Kubota Ryuichi, Endo Yoko, Takeuchi Akito, Inoue Yoshinori, Ogata Hiroko, Ogawa Masanori, Nakagawa Tomoo, Onda Nobuhiko, Endo Ginji
Research Center for Occupational Poisoning, Tokyo Rosai Hospital, Japan Labour Health Organization, 4-13-21 Ohmori-Minami, Ota-ku, Tokyo 143-0013, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jul 1;854(1-2):204-10. doi: 10.1016/j.jchromb.2007.04.022. Epub 2007 Apr 25.
An analytical method using a combination of solid-phase extraction (SPE) and gas chromatography with a flame thermionic detector (GC/FTD) was developed for determination of N-methyl-2-pyrrolidone (NMP), N-methylsuccinimide (MSI), and 2-hydroxy-N-methylsuccinimide (2-HMSI) in human urine. The SPE cartridge of poly(divinylbenzene/hydroxymethacrylate) used was directly loaded with urine sample, followed by elution with methyl isobutyl ketone (MIBK) and subsequent centrifugation, and the supernatant was injected into the capillary GC using a DB1701. This method allowed efficient separation of NMP, MSI, and 2-HMSI, which were nearly free of interference by other GC peaks arising from urine. Recoveries of NMP, MSI, and 2-HMSI from the SPE cartridge were about 98, 101, and 67%, respectively, with limits of detection of 0.04, 0.02, and 0.06 mg/L, respectively, which met the regulatory requirements. The present method was used for assay in biological monitoring of workers exposed to NMP in their occupational environment.
开发了一种结合固相萃取（SPE）和带火焰热离子检测器的气相色谱法（GC/FTD）的分析方法，用于测定人尿中的N-甲基-2-吡咯烷酮（NMP）、N-甲基琥珀酰亚胺（MSI）和2-羟基-N-甲基琥珀酰亚胺（2-HMSI）。所用的聚（二乙烯基苯/甲基丙烯酸羟乙酯）固相萃取柱直接加载尿液样本，随后用甲基异丁基酮（MIBK）洗脱并进行离心，上清液使用DB1701毛细管气相色谱仪进样。该方法能有效分离NMP、MSI和2-HMSI，几乎不受尿液中其他气相色谱峰的干扰。NMP、MSI和2-HMSI从固相萃取柱的回收率分别约为98%、101%和67%，检测限分别为0.04、0.02和0.06 mg/L，均符合监管要求。该方法用于职业环境中接触NMP的工人的生物监测分析。
