs and preparations by the U.S. and European Pharmacopoeias.

► New column set-up for effective concurrent backflushing was optimized and evaluated.
► Its use resulted in rugged and fast analysis of pesticides in dietary supplements.
► Instrument sample throughput was increased by about 50%.
► Decreased instrument maintenance and down-time were achieved in routine analysis.
► Optimization of all important GC–MS/MS method parameters is discussed in detail.