超高效液相色谱-质谱法测定涂料中四溴双酚A和磷酸三(1,3-二氯-2-丙基)酯

Determination of tetrabromobisphenol A and tris (1,3-dichloroisopropyl) phosphate in coatings by UPLC-MS

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 reliable Ultra Performance Liquid Chromatography-mass Spectrometer（ UPLC-MS）method was developed for the simultaneous determination of tetrabromobisphenol A（ TBBPA） and tris（ 1,3-dichloroisopropyl） phosphate（ TDCPP） in coatings. Water-based coatings were ultrasonic extracted with acetate,and then the solvent was replaced with acetonitrile by nitrogen sweeping.Organic solvent-based coatings were directly ultrasonic extracted with acetonitrile. Matrix interference of the filtered extracts was eliminated by gradient elution on a C18 column modified with phenyl.Results showed that the calibration curves were linear within 2 orders of magnitude. The limits of quantification of the method were between 0. 05 to 1 mg/kg. The recoveries ranged from 84. 4% -103. 1% with 3 addition levels,and RSDs were within 5%. The selectivity,sensitivity and recovery of the method can fully meet the requirements of practical work.