气相色谱-质谱法测定塑料制品中1,2-苯二酸-二烷基酯类的含量

GC-MS Determination of 1,2-Benzene Dicarboxylic Acid-Dialkyl Esters in Plastic Products

建立了测定塑料制品中1,2-苯二酸-二(C6-8支链)烷基酯(富C7)(DIHP)和1,2-苯二酸-二(C7^(-1)1支链与直链)烷基(醇)酯(DHNUP)含量的气相色谱-质谱法。以乙酸乙酯20mL为提取剂提取样品(0.500 0g),于100℃微波萃取30 min,取提取液2.0 mL用乙酸乙酯定容至5.0mL,过滤后,在选择离子监测(SIM)模式下扫描,用气相色谱-质谱法进行测定,以特征碎片离子的丰度比定性,外标法定量。结果表明,DIHP和DHNUP的线性范围均为0.40~4.0 mg·L^(-1),检出限(3S/N)为1.0~2.0 mg·kg^(-1)。按标准加入法进行回收试验,回收率在88.6%~115%之间,相对标准偏差(n=6)均小于5.0%。

A method for the determination of DIHP and DHNUP in plastic products by gas chromatographymass spectrometry（GC-MS）was proposed.DIHP and DHNUP in the sample（0.500 0 g）were extracted by microwave extraction at 100℃for 30 min using 20 mL of ethyl acetate as extraction solvent,and then 2.0 mL of the extract was taken,made its volume up to 5.0 mL with ethyl acetate and filtrated.DIHP and DHNUP were analyzed by GC-MS under selected ion monitor（SIM）mode.The abundance ratio of the characteristic fragment ions was adopted for qualitative analysis,and the external standard method was adopted for quantification.As shown by the results,linear ranges of DIHP and DHNUP were both 0.40-4.0 mg·L^-1,with detection limits（3 S/N）ranged from 1.0 mg·kg^-1 to 2.0 mg·kg^-1.Test for recovery was made by standard addition method,giving results in the range of 88.6%^-115%,with RSDs（n=6）all less than 5.0%.