高效液相色谱法测定塑料、橡胶制品中的偶氮二甲酰胺

Determination of Azodicarbonamide in Plastic and Rubber by High Performance Liquid Chromatography

建立了塑料、橡胶制品中偶氮二甲酰胺(ADA)的高效液相色谱测定方法。以体积分数2.5%二甲亚砜(DMSO)的丙酮为提取溶剂,采用配有紫外检测器的高效液相色谱仪进行测定,色谱柱为CN柱(4.6 mm×250 mm, 5μm),流动相为V(乙腈)∶V(20 mmol/L乙酸铵)=5∶95,等度洗脱,紫外检测波长为254 nm。当ADA质量浓度在0.1~100 mg/L时,其HPLC峰面积与其浓度呈良好的线性关系。ADA测定低限(S/N=10)为5.0 mg/kg,ADA的加标回收率为91.9%~99.6%,相对标准偏差为0.7%~4.0%。该方法准确、灵敏、快速、重复性好,满足塑料、橡胶制品中ADA定量分析的要求。

The analytical method for the determination of azodicarbonamide(ADA)in plastic and rubber samples by high performance liquid chromatography(HPLC)was established.ADA in plastic and rubber was ultrasonically extracted with dimethyl sulfoxide/acetone mixture(2.5∶97.5,V∶V),and determined by HPLC equipped with an ultraviolet(UV)detector.The compounds were separated on an CN column(4.6 mm×250 mm,5μm)with isocratic elution using acetonitrile/20 mmol/L ammonium acetate(5∶95,V∶V)as mobile phase,and the UV detection was at 254 nm.Results showed a good linear behavior in the ADA concentration range from 0.1 to 100 mg/L with a detection limit of 5.0 mg/kg.The spiked recoveries was 91.9%~99.6%and the relative standard deviation of ADA was in the range of 0.7%~4.0%.This method is sensitive,fast and simple with high accuracy and precision so that it can be used to determine ADA in plastic and rubber.