The method of determination for 2, 3-Butanedione in the air of workplace by high performance liquid chromatography with derivatization
10.3760/cma.j.cn121094-20221201-00574
- VernacularTitle:工作场所空气中2，3-丁二酮测定的衍生化-高效液相色谱法
- Author:
Haipeng YE
1
;
Hong FU
;
Ji SHAO
;
Xiaoyue SHAN
;
Ling ZHANG
;
Lei ZHANG
Author Information
1. 杭州市职业病防治院卫生检测科，杭州 310014
- Keywords:
Workplace;
Air;
2, 3-Butanedione;
Derivatization;
High performance liquid chromatography
- From:
Chinese Journal of Industrial Hygiene and Occupational Diseases
2024;42(2):129-132
- CountryChina
- Language:Chinese
-
Abstract:
Objective:To establish a method for the determination of 2, 3-Butanedione (BUT) in the air of workplace, which including the process of collection by absorption in phosphoric acid aqueous solution and the process of analysis and detection by high performance liquid chromatography with derivatization.Methods:In October 2022, a porous glass plate absorption tube containing 10 ml of 0.01% phosphoric acid solution was used to collect BUT in the air of the workplace at a flow rate of 0.2 L/min. The absorption solution was derived by 2, 4-dinitrophenylhydrazine for 75 min and separated on a SB-C18 column (250 mm×4.6 mm, 5 μm) . At the column temperature of 30 ℃, the mixture of acetonitrile-water ( V∶ V, 1∶1) was eluted at the flow rate of 1.0 ml/min. It was detected by UV detector (λ=365 nm) , qualitatived by retention time and quantitatived by external standard. Results:It showed that BUT in phosphoric acid aqueous solution could be stored for at least 7 d at 4 ℃. There was a linear relationship within the determination range of 0.05-6.00 μg/ml, the linear regression equation was y=89.610 x+0.133, r=0.9999. The sampling absorption efficiencies were 98.33%-100.00%, the detection limit of the method was 0.005 μg/ml, the minimum detection concentration was 0.016 mg/m 3 (based on V0=3.0 L) . The recovery rates were 95.96%-102.44%, the intra batch precision were 4.36%-7.78%, and the inter batch precision were 4.96%-6.06%. Conclusion:The method has the advantages of simple operation, high sensitivity and good accuracy. It can prevent the loss and degradation of BUT. It can be used for the determination of BUT in the air of workplace.
