论文部分内容阅读
目的建立一种同位素稀释-气相色谱-质谱法(GC-MS)同时测定食用油中16种邻苯二甲酸酯类化合物含量的方法。方法样品经正己烷溶解,乙腈提取,经固相萃取柱净化,以GC-MS在选择离子监测模式(SIM)下测定,并采用同位素内标法定量分析。结果空白基质加标回收实验添加水平分别为500.0、1000.0、2500.0μg/kg时,大豆油中16种邻苯二甲酸酯的回收率在67.4%~110.5%之间,相对标准偏差在0.3%~12.7%之间;黄油中16种邻苯二甲酸酯的回收率在60.5%~108.3%之间,相对标准偏差在0.6%~12.7%之间。该方法在50.0~1000.0μg/kg浓度范围内线性关系良好,相关系数大于0.999,方法检出限为500.0μg/kg。结论该方法灵敏度、精密度和检出限均符合实际样品检测要求,适用于食用油中PAEs化合物的同时检测。
Objective To establish a method for simultaneous determination of 16 phthalate esters in edible oil by isotope dilution-gas chromatography-mass spectrometry (GC-MS). Methods The sample was dissolved in n-hexane, extracted with acetonitrile, purified by solid phase extraction (SPE) column, determined by GC-MS in SIM mode and quantified by isotope internal standard method. Results The recoveries of 16 kinds of phthalates in soybean oil were between 67.4% and 110.5% with the relative standard deviations of 0.3% at the spiked levels of 500.0, 1000.0 and 2500.0 μg / kg respectively. ~ 12.7%. The recovery of 16 phthalates in butter ranged from 60.5% to 108.3% with relative standard deviations between 0.6% and 12.7%. The method has a good linearity in the range of 50.0 ~ 1000.0μg / kg, the correlation coefficient is greater than 0.999, and the detection limit is 500.0μg / kg. Conclusion The sensitivity, precision and detection limit of the method are in line with the actual sample testing requirements for the simultaneous detection of PAEs compounds in edible oils.