基于气相色谱-离子阱法的纺织品及皮革中的富马酸二甲酯检测

为了解决样品基体复杂,干扰测定的难题,建立了一种基于气相色谱离子阱二级质谱(GC-MS/MS)检测纺织品及皮革制品中富马酸二甲酯的方法。样品中富马酸二甲酯经乙腈提取,PSA/SAX小柱净化,GC-MS/MS进行定量和定性分析。该法采用化学源电离,甲醇作为反应气,并对前处理过程所用提取溶剂,净化过程,CID电压进行了优化,大大提高灵敏度和选择性。该方法在0.05~10.0μg/mL浓度范围内呈线性关系,相关系数为0.999 8,仪器定量检出限LOQ为0.05 mg/kg,外标法定量。在50,500,1 000μg/kg 3个水平的相对标准偏差为3.52%~6.12%,回收率为84.0%~99.5%。结果表明,相对于GC、GC-MS方法,GC-MS/MS分析时间短,无杂质峰干扰,灵敏度高,可以满足纺织品及皮革制品中检测大批量筛选要求。

Determination of dimethyl fumarate in textiles and leather products by Gas Chromatography-Ion Trap mass spectrometry

To solve the interference of complex matrix sample,determination method of dimethyl fumarate in textiles and leather products was established based on Gas Chromatography-Ion Trap mass spectrometry.Dimethyl fumarate in sample was extracted with acetonitrile and purified by the Supleco PSA/SAX SPE column,and then quantative and qualitative analyses were performed by the GC-MS/MS.Chemical ionization mode was selected with methanol as reagent gas,and the extraction solvent,purification and CID voltage used in t...