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在线还原后荧光检测生物样品中1-硝基芘及其代谢物的色谱测定方法

Chromatographic determination method for 1-nitropyrene and its metabolites in biological samples with fluorescence detection after on-line reduction.

作者信息

Hayakawa K, Terai N, Suzuki K, Dinning P G, Yamada M, Miyazaki M

机构信息

Faculty of Pharmaceutical Sciences, Kanazawa Univeristy, Japan.

出版信息

Biomed Chromatogr. 1993 Sep-Oct;7(5):262-6. doi: 10.1002/bmc.1130070505.

DOI:10.1002/bmc.1130070505
PMID:8305856
Abstract

A high performance liquid chromatographic (HPLC) method with fluorescence detection after on-line reduction for the determination of 1-nitropyrene (NP), 1-nitrosopyrene (NSP), 1-aminopyrene (AP) and N-acetylaminopyrene (AAP) has been developed. The reduction efficiency of NP and NSP on a zinc column was found to be higher than that of an electrochemical reducer. Using a HPLC system equipped with a zinc column (4.0 mm i.d. x 10 mm) and an imidazole/HClO4 (pH 6.8): acetonitrile mobile phase, detection limits (S/N = 3) of 20-30 fmol for NP, NSP and AP and 350 fmol for AAP were obtained. NP, NSP and AP were determined in the incubation mixture of NP and Salmonella typhimurium, YG1021, by this method. Time course studies showed that a large ratio of NP was metabolized in the pre-incubation step of the Ames test.

摘要

已开发出一种高效液相色谱(HPLC)方法,该方法通过在线还原后进行荧光检测来测定1-硝基芘(NP)、1-亚硝基芘(NSP)、1-氨基芘(AP)和N-乙酰氨基芘(AAP)。发现NP和NSP在锌柱上的还原效率高于电化学还原剂。使用配备锌柱(内径4.0 mm×10 mm)和咪唑/高氯酸(pH 6.8):乙腈流动相的HPLC系统,NP、NSP和AP的检测限(S/N = 3)为20 - 30 fmol,AAP的检测限为350 fmol。通过该方法测定了NP与鼠伤寒沙门氏菌YG1021的孵育混合物中的NP、NSP和AP。时间进程研究表明,在艾姆斯试验的预孵育步骤中,很大比例的NP被代谢。

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