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Determination of Tretoquinol in Pungent Spice by Solid-phase Extraction Coupled Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry |
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DOI: |
KeyWord:tretoquinol solid-phase extraction ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) pungent spice |
Author | Institution |
ZHANG Hai-chao,WANG Jing,JIA Hai-tao,LI Wei,AI Lian-feng,KANG Wei-jun |
1. Shijiazhuang Customs Technology Center,Shijiazhuang ,China; 2. School of Public Health,Hebei Medical University,Shijiazhuang ,China |
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Abstract: |
An ultra-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of tretoquinol in pungent spice with MCX solid-phase extraction(SPE) purification. The samples were extracted with 0.2% acid ethanol, purified with a MCX column, and quantified by UPLC-MS/MS in MRM mode after gradient elution on an ACQUITY BEH C18 column with acetonitrile and 0.1% formic acid solution as mobile phase. The results showed that the calibration curves were linear in the range of 0.1-50 ng/mL with correlation coefficients(r) more than 0.998. The limits of detection (LODs) were 0.2 μg/kg and the limits of quantitation (LOQs) were 0.5 μg/kg. The average recoveries of tretoquinol at four different spiked levels (0.5, 2, 10, 100 μg/kg) ranged from 74.5% to 98.8%,with relative standard deviations(RSD) of 3.1%-9.1%. The proposed method is sensitive, accurate and reliable, and could be used for the determination of tretoquinol in pungent spice. |
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