固相萃取-气相色谱-质谱法测定柳树皮中卤代阻燃剂

Determination of Halogenated Flame Retardants in Willow Bark by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

建立了固相萃取-气相色谱-负化学电离源-质谱（GC-NCI-MS）法同时测定柳树皮中四溴对二甲苯（pTBX）,五溴苯（PBBz）,五溴甲苯（PBT）,五溴乙苯（PBEB）,六溴苯（HBB）,顺式双（六氯环戊二烯）环辛烷（s-DP）,反式双（六氯环戊二烯）环辛烷（a-DP）和多溴联苯醚（PBDEs）的方法.树皮样品经过正己烷-丙酮（1∶1,V/V）索氏提取24 h后,利用硅胶/氧化铝柱净化,并用正己烷-二氯甲烷（3∶7,V/V）混合溶液作为淋洗液.结果表明,各卤代阻燃剂树皮基质加标回收率为76.2％～92.3％,检出限在0.1～5.0 ng/g脂肪.13C6-HBB,13 C12-BDE-139和13C10-S-DP的加标回收率为75.6％±2.2％,77.3％±3.4％,76.0％±2.8％.应用本方法测定柳树皮样品中卤代阻燃剂的含量,pTBX,PBT,PBBz,HBB,s-DP,a-DP和PBDEs在所有样品中均有检出,而PBEB的检出率则为16.7％.

A solid phase extraction-gas chromatography-negative chemical ionization-mass spectrometric method was developed for the simultaneous determination of 2, 3,5, 6-tetrabromo-P-xylene （pTBX）, 1,2,3,4,5-pentabromobenzene （ PBBz ）, Pentabromotoluene （ PBT）, 2,3,5,5,6-pentabromoethylbenzene （PBEB）, Hexabromobenzene （ HBB ）, sys-Dechlorane Plus （ s-DP ） , anti-Dechlorane Plus （a-DP） and polybrominated diphenyl ethers （PBDEs） . Willow bark samples were extracted with hexane-acetone （ 1 ： 1, V/V） for 24 h by Soxhlet extraction apparatus and cleaned with a silica/alumina column, which was eluted by hexane：dichloromethane （3：7）. Recoveries in the matrix ranged from 76.2% to 92.3%, and limits of detection were from 0.1 to 5.0 ng/g lipid. Recoveries of 13C6-HBB, 13Ca2-BDE-139 and 13C10-s-DP in the samples were 75.6% _＋2.2% , 77.3% _＋3.4% and 76.0% ＋2.8% , respectively, pTBX, PBT, PBBz, HBB, s-DP, a-DP and PBDEs were detected in all bark samples, while the detection rate of PBEB was 16.7%.