汽车用胶黏剂产品中16种邻苯二甲酸酯类增塑剂的快速检测

Rapid determination of 16 phthalate esters in automotive adhesives

目的:本研究采用气相色谱-三重四极杆质谱联用技术,同时结合改进的QuEChERS技术,建立了汽车用胶黏剂产品中16种邻苯二甲酸酯类增塑剂(PAEs)的同时检测技术。方法:样品经乙腈溶液提取,无水硫酸钠和氯化钠盐析后,经N-丙基乙二胺(PSA)填料净化,多反应监测模式,外标法定量。结果:16种增塑剂在0.05-20μg/mL范围内存在良好的线性关系,相关系数r在0.9902-0.9981之间;在0.02、0.2、2.0 mg/kg的加标水平下,回收率为80.7%-106.2%,相对标准偏差为0.41%-11.4%;检出限(S/N=3)与定量限(S/N=10)分别为0.05-0.33mg/kg和0.18-1.09 mg/kg。结论:该方法准确性和重复性好、灵敏度高,完全满足汽车用胶黏剂产品的检测需要。

Aims:A modified QuEChERS method was developed for the simultaneous determinationn of 16 phthalate esters(PAEs)in automotive adhesives by gas chromatography-mass/mass spectrometry(GC-MS/MS)analysis.Methods:The PAEs in automotive adhesives samples were extracted into acetonitrile solution,and salted out by anhydrous Na2SO4 and NaCl.The PSA adsorbent is added to the upper liquid to purify it,Multi-response monitoring model,external standard method quantization was used to determine the extraction efficiency of each sample.Results:16 PAEs possessed an excel.lent linear relation by using matrix-matched curve under 0.05-20μg/ml,and the correlation coefficients(r)were 0.9902-0.9981.The recoveries of 16 PAEs in automotive adhesives matrixes at three spiked levels of 0.02,0.2 and 2.0 mg/kg ranged from 80.7%-106.2%with relative standard deviations from 0.41%-11.4%.The LODs and LOQs for PAEs,based on S/N of 3 and 10,ranged from 0.05-0.33 mg/kg and 0.18-1.09 mg/kg.Conclusion:The applicability of the method was accurate,repeatable and sensitive,and fully meets the needs of automotive adhesive testing products.