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Abstract: A novel method for the analysis of (3-hydroxypropyl)mercapturic acid (HPMA), a major acrolein metabolite in human urine incorporating a molecularly imprinted solid-phase extraction (MISPE) process using N-acetylcysteine-imprinted mesoporous silica particles coupled with LC-MS/MS detection was developed. The molecularly imprinted mesoporous silica particles were synthesized based on the supported material of ordered mesoporous silica SBA-15 with N-acetylcysteine (NAC) as template using surface molecular imprinting technology. The condition of MISPE procedures was optimized. The use of MISPE improved the accuracy and precision of the LC-MS method and lowered the limit of detection (0.23 ng/mL). The recoveries at three spiked levels ranged between 88.5% to 108.6%. The developed MISPE method enabled the selective extraction of HPMA successfully in human urine and could be used as an effective approach for the determination of ultra-trace HPMA in complex biological matrices. The results in real samples showed that median levels of HPMA were significantly higher (1922.0 ng/mg of creatinine, N = 75) in smokers than in nonsmokers (759.1 ng/mg of creatinine, N = 5), demonstrating the higher acrolein uptake in smokers than in nonsmokers
Template and target information: N-acetylcysteine, NAC, (3-hydroxypropyl)mercapturic acid, HPMA
Author keywords: 3-Hydroxypropylmercapturic acid, Acrolein, Molecularly imprinted mesoporous silica polymers, Solid-phase extraction, liquid chromatography tandem mass spectrometry