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Updated: Nov 22, 2025

Sample Preparation for Probe Electrospray Ionization Mass Spectrometry
Published on: February 19, 2020
Electrospray Ionization Inlet Tandem Mass Spectrometry: A Hyphenated Method for the Sensitive Determination of
Shubhashis Chakrabarty1, Weilin L Shelver1, David J Smith1
1USDA-Agricultural Research Service, Edward T. Schafer Agricultural Research Center, Biosciences Research Laboratory, 1616 Albrecht Boulevard, Fargo, North Dakota 58102, United States.
Abstract:
This study demonstrates the utility of electrospray ionization inlet mass spectrometry (ESII-MS/MS) for the quantitative determination of analytes in complex animal matrices without chromatographic separation. Veterinary drugs including flunixin, its metabolite 5-hydroxyflunixin, and zilpaterol and persistent organic perfluoroalkyl compounds were determined in incurred plasma, urine, and/or tissue samples. Limits of detection (LOD) of zilpaterol in kidney, liver, lung, and muscle ranged from 0.02 to 0.06 ng/g, whereas the limit of quantitation (LOQ) for zilpaterol in all tissues was 0.1 ng/g. For urinary or plasma flunixin, 5-hydroxyflunixin, and PFOS/PFHxS, LODs ranged from 0.1 to 0.7 ng/mL while the LOQs ranged from 0.4 to 50 ng/mL. Regression coefficients for matrix-matched standard curves were 0.993-0.997, 0.977-0.999, and 0.999 for plasma, tissues, and urine, respectively. Correlations between quantitative results obtained by ESII-MS/MS and LC-MS for flunixin, 5-hydroxyflunixin, and zilpaterol ranged from 0.930 to 0.985. ESII-MS/MS provided rapid, sensitive, and accurate analyses of veterinary drugs and environmental contaminants from complex matrices without chromatographic separation.
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