Determination of methyl isobutyl ketone in urine by headspace coupled with gas chromatography-mass spectrometry / 中华劳动卫生职业病杂志
Chinese Journal of Industrial Hygiene and Occupational Diseases
;
(12): 65-68, 2022.
Artículo
en Chino
| WPRIM
| ID: wpr-935746
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.
Texto completo:
Disponible
Índice:
WPRIM (Pacífico Occidental)
Asunto principal:
Cromatografía de Gases y Espectrometría de Masas
/
Metil n-Butil Cetona
Tipo de estudio:
Investigación cualitativa
Límite:
Humanos
Idioma:
Chino
Revista:
Chinese Journal of Industrial Hygiene and Occupational Diseases
Año:
2022
Tipo del documento:
Artículo
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