摘要
目的建立工作场所空气中氨基氰测定的高效液相色谱法。方法工作场所空气样品以水溶液作吸收液，用冲击式吸收管，以2．8—3．0ml／min速度采集60min，以丹磺酰氯为衍生试剂，进行柱前衍生，衍生方法为待测样品中加入2．5ml丙酮溶液，1．0ml含0．016mol／L碳酸钠和0．184mol／L碳酸氢钠混合溶液，0．5ml丹磺酰氯丙酮溶液（浓度为10mg／m1），50oC水浴中反应1h。经色谱柱250mm×4．6mm×5μm，ODS（C18）分离；流动相为乙腈一磷酸盐缓冲液（35：65）；流速：1．0ml／min，柱温25℃；荧光检测器检测，激发波长360nm，发射波长495nm。结果本法最低检出浓度为O．05μg／ml，当氨基氰浓度为0．2～100．0μg／ml呈良好线性关系，日内相对标准偏差0．28％-1．18％，日间相对标准偏差0．22％-2．16％；回收率95．7％-103．0％，采样效率为95．8％～96．9％。在避光条件下，氨基氰水溶液（pH〈6．5）常温可稳定7d。结论本方法稳定，可靠，操作方便，灵敏度高。适用于工作场所空气中氨基氰的测定。
Objective To establish a method for determining cyanamide in workplace air by high- performance liquid chromatography （HPLC）. Methods Air samples were collected from the workplace using the shock absorption tube containing water solution at a rate of 2.8-3.0 ml/min for 60 min; dansyl chloride was used as a derivatization reagent to conduct pre-column derivatization, and the procedure was as follows： acetone solution （2.5 ml）, mixed solution （1.0 ml） containing 0.016 mol/L Na2CO3 and 0.184 mol]L NaHCO3, and 10 mg/ml acetone solution of dansyl chloride （0.5 ml） were added into the samples, and reaction proceeded in a water bath （50 ℃） for 1 h. HPLC was performed on an ODS C18 column （250 mm × 4.6 mm, 5 μm） with a mobile phase of acetonitrile-phosphate buffer （35：65 ） at a flow rate of 1.0 ml/min and a column temperature of 25℃; a fluorescence detector was used at an excitation wavelength of 360 nm and an emission wavelength of 495 nm. Results The minimum detectable concentration of cyanamide was 0.05 μg/ml; a good linear relationship was noted when the concentration of cyanamide was 0.2-100.0 μg/ml; the intraday relative standard deviation （RSD） was 0.28%-1.18%, and the interday RSD was 0.22-2.16%; the recovery rate was 95.7%- 103.0%, and the sampling efficiency was 95.8%-96.9%. Water solution of cyanamide （pH〈6.5） could be stable in the dark at room temperature for 7 d. Conclusion This method is stable, reliable, easy to operate, and highly sensitive and suitable for determination of cyanamide in workplace air.
出处
《中华劳动卫生职业病杂志》
CAS
CSCD
北大核心
2014年第1期72-74,共3页
Chinese Journal of Industrial Hygiene and Occupational Diseases
基金
国家十五科技攻关专项课题（2002BA06A6B-2）
关键词
工作场所
氨基氰
色谱法
高效液相
Workplace
Cyanamide
High-performance liquid chromatography
