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

作　　者：赖莺[1] 黄旖珏 黄宗平[1] 董清木[1] 林睿[1] 李彬[2] 涂星朋[1] 丁华军[1] 孙伟佳[1] 

机构地区：[1]厦门出入境检验检疫局技术中心,厦门361026 [2]深圳职业技术学院,深圳518055

出　　处：《分析试验室》2017年第8期881-885,共5页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划(2016YFF0203705);国家质检总局科研项目(2014IK160;2015IK186);福建省自然科学基金项目(2016J01072);厦门市科技计划项目(3502Z20164076);检疫检疫行业标准(2015B066)资助

摘　　要：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.

关 键 词：涂料 高关注物质 四溴双酚A 磷酸酯 超高效液相色谱-质谱法 

分 类 号：TQ041.7[化学工程]