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
The method of determination for 2,3-Butanedione in the air of workplace by high performance liquid chromatography with derivatization
叶海朋 1傅红 1邵吉 1单晓月 1张玲 1张磊1
作者信息
- 1. 杭州市职业病防治院卫生检测科,杭州 310014
- 折叠
摘要
目的 建立磷酸溶液采集、衍生化-高效液相色谱法测定工作场所空气中2,3-丁二酮(简称丁二酮).方法 于2022年10月,用多孔玻板吸收管盛装0.01％的磷酸溶液10 ml,以0.2 L/min流量采集工作场所空气中丁二酮,吸收液经2,4-二硝基苯肼衍生化75 min,SB-C18色谱柱(250 mm×4.6 mm,5 μm)分离,在30℃柱温下,用乙腈-水(V∶V,1∶1)混合液作流动相,以1.0 ml/min的流速洗脱,紫外检测器(λ=365 nm)检测,保留时间定性,外标法定量.结果 本方法中丁二酮的磷酸溶液吸收样在4 ℃下可保存7 d,在0.05～6.00 μg/ml范围内线性关系良好,线性回归方程为y=89.610x+0.133,r=0.999 9,采样效率为98.33％～100.00％,方法的检出限为0.005 μg/ml,最低检出浓度为0.016 mg/m3(以V0=3.0 L计),方法回收率为95.96％～102.44％,批内精密度为4.36％～7.78％,批间精密度为4.96％～6.06％.结论 本方法简单实用,准确度好,灵敏度高,可防止丁二酮损失降解,可用于工作场所空气中丁二酮的检测.
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 for75 min and separated on a SB-C18 column(250 mmx4.6 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=89.610x+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/m3(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.
关键词
工作场所/空气/2,3-丁二酮/衍生化/高效液相色谱法Key words
Workplace/Air/2,3-Butanedione/Derivatization/High performance liquid chromatography引用本文复制引用
出版年
2024
NETL
NSTL
万方数据