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    高效液相色谱法测定塑胶跑道中3,3'-二氯-4,4'-二氨基二苯甲烷的残留量

    Determination of Residual Amounts of 3,3'-Dichloro-4,4'-diaminodiphenylmethane in Plastic Track by High Performance Liquid Chromatography

    • 摘要: 将塑胶跑道样品加工粉碎至粒径在0.85~1.40 mm之间,称取此样品0.500 0 g,用丙酮10 mL浸润并超声提取60 min,收集萃取液,将其蒸发浓缩至近干,并用氮气吹干,加入甲醇1.0 mL溶解残渣。溶液经0.22 μm滤膜过滤后,按高效液相色谱仪的仪器条件测定滤液中3,3'-二氯-4,4'-二氨基二苯甲烷(MOCA)的含量。色谱分离中用C18反相色谱柱为固定相,以水(A)和甲醇(B)按不同比例混合作为流动相进行梯度淋洗,洗脱液中MOCA在波长245 nm条件下用二极管阵列检测器检测。结果表明:MOCA的质量浓度在1.0~50.0 mg·L-1内与相应的峰面积之间呈线性关系,其检出限(3S/N)为1.0 mg·kg-1。在2.50,10.0,100 mg·kg-1等3种浓度水平上进行加标回收试验,测得回收率在86.4%~92.3%之间,测定值的相对标准偏差(n=6)在3.2%~4.2%之间。

       

      Abstract: The plastic track sample was made to small particles with sizes ranging between 0.85 mm and 1.40 mm by any of those ready methods. A portion (0.500 0 g) of the crushed sample was taken and extracted ultrasonically with 10 mL of acetone for 60 min. The extract was collected and evaporated to near dryness and then to dryness by N2-blowing. The residue was taken up with 1.0 mL of methanol, and the solution was filtered through 0.22 μm filtering membrane. The filtrate was used for HPLC determination of the content of 3,3'-dichloro-4,4'-diaminodiphenylmethane (MOCA). In HPLC separation, C18 reverse phase chromatographic column was used as stationary phase, and mixtures of water (A) and methanol (B) in various ratios were used as mobile phases in the gradient elution. MOCA in the eluate was detected by diode array detector at the wavelength of 245 nm. Linear relationship between values of peak areas and the respective mass concentrations of MOCA was found in the range from 1.0 to 50.0 mg·L-1, with detection limit (3S/N) of 1.0 mg·kg-1. Test for recovery was made by standard addition method at 3 concentration levels of 2.50, 10.0 and 100 mg·kg-1, giving results of recovery in the range of 86.4%-92.3%, and RSDs (n=6) ranged from 3.2% to 4.2%.

       

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