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

摘要

Toy sample (0.5 g)of textile fibrous material was extracted ultrasonically with acetone (10 mL) at 60 ℃ for 30 min.The extract was evaported to dryness by N2-blowing,and the residue was dissolved and made up to 5 mL with methanol.Toy sample (0.5 g)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 5 mL 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 CH3 OH and CH3 CN (4 +1)and (B) 10 mmol·L-1 NH4 OAc solution in the volumic ratio of 5 to 95 were used as stationary phase and mobile phase for separation of the 3 isomers of hexabromocyclododecane.Linearity ranges were found same between 1.0 to 2.0 mg· L-1 for the 3 isomers,with detection limits (3S/N)of 0.1,0.2,0.5 μg·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%.%纺织纤维材质的玩具样品（0．5 g）用丙酮10 mL 于60℃超声提取30 min。提取液吹氮蒸干，残渣用甲醇溶解并定容至5 mL。橡胶、塑料材质的玩具样品（0．5 g），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5 mL，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）10 mmol·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1．0～2．0 mg·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。