同位素稀释-气相色谱-串联质谱法同时测定肉制品中16种欧盟优控多环芳烃

Simultaneous determination of 16 kinds of European priority polycyclic aromatic hydrocarbons in meat products by isotope dilution-gas chromatography-tandem mass spectrometry

中文关键词:  多环芳烃  气相色谱串联质谱法  同位素稀释  分子印迹柱  肉制品

英文关键词:European priority polycyclic aromatic hydrocarbons  gas chromatography-tandem mass spectrometry  isotope dilution  molecular imprinted column  meat products

中文摘要:

      目的 基于分子印迹特异性净化及同位素稀释-气相色谱-串联质谱法建立同时检测肉制品中16种欧盟优控多环芳烃的分析方法。方法 样品中加入氘代同位素内标, 经正己烷-二氯甲烷(7:3, V:V)混合溶液提取, 特异性分子印迹柱净化, 采用DB-EUPAH色谱柱分离, 在多反应监测(multiple reaction monitoring, MRM)模式下采集, 内标法定量。结果 为降低基质效应, 采用基质匹配标准曲线的定量方法。在0.2~200.0 ng/mL范围内, 16种欧盟优控多环芳烃均有良好的线性关系, 线性相关系数(r2)均大于0.9990, 在1.0、5.0、10.0 μg/kg 3个浓度水平下进行加标回收实验, 16种欧盟优控多环芳烃的回收率在85.9%~118.3%之间, 相对标准偏差(n=6)在0.4%~6.6%之间, 方法的检出限为0.03~0.10 μg/kg, 定量限为0.10~0.30 μg/kg。结论 该方法前处理简便高效、灵敏度高、准确度高、抗干扰能力强, 可同时实现肉制品中16种欧盟优控多环芳烃的测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of 16 kinds of European priority polycyclic aromatic hydrocarbons in meat products based on the molecular imprinting purification and isotope dilution-gas chromatography-tandem mass spectrometry. Methods Deuterium isotope internal standards were added to the samples, which were extracted by n-hexane-dichloromethane (7:3, V:V) mixed solution. The samples were purified by the molecular imprinted column, separated by the DB-EUPAH column, and collected in multiple reaction monitoring (MRM) mode, then quantified by the internal standard method. Results In order to reduce the matrix effect, the quantitative method of matrix matching standard curve was used in this experiment. In the range of 0.2?200.0 ng/mL, all the 16 kinds of European priority polycyclic aromatic hydrocarbons had good linear relationships, and the linear correlation coefficients were all greater than 0.9990. The detection limits of the method were 0.03?0.10 μg/kg, and the limits of quantification were 0.10?0.30 μg/kg. The recoveries of 16 kinds of European priority polycyclic aromatic hydrocarbons ranged from 85.9% to 118.3% and the relative standard deviations (n=6) ranged from 0.4% to 6.6% at the spiked levels of 1.0, 5.0 and 10.0 μg/kg. Conclusion The method has the advantages of simple pretreatment, high sensitivity, high accuracy and strong anti-interference ability, and can determine the 16 kinds of European priority polycyclic aromatic hydrocarbons in meat products simultaneously.