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建立了涂料中四溴双酚A(TBBPA)和磷酸三(1,3-二氯-2-丙基)酯(TDCPP)测定的超高效液相色谱-质谱检测方法。水基型涂料采用乙酸乙酯超声萃取,通过氮吹将溶剂置换为乙腈,溶剂型涂料直接用乙腈超声萃取。提取液经过滤后,选择苯基修饰的C18柱梯度洗脱排除基体干扰。结果表明待测物质在2个数量级浓度范围内呈良好的线性关系。方法定量限(S/N=10)为0.05~1 mg/kg。三水平的添加回收率介于84.4%~103.1%之间,相对标准偏差(n=6)在5%以内。方法选择性好,灵敏度、回收率高,能满足实际工作的要求。
A ultra performance liquid chromatography-mass spectrometry method for the determination of TBBPA and TDCPP was established. Water-based coatings were extracted with ethyl acetate by ultrasonic, the solvent was replaced with acetonitrile by nitrogen blowing, and the solvent-borne coatings were directly extracted with acetonitrile. The extract was filtered, select the phenyl-modified C18 column gradient elution matrix interference. The results show that the test substance has a good linear relationship in the concentration range of two orders of magnitude. The limit of quantification (S / N = 10) was 0.05-1 mg / kg. The recoveries of three levels ranged from 84.4% to 103.1%, and the relative standard deviations (n = 6) were within 5%. The method has good selectivity, high sensitivity and high recovery rate, which can meet the requirements of practical work.