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Related Experiment Video

Updated: May 18, 2026

Integration of Miniaturized Solid Phase Extraction and LC-MS/MS Detection of 3-Nitrotyrosine in Human Urine for Clinical Applications
08:41

Integration of Miniaturized Solid Phase Extraction and LC-MS/MS Detection of 3-Nitrotyrosine in Human Urine for Clinical Applications

Published on: July 14, 2017

Quantification of limonin in human urine using solid-phase extraction by LC-MS/MS.

Shijia Liu1, Jun Zhang, Ling Zhou

  • 1State Key Laboratory of Natural Medicines (China Pharmaceutical University), Nanjing 210009, China.

Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
|September 25, 2012
PubMed
Summary

A new method accurately measures limonin in urine, crucial for understanding its effects in the body. This validated assay enables precise pharmacokinetic studies of limonin in humans.

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Area of Science:

  • Pharmacology
  • Analytical Chemistry
  • Biochemistry

Background:

  • Limonin, a citrus compound, has potential health benefits requiring pharmacokinetic evaluation.
  • Accurate quantification of limonin in biological matrices like urine is essential for such studies.

Purpose of the Study:

  • To develop and validate a highly sensitive analytical method for determining limonin in human urine.
  • To utilize this method for pharmacokinetic investigations of limonin in humans.

Main Methods:

  • Development of a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method.
  • Solid-phase extraction (SPE) for sample preparation.
  • Isocratic elution on a C18 column with subsequent MS/MS detection in multi-reaction monitoring (MRM) mode.

Main Results:

  • The method demonstrated high sensitivity with a linear range of 0.0783-10 ng/mL and a lower limit of quantification (LLOQ) of 0.0783 ng/mL.
  • Extraction recovery exceeded 76.7%, and precision (inter- and intra-day) was less than 7.4%.
  • The validated method was successfully applied to a human pharmacokinetic study.

Conclusions:

  • A robust and sensitive LC-MS/MS method for limonin determination in human urine has been established.
  • This validated assay is suitable for pharmacokinetic studies, facilitating further research into limonin's biological activity.