QuEChERS-气相色谱—三重四极杆质谱法测定辣条中16种多环芳烃

Determination of 16 kinds of polycyclic aromatic hydrocarbons in spicy strip by QuEChERS gas chromatography-triple quadrupole mass

目的:有效提高辣条中多环芳烃污染风险预警和质量安全监管。方法:采用乙腈提取样品中的目标物,经含100 mg N-丙基乙二胺(PSA)、100 mg十八烷基硅烷键合硅胶(C_(18))、1000 mg中性氧化铝吸附剂的QuEChERS净化,选择DB-EUPAH色谱柱分离待测物,以气相色谱—三重四极杆质谱仪检测,采用多反应监测模式,基质匹配外标法定量。结果:16种PAHs在0.005~0.500μg/mL范围线性良好,相关系数为0.9984~0.9999。方法的检出限和定量限分别为0.04~0.55μg/kg和0.12~1.85μg/kg;10,20,100μg/kg三水平加标样品,16种PAHs平均加标回收率达71.54%~103.70%,相对标准偏差为2.4%~9.3%。采用该方法对20批次市售辣条样品中16种PAHs污染情况进行了分析,其中14批次样品检出多环芳烃,含量在0.42~42.28μg/kg。结论:该方法操作简单、灵敏度高,适用于辣条中16种PAHs的日常检测。

Objective:This study aimed to effectively improve the risk warning and quality and safety supervision of polycyclic aromatic hydrocarbons(PAHs)in spicy strip.Methods:The target compounds in the samples were extracted with acetonitrile and purified by QuEChERS,containing 100 mg N-propyl ethylenediamine(PSA),100 mg octadecylsilane bonded silica gel(C_(18)),and 1000 mg neutral alumina adsorbent,and then were separated by DB-EUPAH column.It was detected by gas chromatography-triple quadrupole mass spectrometer with multiple reaction monitoring mode and matrix matching external standard method.Results:The 16 kinds of PAHs showed good linearity in the range of 0.005~0.500μg/mL,and the correlation coefficients were 0.9984~0.9999.The limits of detection and quantification were 0.04~0.55μg/kg and 0.12~1.85μg/kg,respectively.The average recoveries of 16 kinds of PAHs were 71.54%~103.70%with the relative standard deviations of 2.4%~9.3%at three-level spiked standard sample of 10,20 and 100μg/kg.The method was used to analyze the contamination of 16 kinds of PAHs in 20 batches of spicy strip.PAHs were detected in 14 batches with the content ranging from 0.42μg/kg to 42.28μg/kg.Conclusion:The method is easy to operate with high sensitivity,and suitable for daily detection of 16 kinds of PAHs in spicy strip.