摘要
建立了一种加速溶剂萃取-气相色谱-质谱法测定塑料中三-(2-氯乙基)磷酸酯(TCEP)、三-(2-氯丙基)磷酸酯(TCPP)、三-(2,3-二氯丙基)磷酸酯(TDCP)、磷酸三苯酯(TPh P)、三-(邻甲苯基)磷酸酯(To CP)、三-(间甲苯基)磷酸酯(Tm CP)和三-(对甲苯基)磷酸酯(Tp CP)7种有机磷酸酯阻燃剂和增塑剂的分析方法。以甲苯为溶剂,采用加速溶剂萃取方式提取样品中7种有机磷酸酯阻燃剂和增塑剂,外标法定量,GC-MS分析。TCEP,TCPP,TDCP,TPh P,To CP,Tm CP和Tp CP的线性范围均为0.5~10 mg/L(R2≥0.998),检出限(S/N>3)分别为0.1,0.035,0.045,0.1,0.1,0.1和0.1 mg/kg。塑料制品中TCEP,TCPP,TDCP,TPh P,To CP,Tm CP和Tp CP在3个添加浓度水平的加标回收率范围在85.4%~110.6%;相对标准偏差(RSD,n=5)小于5.0%。方法已应用于塑料制品中上述7种有机磷酸酯阻燃剂和增塑剂的测定。
A method for determination of tris (2-chloroethyl) phosphate ( TCEP), tris ( 2-chloro - 1- methylethyl) phosphate (TCPP), tris- (1,3-dichloropropyl) phosphate (TDCP), triphenyl phosphate (TPhP), tri-o-cresyl phosphate (ToCP), tri-m-cresyl phosphate (TmCP), and tri-p-cresyl phosphate (TpCP) in plastic products by accelerated solvent extraction-gas chromatography-mass spectrometry has been developed. Toluene as an extraction solvent and accelerated solvent extraction as an extraction method have been adopted. The quantification was performed with external standard. There was a linear correlation between peak area and the concentration of each organophosphate ester flame retardants and plasticizers in the range of 0. 1 - 5 mg/L (R^2≥ 0. 998 ). The limits of determination (LODs) (S/N 〉3) for TCEP, TCPP, TDCP, TPhP, ToCP, TmCP and TpCP were 0. 1, 0. 035, 0. 045, 0. 1, 0. 1, 0. 1 and 0. 1 mg/kg, respectively. The recoveries of TCEP, TCPP, TDCP, TPhP, ToCP, TmCP and TpCP spiked in plastic sample at different levels were from 85.4% to 110. 6% ; the repeatabilities of peak areas for 7 organophosphate ester flame retardants and plasticizers were less than 5.0% ( RSD, n = 5 ). The seven organophosphate ester flame retardants and plasticizers in plastic products have been determined by the proposed method.
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第1期109-113,共5页
Chinese Journal of Analysis Laboratory
关键词
有机磷酸酯阻燃剂和增塑剂
气相色谱-质谱
加速溶剂萃取
Organophosphate ester flame retardants and plasticizers
Gas chromatography-mass spectrometry
Accelerated solvent extraction