摘要
目的建立测定面膜中六溴环十二烷3种异构体的液相色谱质谱法。方法采用Kinetex C18反相色谱柱(100 mm×4.6 mm,2.6μm),流动相为甲醇/乙腈(50/50体积比)-5 mmol甲酸铵水溶液,采用梯度洗脱的方式,检测离子对640.6/78.9和640.6/80.9作为定性、定量离子对,流速0.6 ml/min,外标法定量测量。结果在此条件下六溴环十二烷在0.05~50.00 ng/ml范围内线性良好,检出限为0.01 ng/ml;不同类型的面膜中六溴环十二烷的平均回收率在85.8%~103.2%范围内。结论本方法操作简便,分离速度快,准确度高,检出限低,适合于面膜中六溴环十二烷的测定。
Objective To establish a method for determination of hexabromocyclododecane in face mask with liquid chromatography - tandem mass spectrometry. Methods Quantitative method was carried out for the analyte under the chromatographic separation on Kinetex C18 ( 100 mm × 4. 6 mm, 2. 6 μm) column with methanol/acetonitrile ( V : V = 50/50 ) - 5 mM NH4COOH water solution gradientelution. During the selected reaction monitoring mode,640. 6/78.9 and 640. 6/80. 9 transitions were detected, while the flow rate was 0. 6 ml/min. Results The detection limit of hexabromocyclododecane was 0.01 ng/ml,and the mean recovery was from 85.8% to 103.2%. Conclusion This method is operated easily, and has a fast separate rate,low LOQ, as well as can be applied for the determination of hexabromocyclododecane in face mask.
出处
《中国卫生工程学》
CAS
2013年第2期157-159,共3页
Chinese Journal of Public Health Engineering
关键词
面膜
六溴环十二烷
同分异构体
液相质谱法
Face mask
Hexabromocyelododecane diastereoisomers
Chromatography - tandem mass spectrometry