Citation: LI Chun-Zheng, CHEN Jia, ZHONG Yu-Huan, ZHONG Yu-Xu, XIE Jian-Wei, LI Hua. Simultaneous Quantification of Thioglycol and Thioglycol Sulfoxide in Rat Plasma by Isotope Dilution-Liquid Chromatography Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2012, 40(10): 1567-1572. doi: 10.3724/SP.J.1096.2012.20249 shu

Simultaneous Quantification of Thioglycol and Thioglycol Sulfoxide in Rat Plasma by Isotope Dilution-Liquid Chromatography Tandem Mass Spectrometry

1.
Beijing Institute of Pharmacology and Toxicology, Beijing 100850, China

Corresponding author: LI Hua,
Received Date: 12 March 2012
Available Online: 15 May 2012
Fund Project: 本工作系国家"重大新药创制"科技重大专项(2008ZXJ09006-001,2010ZXJ0900X-003-002)资助 (2008ZXJ09006-001,2010ZXJ0900X-003-002)

A method based on isotope dilution-liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed and validated to simultaneously quantify metabolites of sulfur mustard, thioglycol (TDG) and thioglycol sulfoxide (TDGO), in rat plasma. Plasma samples were pretreated with the mixed solvent of methanol and acetonitrile to precipitate proteins. The separation of TDG and TDGO was achieved on a ZORBAX-C₁₈ column (3.0 mm×100 mm, 3.5 μm) by gradient elution with mobile phase consisting of methanol and 5 mmol/L ammonium formate aqueous solution. The mass spectrometric identification and quantification were performed using positive electrospray ionization and multiple reactions monitoring mode. An isotopic labeled TDG (d₈-TDG) was used as internal standard. The calibration curves for TDG and TDGO were linear (R²＞0.991) over the range from 5-800 μg/L, and 0.5-80 μg/L, with the lower limit of quantification at 5 and 0.5 μg/L. The recovery of the analytes ranged from 101% to 118%. The intra- and inter-day precisions (RSD) were all within 10%. The plasma was collected and analyzed from HD-exposure rats after subcutaneous administration, and the kinetics parameters of TDG and TDGO were calculated and demonstrated as follow: t_max 30 min and 60 min, c_max (1724±227) μg/L and (301±115) μg/L, AUC (3286±249) μg·h/L and (1010±363) μg·h/L, respectively.
- Sulfur mustard,
- Thioglycol,
- Thioglycol sulfoxide,
- Liquid chromatography-tandem mass spectrometry,
- Plasma,
- Toxicokinetics
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