超声提取-固相萃取-GC-MS/MS测定灰尘中10种有机磷阻燃剂

Determination of 10 organophosphate flame retardants in dust by ultrasonic extraction and solid phase extraction coupled with GC-MS/MS

基于超声提取和固相萃取技术建立了灰尘样品中10种有机磷阻燃剂(OPFRs)的前处理方法,采用气相色谱串联三重四级杆质谱法进行定性定量分析。优化了超声提取的溶剂种类及用量、时间、频率、温度以及固相萃取的活化与洗脱溶剂的种类和用量等条件。优化实验条件下,10种OPFRs在相应浓度范围内线性良好,相关系数R为0.999 0~0.999 8。检出限(S/N=3)为0.44~11.08 ng/g。灰尘样品平均加标回收率为51.4%~123.5%,RSD为3.0%~13.7%。该方法操作简单、灵敏度高、检出限低,适用于灰尘样品中多种有机磷阻燃剂的同时测定。

An effective method is established for the simultaneous determination of ten organophosphate flame retardants（OPFRs） in dust by triple quadrupole gas chromatography-mass spectrometer（GC-MS/MS） combined with ultrasonic extraction（UE） and solid phase extraction（SPE）.The conditions of UE and SPE,such as variety and dosage of solvents,temperature,frequency and time are optimized. Under the optimized experimental conditions,good linearities of ten OPFRs can be achieved when the analytes are in the corresponding concentration range,with correlation coefficients（R） ranging from 0. 999 0 to 0. 999 8.The detection limits（S/N = 3） of these 10 OPFRs range from 0. 44 to11. 08 ng·g-1. The average recoveries of 10 OPFRs in dust at three spiked concentration levels range from 51. 4% to123. 5% with RSD less than 13. 7%.The proposed method has the characteristics of simple operation,high sensitivity and low detection limit,which makes it suitable for the detection of varies OPFRs in dust.