Objective  To establish a method for rapid screening and quantifying the illegal addition of metolazone in tablet candy by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS).

Methods The component in samples was extracted with acetonitrile, then purified by Captiva EMR-Lipid purification column, detected by UPLC-Q-TOF/MS with Agilent RRHD Eclipse Plus C₁₈ chromatographic column (100 mm×2.1 mm, 1.8µm) under Targeted MS/MS mode.

Results The linear regression analysis data for the calibration plots showed a good linear relationship over the concentration range of 50-1 000 ng·mL^-1 for metolazone (r=0.999 0); the value of detection limit and quantification limit was found to be 1.0 μg·g^-1 and 2.5 μg·g^-1. The average recovery rate was 98.15% (RSD=2.2%, n=18).

Conclusion  The method had the advantages of simple operation, qualitative and quantitative accuracy. It could be applied to daily inspection.

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