液液萃取-固相萃取-气质联用测定指甲中的多溴联苯醚与多氯联苯

Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in nails by liquid-liquid extraction, solid phase extraction, and GC-MS

利用液液萃取(LLE)与固相萃取法(SPE)提取和净化人体指甲中的多溴联苯醚(PBDEs)和多氯联苯(PCBs),经浓硫酸除脂后,利用气相色谱-质谱联用仪(GC-MS)测定PBDEs和PCBs.对提取溶剂比例、净化柱类型(复合硅胶柱与固相萃取柱)、固相萃取条件(洗脱溶剂及体积)以及脂肪的去除方法进行了优化,加标回收率较前人基础上均有明显提高.加标回收试验结果显示,PBDEs和PCBs平均基质加标回收率分别为90%—110%和71%—102%,空白加标回收率分别为70%—110%和60%—100%之间,仪器检出限(IDL)分别为0.034—0.120μg·L-1和0.032—0.392μg·L-1.本方法快速、简单、高效,能够满足指甲中PBDEs和PCBs的分析.同时本研究利用该方法对电子垃圾拆解地区居民的指甲样品进行测定,PBDEs和PCBs平均浓度分别为623 ng·g-1和148 ng·g-1,BDE(-154、-153、-183、-209)和PCB(-8、-28、-52、-66、-101、-77、-118、-153、-187)在所有样品中均检出,女性指甲中PBDEs与PCBs的浓度普遍高于男性.

Liquid-liquid extraction(LLE)and solid phase extraction(SPE)were used to extract and purify polybrominated diphenyl ethers(PBDEs)and polychlorinated biphenyls(PCBs)in human nails.The extracts were then treated with concentrated sulfuric acid to remove lipid,and the target compounds were analyzed by a gas chromatography tandem mass spectrometry.The extraction solvent ratios,purification methods(composite silica column and SPE column),SPE conditions(elution solvent and volume),and fat removal method were optimized.The recoveries of PBDEs and PCBs in spiked snail samples were 90%—110%and 53%—101%,respectively.Their recoveries in spiked blanks were 70%—110%and 60%—100%,respectively.The instrument detection limits(IDLs)were 0.034—0.120μg·L-1 for PBDEs and 0.032—0.392μg·L-1 for PCBs.The developed method was simple,efficient,and timesaving for analyzing nail PBDEs and PCBs.The average total concentrations of PBDEs and PCBs in nail samples of residents near an electronic waste dismantling site were 623 ng·g-1 and 148 ng·g-1,respectively.Four PBDEs(BDE-154,-153,-183,-209)and nine PCB(CB-8,-28,-52,-66,-101,-77,-118,-153,-187)were detected in all the samples.The nail concentrations of PBDEs and PCBs in female were generally higher than those in male.