Screening for basic drugs in equine urine using direct-injection differential-gradient LC-LC coupled to hybrid tandem MS/MS

Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Shawn M R Stanley, Hsiao Ching Foo

Abstract

A rapid, selective and robust direct-injection LC/hybrid tandem MS method has been developed for simultaneous screening of more than 250 basic drugs in the supernatant of enzyme hydrolysed equine urine. Analytes, trapped using a short HLB extraction column, are refocused and separated on a Sunfire C(18) analytical column using a controlled differential gradient generated by proportional dilution of the first column's eluent with water. Independent data acquisition (IDA) was configured to trigger a sensitive enhanced product ion (EPI) scan when a multiple reaction monitoring (MRM) survey scan signal exceeded the defined criteria. The decision on whether or not to report a sample as a positive result was based upon both the presence of a MRM response within the correct retention time range and a qualitative match between the EPI spectrum obtained and the corresponding reference standard. Ninety seven percent of the drugs targeted by this method met our detection criteria when spiked into urine at 100 ng/ml; 199 were found at 10 ng/ml, 83 at 1 ng/ml and 4 at 0.1 ng/ml.

References

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Citations

Jun 23, 2009·Journal of the American Society for Mass Spectrometry·J Larry CampbellJ C Yves Le Blanc
Aug 15, 2009·Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment·Y ChenY Wu
Nov 21, 2014·Bioanalysis·Maryam RezazadehShahram Seidi
Jan 15, 2017·Drug Testing and Analysis·A G FragkakiM Tsivou
Jan 31, 2007·Journal of Mass Spectrometry : JMS
Mar 10, 2015·Analytical and Bioanalytical Chemistry·Pierre-Luc Latreille, Xavier Banquy
Jan 14, 2021·Drug Testing and Analysis·Fernando MoreiraMaria de Lourdes Bastos
Mar 13, 2021·Analytical Methods : Advancing Methods and Applications·Youwen YouMary A Robinson

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