气相色谱-三重四级杆串联质谱同时测定香精中22种邻苯二甲酸酯
Determination of 22 Phthalate Esters in Essence by Gas Chromatography-Triple Quadrupole Mass Spectrometry
-
摘要: 建立了固相萃取法结合气相色谱-三重四级杆串联质谱同时检测香精中22种邻苯二甲酸酯(PAEs)残留量的方法。样品经乙腈和正己烷混合溶液提取,固相萃取小柱净化,然后进行测定,内标法定量。结果表明,22种邻苯二甲酸酯在3~1000 μg/L范围内呈线性相关关系,判定系数R2 ≥ 0.9922。方法检出限为0.3~1.0 μg/kg,方法定量限为1.0~3.0 μg/kg。添加20、40和200 μg/kg三个不同浓度水平,香精中22种邻苯二甲酸酯加标回收率为82.4%~107.1%,相对标准偏差为≤ 9.1%(n=6)。用此建立的方法测定了实际香精样品中的22种邻苯二甲酸酯,检出率为45.0%。此方法操作简单,灵敏度高和准确度高,适用范围广,适合香精中22种邻苯二甲酸酯残留量的检测。Abstract: A method was developed for 22 phthalate esters residues in essence using gas chromatography-triple quadrupole mass spectrometry. The samples were extracted with acetonitrile and N-hexane,cleaned up with solid phase extraction,and quantified using internal standard. The results showed that the calibration curves of the 22 phthalate esters showed good linearity in the range of 3~1000 μg/L,with the coefficient of determination(R2)not less than 0.9922.The limits of detection(LODs)were 0.3~1.0 μg/kg and the limits of quantification(LOQs)were 1.0~3.0 μg/kg. The mean recoveries in essence at the three spiked levels of 20,40 and 200 μg/kg were 82.4%~107.1%,the relative standard deviation(RSD)were not more than 9.1%(n=6). The 22 phthalate esters in the actual samples were determined by this method with the detection rate of 45.0%. The method is suitable for the determination of the 22 phthalate esters in essence with easy operation,high sensitivity and accuracy,and wide ranges of applications.