Determination of methyl isobutyl ketone in urine by headspace coupled with gas chromatography-mass spectrometry.
10.3760/cma.j.cn121094-20201130-00658
- Author:
Hai Peng YE
1
;
Ji SHAO
1
;
Si Wei TAN
1
;
Yan Peng SHI
1
;
Ke Wen SU
1
;
Ling ZHANG
1
Author Information
1. Department of Sanitary Analysis, Hangzhou Occupational Disease Prevention and Control Hospital, Hangzhou 310014, China.
- Publication Type:Journal Article
- Keywords:
Gas Chromatography-mass spectrometry;
Headspace;
Methyl isobutyl ketone;
Urine
- MeSH:
Gas Chromatography-Mass Spectrometry;
Humans;
Methyl n-Butyl Ketone
- From:
Chinese Journal of Industrial Hygiene and Occupational Diseases
2022;40(1):65-68
- CountryChina
- Language:Chinese
-
Abstract:
Objective: To establish a method for the determination of methyl isobutyl ketone (MIBK) in urine samples by headspace-gas chromatography-mass spectrometry. Methods: Automatic headspace sampling technique was adopted to optimize the headspace conditions (headspace bottle heating temperature and equilibration time) and gas chromatographic conditions. A total of 5 ml samples were taken and added with 3.0 g ammonium sulfate into a 20 ml headspace bottle. After heated at 60 ℃ for 30 mins, gas from the upper part of headspace bottle was injected into gas chromatography with an injection volume of 100 μl. The target was separated by HP-5MS UI (30 m×0.25 mm×0.25 μm) capillary column and then detected by mass spectrometry detector. The retention time and external standard method were used for qualitative and quantitative analysis of MIBK in samples, respectively. Results: The standard curve of MIBK showed significant linearity between 20.0-1 000.0 μg/L. The standard curve was y=62.9x-652.5, and the correlation coefficient r=0.9998. The detection limit of MIBK was 5.0 μg/L and the quantification limit of MIBK was 16.0 μg/L. The average recovery rate was 95.3%~100.2% at three spiked concentrations of low (50.0 μg/L) , medium (200.0 μg/L) and high (500.0 μg/L) . The intra-day and inter-day precisions were 1.7%~3.8% (n=6) and 1.2%~4.0% (n=6) respectively. This method was stable for the determination of MIBK, and the urine could be kept 14 d at -20 ℃ without significantly loss. Conclusion: This method is proved to be simple, practical and highly sensitive. It can satisfy the request for the determination of urine samples of workers exposed to MIBK.
