索氏提取-气相色谱质谱法测定纸质包装材料中五种多溴联苯

Determination of five kinds of polybromobiphenyls in paper packaging material by soxhlet extraction and gas chromatography-mass spectrometry

建立了测试纸质包装材料中5种多溴联苯含量的气相色谱-质谱法(GC-MS)。以甲苯为提取剂,采用索氏提取方式提取纸质包装材料中多溴联苯,考察了提取溶剂和提取时间对提取效果的影响。提取液经浓缩、净化后用气相色谱-质谱法测定,外标法定量分析。结果表明,在0.2～10mg/l浓度范围内,5种多溴联苯均具有较好线性关系,其相关系数(r^2)均大于0.992,5种多溴联苯的检出限在0.35～0.50mg/l之间。样品平均加标回收率在86.4%～94.2%之间,相对标准偏差小于7.4%。

A method was developed for the determination of 5 polybromobiphenyls in paper packaging material by toluene assisted soxhlet extraction and gas chromatography-mass spectrometry(GC-MS).The condition of extraction solution and time of soxhlet extraction were optimized.The extract was concentrated,purified,and analyzed by GC-MS.Qualitative and quantitative analysis was carried out based on the retention time of polybromobiphenyls by external standard method.The experimental results indicated that the calibration curves are linear in the range of 0.2~10 mg/l with correlation coefficients(r2)of more than 0.992,and the detection limits of the five polybromobiphenyls are about 0.35~0.5μg/l.The average recoveries are in the range of 86.4%~94.2%for five polybromobiphenyls with the relative standard deviations below 7.4%.