超高效液相色谱-串联质谱法测定玩具材料中六溴环十二烷的3种同分异构体的含量

UHPLC-MS/MS Determination of 3 Isomers of Hexabromocylododecane in Materials for Making Toys

纺织纤维材质的玩具样品(0.5g)用丙酮10mL于60℃超声提取30min。提取液吹氮蒸干,残渣用甲醇溶解并定容至5mL。橡胶、塑料材质的玩具样品(0.5g),用甲苯-甲醇(10+1)混合液进行索氏提取。将提取液蒸至近干,残渣用甲醇溶解并定容至5mL,所得溶液供超高效液相色谱-串联质谱分析。用Acquity UPLC BEH C18色谱柱作固定相,用(A)甲醇-乙腈(4+1)混合液和(B)10mmol·L-1乙酸铵溶液(5+95)混合液作流动相进行洗脱,实现了六溴环十二烷的3种同分异构体的色谱分离。α,β,γ-六溴环十二烷的质量浓度均在1.0~2.0mg·L-1范围内呈线性,3种异构体的检出限(3S/N)依次为0.1,0.2,0.5μg·L-1。加标回收率在70.0%~112%之间,测定值的相对标准偏差(n=6)在0.070%~9.9%之间。

Toy sample(0.5g)of textile fibrous material was extracted ultrasonically with acetone(10mL)at 60℃ for 30min.The extract was evaported to dryness by N2-blowing,and the residue was dissolved and made up to 5mL with methanol.Toy sample(0.5g)of plastic or rubber material was treated by soxhlet extraction with mixture of toluene and methanol(10+1)and the extract was evaporated to dryness.The residue was dissolved and made up to 5mL with methanol.The methanol solution was used for UHPLC-MS/MS analysis.Chromatographic column of Acquity UPLC BEH C18 and mixture of(A)mixed solvent of CH3OH and CH3CN(4+1)and(B)10mmol·L-1 NH4OAc solution in the volumic ratio of 5 to 95 were used as stationary phase and mobile phase for separation of the 3isomers of hexabromocyclododecane.Linearity ranges were found same between 1.0 to 2.0mg·L-1 for the 3 isomers,with detection limits(3S/N)of 0.1,0.2,0.5μg·L-1 respectively.Values of recovery found by standard addition method were in the range of 70.0%-112% with RSD′s(n=6)ranged from 0.070% to 9.9%.