全二维气相色谱串联质谱法测定全血中萘烷及其代谢产物

Development of a comprehensive two-dimensional gas chromatography-mass spectrometry for determination of naphthene and its metabolites in whole blood samples

目的建立全血中萘烷及其代谢产物(萘烷醇、萘烷酮)的全二维气相色谱检测方法。方法全血经环己烷提取、固相萃取柱净化后,采用Rxi-5Sil MS作一维柱、DB-17 MS作二维柱进行分离,质谱仪检测,以外标法定量。结果萘烷及其代谢产物萘烷醇、萘烷酮在二维谱图上有效分离,检出限为7~9μg/L,定量限为19~27μg/L,在0~5μg/mL范围内线性关系良好(r>0.999)。血液样本平均加标回收率为96.4%~102.8%,相对标准偏差(RSD)为3.1%~5.9%。结论建立的方法简便灵敏,分离度好,回收率高,适用于血液样本中萘烷及其代谢产物的检测。

Objective To develop a comprehensive two-dimensional gas chromatography assay for determination of naphthene and its metabolites(naphthanol and naphthanone)in whole blood samples.Methods Following cyclohexane extraction and cleaning with solid-phase extraction columns,whole blood samples were separated with one-dimensional Rxi-5Sil MS columns and two-dimensional DB-17 MS columns.Mass spectrometry was performed and qualitative analysis was performed with the external standard method.Results Naphthene and its metabolites naphthanol and naphthanone were effectively separated on two-dimensional spectra,with 7 to 9μg/L limits of detection and 19 to 27μg/L limits of quantitation,and the comprehensive two-dimensional gas chromatography-mass spectrom-etry showed a good linear relationship at mass concentrations of 0 to 5μg/mL(r>0.999).The mean spiked recovery of blood samples was 96.4%to 102.8%,with relative standard deviations of 3.1%to 5.9%.Conclusions sThe developed comprehensive two-dimensional gas chromatography-mass spectrometry is simple,sensitive,and high in separation and recovery,which is feasible for deter-mination of naphthene and its metabolites in whole blood samples.