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http://dx.doi.org/10.5012/bkcs.2010.31.8.2322

Analysis of Heterocyclic Amines in Human Urine Using Multiple Solid-Phase Extraction by Liquid Chromatography/Mass Spectrometry  

Cha, Hyun-Jeong (Seoul Center, Korea Basic Science Institute)
Kim, Nam-Hee (Seoul Center, Korea Basic Science Institute)
Jeong, Eun-Kyung (Seoul Center, Korea Basic Science Institute)
Na, Yun-Cheol (Seoul Center, Korea Basic Science Institute)
Publication Information
Bulletin of the Korean Chemical Society / v.31, no.8, 2010 , pp. 2322-2328 More about this Journal
Abstract
A multiple solid-phase extraction (SPE) method was used with liquid chromatography, coupled with mass spectrometry (LC/MS), for the analysis of heterocyclic amines (HCAs) in human urine. Separation efficiencies based on the pH of the mobile phase and the types of columns were compared. An amide column showed better baseline separation and narrower HCA peak widths at pH 5.0 for the mobile phase than a $C_8$ column. Each SPE step, HLB, MCX, and HybridSPE, was optimized by controlling the pH conditions. The combined method with the three SPEs effectively removed interfering species that cause ion-suppression during HCA detection. Validation of the method, performed with SIM and SRM detection, showed correlation coefficients above 0.991 in the range 0.3 - 16.7 ng/mL. Recovery rates were 45.4 - 97.3% on the $C_8$ column and 71.8 - 101.4% on the amide column, and method detection limits were 0.11 - 0.65 ng/mL on the $C_8$ column and 0.12 - 0.48 ng/mL on the amide column. This method using multiple SPEs offers significant benefits for high-throughput determination of HCAs in urine.
Keywords
Heterocyclic amines; Urine; LC/MS; Solid-phase extraction;
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