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Open AccessArticle

Simultaneous Determination of Etomidate and Its Major Metabolite, Etomidate Acid, in Urine Using Dilute and Shoot Liquid Chromatography–Tandem Mass Spectrometry

1
Department of Chemistry, Yonsei University, Wonju 26493, Korea
2
Forensic Genetics and Chemistry Division, Supreme Prosecutors’ Office, Seoul 06590, Korea
*
Author to whom correspondence should be addressed.
Molecules 2019, 24(24), 4459; https://doi.org/10.3390/molecules24244459
Received: 14 October 2019 / Revised: 3 December 2019 / Accepted: 3 December 2019 / Published: 5 December 2019
(This article belongs to the Special Issue Forensic Analytical Chemistry)
Etomidate (ET) is a commonly used sedative-hypnotic agent such as propofol to induce anesthesia, and it is rapidly metabolized to etomidate acid (ETA) in liver. Herein, a simple method to determine ET and ETA in urine simultaneously was developed using liquid chromatography–tandem mass spectrometry (LC–MS/MS). A simple sample preparation method reduced the total analysis time. For all analytes, the separation was achieved in 6.5 min using reversed-phase chromatography with gradient elution. The best separation and detection of ETA was achieved using a porous graphitic carbon column. The column temperature was maintained at 30 °C to improve the efficiency and sensitivity. The calibration curves were linear over the concentration ranges of 0.4–120.0 ng/mL (ET) and 1.0–300.0 ng/mL (ETA), obtained with a weighting factor of 1/x2. The coefficients of determination (r2) were greater than 0.9958. The lower limits of quantification were 0.4 ng/mL (ET) and 1.0 ng/mL (ETA), intra-day (n = 6) and inter-day (n = 24) precision values for all compounds were less than 10.2% and 8.4%, respectively, while the intra- and inter-day accuracies were in the −9.9–2.9%, and −7.0–0.6%. The applicability of the method was examined by analyzing the urine samples obtained from ET users. View Full-Text
Keywords: etomidate; etomidate acid; metabolite; urine; dilute and shoot; LC-MS/MS etomidate; etomidate acid; metabolite; urine; dilute and shoot; LC-MS/MS
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MDPI and ACS Style

Jung, Y.-K.; You, S.Y.; Kim, S.-Y.; Kim, J.Y.; Paeng, K.-J. Simultaneous Determination of Etomidate and Its Major Metabolite, Etomidate Acid, in Urine Using Dilute and Shoot Liquid Chromatography–Tandem Mass Spectrometry. Molecules 2019, 24, 4459.

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