超声辅助-固相萃取-GC-MS法测定儿童化妆品中TBP,TCEP,TCPP和TDCPP  

Determination of TBP, TCEP, TCPP and TDCPP in children’s cosmetics by ultrasound-assisted solid phase extraction-GC-MS

作　　者：徐春丽 贾振福[1] 邱会东[1] 刘恩余 黄瑶瑶 苏小东[1] Chunli Xu;Zhenfu Jia;Huidong Qiu;Enyu Liu;Yaoyao Huang;Xiaodong Su(Department of Chemistry and Chemical Engineer,Chongqing University of Science and Technology,Chongqing 401331,China)

机构地区：[1]重庆科技学院化学化工学院,重庆401331

出　　处：《日用化学工业》2022年第5期572-576,共5页China Surfactant Detergent & Cosmetics

基　　金：重庆市社会民生科技创新专项:儿童化妆品中多种有机磷酸酯类物质的检测技术研究;重庆科技学院生活垃圾资源化处理省部共建协同创新中心资助项目(shljzyh2021-08)。

摘　　要：基于超声辅助溶剂萃取技术结合气相色谱-质谱联用建立了儿童化妆品中TBP,TCEP,TCPP和TDCPP 4种有机磷酸酯阻燃剂(Organophosphate Flame Retardants, OPFRs)的测定方法。优化了萃取剂种类、超声时间、溶剂用量、洗脱剂种类、洗脱剂用量、固相萃取柱类型、色谱条件等条件。结果表明,在优化条件下TCPP与TBP的质量浓度在0.002~20 mg/L、TDCPP与TCEP质量浓度在0.004~30 mg/L范围内,分别与其对应的峰面积成良好的线性关系,相关系数R2>0.998。利用该方法测定了国产和进口儿童化妆品中4种有机磷酸酯的含量,不含阻燃剂的空白基质中4种OPFRs在3个不同添加水平(500,2 500和5 000 ng/g)的加标回收率在101.7%~119.0%之间,相对标准偏差在2.5%~8.4%之间。该方法操作简单、灵敏度高、准确度好,可用于儿童化妆品中4种有机磷酸酯阻燃剂的同时测定。An effective method for the determination of tributyl phosphate( tbp), tris( 2-chloroethyl) phosphate( tcep), tris( 1-chloro-2-propyl) phosphate( tcpp) and tris(2, 3-dichloropropyl) phosphate( tdcpp) in children’s cosmetics was established based on ultrasonic assisted solvent extraction followed by gas chromatography-mass spectrometry. The conditions of extractant solvent, ultrasonic time, eluent type, eluent dosage, solid phase extraction column and chromatographic conditions were optimized. The optimal conditions were as follows: extraction solvent: acetonitrile;purification column: Florisil;extraction time: 20 min;eluent: acetonitrile. The results show that under the optimized conditions, the mass concentrations of TCPP and TBP are in the range of 0.002-20 mg/L and the mass concentrations of TDCPP and TCEP are in the range of 0.004-30 mg/L, which have a good linear relationship with their corresponding peak areas, and the correlation coefficient R2 is greater than 0.998. The contents of four organic phosphates in domestic and imported children’s cosmetics are determined by this method. The recoveries of four organic phosphate flame retardants in blank matrix at three different addition levels( 500, 2 500 and 5 000 ng/g) are varied from 101.7% to 119.0% with the relative standard deviations of 2.5%-8.4%. The method is simple, sensitive and accurate, and can be used for the simultaneous determination of four organic phosphate flame retardants in children’s cosmetics.

关 键 词：儿童化妆品 有机磷酸酯 气相色谱-质谱 检测 

分 类 号：TQ658[化学工程—精细化工]