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深圳海关工业品检测技术中心,广东 深圳 518067
张伟亚,博士,研究员,研究方向:石油化工等大宗资源商品检测鉴定,E-mail:zwyciq@163.com
收稿日期:2024-12-17,
修回日期:2025-01-14,
录用日期:2025-01-15,
纸质出版日期:2025-03-15
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王昱霞,张伟亚,陈向阳,李成发,陈国峰.气相色谱-质谱联用法测定润滑油中N-甲基吡咯烷酮残留量[J].分析测试学报,2025,44(03):486-492.
WANG Yu-xia,ZHANG Wei-ya,CHEN Xiang-yang,LI Cheng-fa,CHEN Guo-feng.Determination of N-Methyl-2-pyrrolidone Residue in Lubricating Oil by Gas Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(03):486-492.
王昱霞,张伟亚,陈向阳,李成发,陈国峰.气相色谱-质谱联用法测定润滑油中N-甲基吡咯烷酮残留量[J].分析测试学报,2025,44(03):486-492. DOI: 10.12452/j.fxcsxb.24121717.
WANG Yu-xia,ZHANG Wei-ya,CHEN Xiang-yang,LI Cheng-fa,CHEN Guo-feng.Determination of N-Methyl-2-pyrrolidone Residue in Lubricating Oil by Gas Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(03):486-492. DOI: 10.12452/j.fxcsxb.24121717.
建立了气相色谱-质谱联用(GC-MS)测定润滑油中N-甲基吡咯烷酮(NMP)残留量的方法。润滑油样品采用叔丁基甲醚溶解,加入乙腈将润滑油沉淀,目标物N-甲基吡咯烷酮保留在上清液中。采用气相色谱-质谱法测定上清液,外标法定量。结果表明,N-甲基吡咯烷酮在0.5~50.0 mg/L范围内线性关系良好,方法检出限为8.0 mg/kg,定量下限为20.0 mg/kg。在20、100、200 mg/kg 3个加标水平下,不同种类润滑油中N-甲基吡咯烷酮的回收率为96.2%~108%,相对标准偏差(RSD)为0.99%~4.5%。该方法简单快速、灵敏度高、准确度好,可应用于润滑油中N-甲基吡咯烷酮的测定。
A method for the determination of N-methyl-2-pyrrolidone(NMP) residues in lubricating oil using gas chromatography-mass spectrometry(GC-MS) has been established. Lubricating oil samples were dissolved in tert-butyl methyl ether,and then precipitated by adding acetonitrile. The target substance NMP was retained in the supernatant and determined by gas chromatography-mass spectrometry with external standard method for quantification. Results showed that NMP had a good linear relationship in the range of 0.5 mg/L to 50.0 mg/L,the detection limit was 8.0 mg/kg,and the quantitation limit was 20.0 mg/kg. At three spiked levels of 20 mg/kg,100 mg/kg and 200 mg/kg,the recoveries of NMP in different types of lubricating oils were between 96.2% and 108%,with relative standard deviations(RSDs) ranging from 0.99% to 4.5%. The method is quick,easy,accurate and sensitive,which is suitable for determination of NMP in lubricating oil.
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United States Environmental Protection Agency . Final Risk Evaluation for n-Methylpyrrolidone(NMP) . [ 2024-08-29 ]. https://www.epa.gov/assessing-and-managing-chemicals-under-tsca/final-risk-evaluation-n-methylpyrrolidone-nmp https://www.epa.gov/assessing-and-managing-chemicals-under-tsca/final-risk-evaluation-n-methylpyrrolidone-nmp .
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